_publ_information ; Michael D. Pluth, Darren W. Johnson, Geza Szigethy, Anna V. Davis, Simon J. Teat, Allen G. Oliver, Robert G. Bergman, Kenneth N. Raymond Structural Consequences of Anionic Host- Cationic Guest Interactions in a Supramolecular Assembly ; data_Structure3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Ti4L6 Et4N cluster' _chemical_melting_point 'not measured' _chemical_formula_moiety ; 'C182 H111 N17.50 O36 Ti4' ; _chemical_formula_sum 'C182 H111 N17.50 O36 Ti4' _chemical_formula_weight 3310.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' -0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' -0.0031 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' -0.0041 0.0074 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2263 0.5295 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 20.844(3) _cell_length_b 20.844(3) _cell_length_c 163.55(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 61540(25) _cell_formula_units_Z 12 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7627 _cell_measurement_theta_min 2.256 _cell_measurement_theta_max 19.045 _exptl_crystal_description 'trigonal prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.072 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 20418 _exptl_absorpt_coefficient_mu 0.271 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9579 _exptl_absorpt_correction_T_max 0.9682 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Advanced Light Source Station 11.3.1' _diffrn_radiation_monochromator 'channel cut Si-(111) crystal' _diffrn_measurement_device_type 'Bruker Platinum 200' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean 3.623 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 48435 _diffrn_reflns_av_R_equivalents 0.0722 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -133 _diffrn_reflns_limit_l_max 138 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 19.32 _reflns_number_total 4345 _reflns_number_gt 3636 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v.2.0.2' _computing_cell_refinement 'Bruker SAINT v.7.23' _computing_data_reduction 'Bruker SATIN v.7.23' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 v.1.08, POV-Ray v.3.6.1c.icl8.win32' _computing_publication_material 'ORTEP-3 v.1.08, POV-Ray v.3.6.1c.icl8.win32' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The Ti and Co atoms as well as the N and O atoms in the assembly were refined anisotropically. Hydrogen atoms were included at calculated positions on the ligand and the ordered NEt4+ on the exterior of the assembly and their positions were refined using the riding model. Hydrogen atoms were not included on any of the disordered solvent molecules in the asymmetric unit. The bond distances in the catechol and naphthalene rings were modeled as standard aromatic rings using typical bond length restraints. The encapsulated NEt4+ lies with the nitrogen and one methyl group on a crystallographic 3-fold axis and the remaining arms of the molecule were disordered accordingly. Of the exterior NEt4+ molecules, one is crystallographically ordered and the other sits near a 3-fold axis. Attempts to model the disordered NEt4+ with the nitrogen on the 3-fold axis were unsuccessful. This structure contained large pockets of disordered solvent as well as the remaining NEt4+ molecule per assembly which was not located. The required electron density in the unit cell necessary to account for the remaining NEt4+ molecules is 1200 electrons, and calculation of the electron density in these solvent channels was calculated in Platon by the method of Spek and showed that approximately 3256 electrons of disordered solvent were present throughout the unit cell. This is sufficient to account for the solvated NEt4+ molecules and 5.5 water molecules per asymmetric unit (16.5 molecules per assembly). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4345 _refine_ls_number_parameters 426 _refine_ls_number_restraints 564 _refine_ls_R_factor_all 0.1703 _refine_ls_R_factor_gt 0.1594 _refine_ls_wR_factor_ref 0.4669 _refine_ls_wR_factor_gt 0.4533 _refine_ls_goodness_of_fit_ref 2.161 _refine_ls_restrained_S_all 2.099 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.0000 0.0000 0.07762(2) 0.0978(16) Uani 1 3 d S . . Ti2 Ti 0.35959(13) 0.35111(13) 0.141425(18) 0.1096(14) Uani 1 1 d . . . O01 O 0.0890(4) 0.0275(4) 0.08465(5) 0.096(3) Uani 1 1 d . . . O02 O 0.0497(5) -0.0388(5) 0.07089(5) 0.108(3) Uani 1 1 d . . . O03 O 0.3060(7) 0.1008(8) 0.09438(8) 0.172(5) Uani 1 1 d . . . O04 O 0.1568(7) 0.4043(6) 0.11723(7) 0.147(4) Uani 1 1 d . . . O05 O 0.3648(5) 0.4422(5) 0.14490(8) 0.146(4) Uani 1 1 d . . . O06 O 0.2904(4) 0.3546(4) 0.13320(5) 0.096(3) Uani 1 1 d . . . O07 O 0.3620(4) 0.2674(4) 0.13608(5) 0.096(3) Uani 1 1 d . . . O08 O 0.4498(4) 0.4045(4) 0.13559(7) 0.128(4) Uani 1 1 d . . . O09 O 0.4187(5) 0.1137(5) 0.12520(7) 0.135(4) Uani 1 1 d . . . O10 O 0.1075(7) 0.1711(8) 0.16580(8) 0.173(5) Uani 1 1 d . . . O11 O 0.4071(5) 0.3471(5) 0.15158(6) 0.121(3) Uani 1 1 d . . . O12 O 0.2725(4) 0.2845(4) 0.14782(6) 0.104(3) Uani 1 1 d . . . N01 N 0.1939(6) 0.0925(6) 0.09607(7) 0.110(4) Uani 1 1 d . . . H01B H 0.1490 0.0747 0.0941 0.133 Uiso 1 1 calc R . . N02 N 0.1998(5) 0.3240(5) 0.12013(7) 0.105(4) Uani 1 1 d . . . H02B H 0.2232 0.3125 0.1238 0.126 Uiso 1 1 calc R . . N03 N 0.3498(6) 0.1293(5) 0.13483(6) 0.098(3) Uani 1 1 d . . . H03B H 0.3399 0.1620 0.1370 0.118 Uiso 1 1 calc R . . C01 C 0.1404(7) 0.0155(7) 0.08112(8) 0.101(4) Uiso 1 1 d D . . C02 C 0.1168(7) -0.0228(7) 0.07367(8) 0.107(4) Uiso 1 1 d D . . C03 C 0.1651(8) -0.0384(9) 0.06913(10) 0.157(6) Uiso 1 1 d D . . H03A H 0.1498 -0.0639 0.0641 0.188 Uiso 1 1 calc R . . C04 C 0.2361(8) -0.0155(8) 0.07223(9) 0.143(6) Uiso 1 1 d D . . H04A H 0.2684 -0.0272 0.0693 0.172 Uiso 1 1 calc R . . C05 C 0.2599(8) 0.0240(8) 0.07954(8) 0.131(5) Uiso 1 1 d D . . H05A H 0.3091 0.0417 0.0814 0.157 Uiso 1 1 calc R . . C06 C 0.2114(6) 0.0378(7) 0.08416(7) 0.100(4) Uiso 1 1 d D . . C25 C 0.4244(7) 0.2850(6) 0.13184(8) 0.100(4) Uiso 1 1 d D . . C26 C 0.4713(7) 0.3621(7) 0.13136(9) 0.121(5) Uiso 1 1 d D . . C27 C 0.5392(8) 0.3903(8) 0.12711(9) 0.130(5) Uiso 1 1 d D . . H27A H 0.5733 0.4421 0.1271 0.156 Uiso 1 1 calc R . . C28 C 0.5563(8) 0.3417(7) 0.12296(10) 0.141(6) Uiso 1 1 d D . . H28A H 0.5996 0.3615 0.1197 0.170 Uiso 1 1 calc R . . C29 C 0.5108(7) 0.2644(7) 0.12357(9) 0.127(5) Uiso 1 1 d D . . H29A H 0.5240 0.2320 0.1209 0.152 Uiso 1 1 calc R . . C30 C 0.4445(6) 0.2362(6) 0.12822(8) 0.099(4) Uiso 1 1 d D . . C43 C 0.2310(8) 0.2334(8) 0.16156(9) 0.132(5) Uiso 1 1 d D . . C44 C 0.2547(11) 0.2250(12) 0.16948(11) 0.194(8) Uiso 1 1 d D . . H44A H 0.2195 0.1990 0.1737 0.232 Uiso 1 1 calc R . . C45 C 0.3314(10) 0.2559(11) 0.17099(12) 0.194(8) Uiso 1 1 d D . . H45A H 0.3472 0.2483 0.1762 0.233 Uiso 1 1 calc R . . C46 C 0.3839(10) 0.2967(10) 0.16517(11) 0.166(7) Uiso 1 1 d D . . H46A H 0.4350 0.3186 0.1665 0.199 Uiso 1 1 calc R . . C47 C 0.3622(9) 0.3062(9) 0.15725(10) 0.134(6) Uiso 1 1 d D . . C48 C 0.2855(8) 0.2748(8) 0.15577(9) 0.118(5) Uiso 1 1 d D . . C19 C 0.2376(7) 0.4305(6) 0.12883(7) 0.098(4) Uiso 1 1 d D . . C20 C 0.2324(7) 0.4949(7) 0.13054(8) 0.111(4) Uiso 1 1 d D . . H20A H 0.2013 0.5066 0.1274 0.134 Uiso 1 1 calc R . . C21 C 0.2743(9) 0.5399(9) 0.13699(10) 0.161(6) Uiso 1 1 d D . . H21A H 0.2722 0.5837 0.1380 0.193 Uiso 1 1 calc R . . C22 C 0.3189(9) 0.5252(8) 0.14202(10) 0.144(6) Uiso 1 1 d D . . H22A H 0.3464 0.5575 0.1464 0.173 Uiso 1 1 calc R . . C23 C 0.3215(8) 0.4598(7) 0.14040(8) 0.115(5) Uiso 1 1 d D . . C24 C 0.2827(6) 0.4148(7) 0.13379(7) 0.092(4) Uiso 1 1 d D . . C07 C 0.2395(11) 0.0770(9) 0.09189(10) 0.119(5) Uiso 1 1 d . . . C08 C 0.2102(6) 0.1354(7) 0.10358(8) 0.093(4) Uiso 1 1 d D . . C09 C 0.2511(7) 0.1244(7) 0.10969(7) 0.110(4) Uiso 1 1 d D . . H09A H 0.2662 0.0886 0.1090 0.132 Uiso 1 1 calc R . . C10 C 0.2690(7) 0.1671(7) 0.11681(8) 0.121(5) Uiso 1 1 d D . . H10A H 0.2991 0.1621 0.1208 0.145 Uiso 1 1 calc R . . C11 C 0.2434(6) 0.2174(7) 0.11814(7) 0.102(4) Uiso 1 1 d D . . H11A H 0.2553 0.2451 0.1231 0.123 Uiso 1 1 calc R . . C12 C 0.2003(6) 0.2261(6) 0.11212(7) 0.092(4) Uiso 1 1 d D . . C13 C 0.1812(6) 0.1823(6) 0.10501(7) 0.092(4) Uiso 1 1 d D . . C14 C 0.1386(9) 0.1917(9) 0.09884(9) 0.142(6) Uiso 1 1 d D . . H14A H 0.1277 0.1649 0.0939 0.170 Uiso 1 1 calc R . . C15 C 0.1133(9) 0.2414(8) 0.10029(9) 0.147(6) Uiso 1 1 d D . . H15A H 0.0839 0.2470 0.0962 0.176 Uiso 1 1 calc R . . C16 C 0.1292(8) 0.2833(9) 0.10746(9) 0.142(6) Uiso 1 1 d D . . H16A H 0.1107 0.3162 0.1083 0.170 Uiso 1 1 calc R . . C17 C 0.1732(6) 0.2750(7) 0.11336(7) 0.090(4) Uiso 1 1 d D . . C18 C 0.1958(8) 0.3860(9) 0.12201(9) 0.116(4) Uiso 1 1 d . . . C31 C 0.4053(8) 0.1573(8) 0.12946(9) 0.100(4) Uiso 1 1 d . . . C32 C 0.3028(7) 0.0538(7) 0.13770(8) 0.105(4) Uiso 1 1 d D . . C33 C 0.3282(8) 0.0029(7) 0.13656(9) 0.121(5) Uiso 1 1 d D . . H33A H 0.3738 0.0170 0.1339 0.146 Uiso 1 1 calc R . . C34 C 0.2833(8) -0.0693(8) 0.13958(10) 0.141(6) Uiso 1 1 d D . . H34A H 0.2970 -0.1057 0.1386 0.169 Uiso 1 1 calc R . . C35 C 0.2197(8) -0.0887(8) 0.14400(10) 0.137(5) Uiso 1 1 d D . . H35A H 0.1922 -0.1370 0.1463 0.164 Uiso 1 1 calc R . . C36 C 0.1954(6) -0.0373(6) 0.14520(8) 0.110(4) Uiso 1 1 d D . . C37 C 0.2384(6) 0.0352(5) 0.14211(7) 0.078(3) Uiso 1 1 d D . . C38 C 0.2178(7) 0.0890(7) 0.14376(8) 0.114(4) Uiso 1 1 d D . . H38A H 0.2469 0.1384 0.1418 0.137 Uiso 1 1 calc R . . C39 C 0.1540(7) 0.0679(7) 0.14830(9) 0.128(5) Uiso 1 1 d D . . H39A H 0.1382 0.1030 0.1492 0.153 Uiso 1 1 calc R . . C40 C 0.1119(9) -0.0039(7) 0.15155(10) 0.145(6) Uiso 1 1 d D . . H40A H 0.0691 -0.0166 0.1547 0.174 Uiso 1 1 calc R . . C41 C 0.1334(7) -0.0570(7) 0.15010(8) 0.098(4) Uiso 1 1 d D . . C42 C 0.1534(10) 0.2054(9) 0.16020(13) 0.120(5) Uiso 1 1 d . . . N50 N 0.1597(10) 0.4025(10) 0.22338(11) 0.085(5) Uiso 0.50 1 d P . . C50 C 0.216(2) 0.379(2) 0.2195(2) 0.149(4) Uiso 0.50 1 d P . . H50A H 0.2018 0.3288 0.2213 0.178 Uiso 0.50 1 calc PR . . H50B H 0.2666 0.4134 0.2216 0.178 Uiso 0.50 1 calc PR . . C51 C 0.2181(19) 0.3816(19) 0.2105(2) 0.149(4) Uiso 0.50 1 d P . . H51A H 0.2536 0.3673 0.2085 0.223 Uiso 0.50 1 calc PR . . H51B H 0.2333 0.4319 0.2086 0.223 Uiso 0.50 1 calc PR . . H51C H 0.1687 0.3471 0.2083 0.223 Uiso 0.50 1 calc PR . . C52 C 0.0785(19) 0.3513(18) 0.2207(2) 0.149(4) Uiso 0.50 1 d P . . H52A H 0.0778 0.3524 0.2146 0.178 Uiso 0.50 1 calc PR . . H52B H 0.0498 0.3744 0.2226 0.178 Uiso 0.50 1 calc PR . . C53 C 0.0343(19) 0.2674(18) 0.2233(2) 0.149(4) Uiso 0.50 1 d P . . H53A H -0.0144 0.2431 0.2207 0.223 Uiso 0.50 1 calc PR . . H53B H 0.0280 0.2641 0.2293 0.223 Uiso 0.50 1 calc PR . . H53C H 0.0619 0.2429 0.2217 0.223 Uiso 0.50 1 calc PR . . C54 C 0.1630(19) 0.4080(19) 0.2325(2) 0.149(4) Uiso 0.50 1 d P . . H54A H 0.1905 0.3916 0.2356 0.178 Uiso 0.50 1 calc PR . . C55 C 0.1195(19) 0.4415(19) 0.2366(2) 0.149(4) Uiso 0.50 1 d P . . H55A H 0.1277 0.4443 0.2426 0.223 Uiso 0.50 1 calc PR . . H55B H 0.0665 0.4101 0.2355 0.223 Uiso 0.50 1 calc PR . . H55C H 0.1368 0.4914 0.2345 0.223 Uiso 0.50 1 calc PR . . C56 C 0.182(2) 0.4792(19) 0.2203(2) 0.149(4) Uiso 0.50 1 d P . . H56A H 0.1432 0.4858 0.2182 0.178 Uiso 0.50 1 calc PR . . C57 C 0.2550(19) 0.5435(19) 0.2203(2) 0.149(4) Uiso 0.50 1 d P . . H57A H 0.2535 0.5846 0.2176 0.223 Uiso 0.50 1 calc PR . . H57B H 0.2890 0.5321 0.2174 0.223 Uiso 0.50 1 calc PR . . H57C H 0.2722 0.5575 0.2259 0.223 Uiso 0.50 1 calc PR . . N60 N 0.0000 0.0000 0.12167(13) 0.116(6) Uiso 1 3 d SD . . C61 C -0.0184(18) 0.0621(14) 0.12173(19) 0.152(12) Uiso 0.50 1 d PD . . C62 C 0.030(2) 0.1419(16) 0.1240(2) 0.160(13) Uiso 0.50 1 d PD . . C63 C 0.000(5) 0.039(3) 0.11379(15) 0.22(3) Uiso 0.33 1 d PD . . C64 C 0.0000 0.0000 0.1060(2) 0.187(13) Uiso 1 3 d SD . . C786 C 0.073(3) 0.115(3) 0.1285(3) 0.27(2) Uiso 0.67 1 d P . . N71 N -0.0323(19) -0.025(2) 0.1848(3) 0.47(3) Uiso 1 1 d D . . C72 C -0.0936(17) -0.102(2) 0.1820(2) 0.421(14) Uiso 1 1 d D A 1 C73 C -0.078(4) -0.164(3) 0.1840(5) 0.53(5) Uiso 1 1 d D A 1 C74 C -0.101(3) -0.065(3) 0.1899(2) 0.54(5) Uiso 1 1 d D A . C75 C -0.162(2) -0.047(2) 0.1883(2) 0.313(17) Uiso 1 1 d D . . C76 C -0.017(3) -0.063(2) 0.1761(3) 0.325(19) Uiso 1 1 d . . 2 C77 C -0.0936(17) -0.102(2) 0.1820(2) 0.421(14) Uiso 1 1 d . A 2 N04 N 0.1316(6) 0.2169(6) 0.15306(7) 0.111(4) Uani 1 1 d . . . H04B H 0.1673 0.2445 0.1496 0.133 Uiso 1 1 calc R . . C878 C 0.0000 0.0000 0.1315(5) 0.32(3) Uiso 1 3 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.106(2) 0.106(2) 0.081(3) 0.000 0.000 0.0532(10) Ti2 0.085(2) 0.0845(19) 0.150(3) -0.0286(15) -0.0260(15) 0.0358(15) O01 0.088(5) 0.111(6) 0.087(6) 0.003(5) 0.007(4) 0.048(5) O02 0.120(7) 0.138(7) 0.082(6) -0.020(5) -0.005(5) 0.077(6) O03 0.117(8) 0.219(12) 0.168(11) -0.047(9) -0.013(8) 0.075(8) O04 0.194(10) 0.177(10) 0.134(8) 0.011(7) -0.005(8) 0.140(9) O05 0.108(7) 0.095(7) 0.220(12) -0.059(7) -0.051(7) 0.040(6) O06 0.086(5) 0.070(5) 0.137(7) 0.001(5) -0.004(5) 0.042(4) O07 0.086(6) 0.078(5) 0.115(7) -0.009(4) -0.017(5) 0.035(4) O08 0.067(5) 0.075(5) 0.231(11) -0.016(6) -0.006(6) 0.028(5) O09 0.123(7) 0.100(7) 0.178(10) -0.005(7) 0.011(7) 0.053(6) O10 0.161(10) 0.228(13) 0.123(9) -0.009(9) 0.004(8) 0.092(10) O11 0.094(6) 0.110(7) 0.151(9) -0.049(6) -0.062(6) 0.046(6) O12 0.073(5) 0.098(6) 0.129(8) -0.024(5) -0.008(5) 0.034(5) N01 0.100(8) 0.136(9) 0.112(9) -0.003(7) -0.006(7) 0.071(7) N02 0.094(7) 0.069(7) 0.160(10) 0.010(7) -0.002(7) 0.046(6) N03 0.109(8) 0.083(7) 0.102(8) -0.001(6) -0.014(7) 0.047(6) N04 0.095(8) 0.125(9) 0.116(10) -0.026(7) -0.008(7) 0.058(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O02 1.943(8) 3 ? Ti1 O02 1.943(8) 2 ? Ti1 O02 1.943(8) . ? Ti1 O01 2.007(8) . ? Ti1 O01 2.007(8) 2 ? Ti1 O01 2.007(8) 3 ? Ti2 O08 1.895(10) . ? Ti2 O05 1.933(10) . ? Ti2 O12 1.948(9) . ? Ti2 O11 1.956(9) . ? Ti2 O07 1.974(8) . ? Ti2 O06 1.999(8) . ? O01 C01 1.347(13) . ? O02 C02 1.345(14) . ? O03 C07 1.285(18) . ? O04 C18 1.315(17) . ? O05 C23 1.348(15) . ? O06 C24 1.348(13) . ? O07 C25 1.353(14) . ? O08 C26 1.362(15) . ? O09 C31 1.283(16) . ? O10 C42 1.258(19) . ? O11 C47 1.291(16) . ? O12 C48 1.363(15) . ? N01 C07 1.334(18) . ? N01 C08 1.456(15) . ? N01 H01B 0.8800 . ? N02 C18 1.371(18) . ? N02 C17 1.418(14) . ? N02 H02B 0.8800 . ? N03 C31 1.331(16) . ? N03 C32 1.454(15) . ? N03 H03B 0.8800 . ? C01 C06 1.403(10) . ? C01 C02 1.405(10) . ? C02 C03 1.414(10) . ? C03 C04 1.403(10) . ? C03 H03A 0.9500 . ? C04 C05 1.394(10) . ? C04 H04A 0.9500 . ? C05 C06 1.402(10) . ? C05 H05A 0.9500 . ? C06 C07 1.458(19) . ? C25 C26 1.406(11) . ? C25 C30 1.409(11) . ? C26 C27 1.415(11) . ? C27 C28 1.406(11) . ? C27 H27A 0.9500 . ? C28 C29 1.406(11) . ? C28 H28A 0.9500 . ? C29 C30 1.422(11) . ? C29 H29A 0.9500 . ? C30 C31 1.439(17) . ? C43 C48 1.397(12) . ? C43 C42 1.44(2) . ? C43 C44 1.428(12) . ? C44 C45 1.416(13) . ? C44 H44A 0.9500 . ? C45 C46 1.376(12) . ? C45 H45A 0.9500 . ? C46 C47 1.418(12) . ? C46 H46A 0.9500 . ? C47 C48 1.412(12) . ? C19 C18 1.433(17) . ? C19 C24 1.397(11) . ? C19 C20 1.428(11) . ? C20 C21 1.391(12) . ? C20 H20A 0.9500 . ? C21 C22 1.385(12) . ? C21 H21A 0.9500 . ? C22 C23 1.416(12) . ? C22 H22A 0.9500 . ? C23 C24 1.395(11) . ? C08 C13 1.403(15) . ? C08 C09 1.405(10) . ? C09 C10 1.399(10) . ? C09 H09A 0.9500 . ? C10 C11 1.410(9) . ? C10 H10A 0.9500 . ? C11 C12 1.405(9) . ? C11 H11A 0.9500 . ? C12 C13 1.407(9) . ? C12 C17 1.405(9) . ? C13 C14 1.419(10) . ? C14 C15 1.400(10) . ? C14 H14A 0.9500 . ? C15 C16 1.398(10) . ? C15 H15A 0.9500 . ? C16 C17 1.400(10) . ? C16 H16A 0.9500 . ? C32 C37 1.397(14) . ? C32 C33 1.416(10) . ? C33 C34 1.407(10) . ? C33 H33A 0.9500 . ? C34 C35 1.381(10) . ? C34 H34A 0.9500 . ? C35 C36 1.410(10) . ? C35 H35A 0.9500 . ? C36 C41 1.396(9) . ? C36 C37 1.409(9) . ? C37 C38 1.413(10) . ? C38 C39 1.390(10) . ? C38 H38A 0.9500 . ? C39 C40 1.408(10) . ? C39 H39A 0.9500 . ? C40 C41 1.405(10) . ? C40 H40A 0.9500 . ? C41 N04 1.448(15) 3 ? C42 N04 1.316(19) . ? N50 C54 1.50(4) . ? N50 C50 1.61(4) . ? N50 C52 1.55(4) . ? N50 C56 1.51(4) . ? C50 C51 1.48(4) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.57(4) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.55(4) . ? C54 H54A 0.9500 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.44(4) . ? C56 H56A 0.9500 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? N60 C878 1.61(7) . ? N60 C61 1.522(18) 2 ? N60 C61 1.522(17) 3 ? N60 C61 1.522(17) . ? N60 C63 1.530(19) . ? N60 C63 1.530(19) 2 ? N60 C63 1.530(19) 3 ? C61 C62 1.496(19) . ? C61 C63 1.495(19) . ? C62 C786 1.47(6) . ? C63 C63 1.43(6) 2 ? C63 C63 1.43(6) 3 ? C63 C64 1.515(19) . ? C64 C63 1.515(19) 3 ? C64 C63 1.515(19) 2 ? N71 C76 1.73(5) . ? N71 C74 1.50(2) . ? N71 C72 1.528(19) . ? N71 C76 1.77(5) 3 ? C72 C74 1.55(2) . ? C72 C73 1.53(2) . ? C74 C75 1.52(2) . ? C76 N71 1.77(5) 2 ? N04 C41 1.448(15) 2 ? N04 H04B 0.8800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O02 Ti1 O02 91.0(4) 3 2 ? O02 Ti1 O02 91.0(4) 3 . ? O02 Ti1 O02 91.0(4) 2 . ? O02 Ti1 O01 166.4(4) 3 . ? O02 Ti1 O01 99.6(3) 2 . ? O02 Ti1 O01 80.5(3) . . ? O02 Ti1 O01 99.6(3) 3 2 ? O02 Ti1 O01 80.5(3) 2 2 ? O02 Ti1 O01 166.4(4) . 2 ? O01 Ti1 O01 90.4(3) . 2 ? O02 Ti1 O01 80.5(3) 3 3 ? O02 Ti1 O01 166.4(4) 2 3 ? O02 Ti1 O01 99.6(3) . 3 ? O01 Ti1 O01 90.4(3) . 3 ? O01 Ti1 O01 90.4(3) 2 3 ? O08 Ti2 O05 91.1(4) . . ? O08 Ti2 O12 170.4(4) . . ? O05 Ti2 O12 96.7(4) . . ? O08 Ti2 O11 94.5(5) . . ? O05 Ti2 O11 90.7(5) . . ? O12 Ti2 O11 79.9(4) . . ? O08 Ti2 O07 80.8(4) . . ? O05 Ti2 O07 170.0(5) . . ? O12 Ti2 O07 91.9(4) . . ? O11 Ti2 O07 95.8(4) . . ? O08 Ti2 O06 99.3(4) . . ? O05 Ti2 O06 81.3(4) . . ? O12 Ti2 O06 87.5(4) . . ? O11 Ti2 O06 164.2(4) . . ? O07 Ti2 O06 94.1(3) . . ? C01 O01 Ti1 114.2(7) . . ? C02 O02 Ti1 114.2(7) . . ? C23 O05 Ti2 113.0(8) . . ? C24 O06 Ti2 114.2(7) . . ? C25 O07 Ti2 115.7(7) . . ? C26 O08 Ti2 115.3(7) . . ? C47 O11 Ti2 115.0(9) . . ? C48 O12 Ti2 115.8(8) . . ? C07 N01 C08 127.2(12) . . ? C07 N01 H01B 116.4 . . ? C08 N01 H01B 116.4 . . ? C18 N02 C17 132.0(11) . . ? C18 N02 H02B 114.0 . . ? C17 N02 H02B 114.0 . . ? C31 N03 C32 130.9(12) . . ? C31 N03 H03B 114.5 . . ? C32 N03 H03B 114.5 . . ? O01 C01 C06 126.3(10) . . ? O01 C01 C02 113.1(10) . . ? C06 C01 C02 120.6(11) . . ? O02 C02 C01 117.4(10) . . ? O02 C02 C03 122.6(11) . . ? C01 C02 C03 119.9(12) . . ? C04 C03 C02 118.9(13) . . ? C04 C03 H03A 120.5 . . ? C02 C03 H03A 120.5 . . ? C05 C04 C03 120.9(13) . . ? C05 C04 H04A 119.5 . . ? C03 C04 H04A 119.5 . . ? C04 C05 C06 120.3(12) . . ? C04 C05 H05A 119.8 . . ? C06 C05 H05A 119.8 . . ? C05 C06 C01 119.3(11) . . ? C05 C06 C07 117.1(12) . . ? C01 C06 C07 123.6(12) . . ? O07 C25 C26 111.2(10) . . ? O07 C25 C30 127.8(11) . . ? C26 C25 C30 121.0(12) . . ? C27 C26 C25 118.8(12) . . ? C27 C26 O08 124.5(11) . . ? C25 C26 O08 116.6(11) . . ? C26 C27 C28 120.0(13) . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C29 C28 C27 121.5(13) . . ? C29 C28 H28A 119.2 . . ? C27 C28 H28A 119.2 . . ? C28 C29 C30 118.1(12) . . ? C28 C29 H29A 120.9 . . ? C30 C29 H29A 120.9 . . ? C25 C30 C31 124.1(12) . . ? C25 C30 C29 120.3(11) . . ? C31 C30 C29 115.3(11) . . ? C48 C43 C42 123.3(15) . . ? C48 C43 C44 117.8(13) . . ? C42 C43 C44 118.6(15) . . ? C43 C44 C45 118.9(15) . . ? C43 C44 H44A 120.6 . . ? C45 C44 H44A 120.6 . . ? C46 C45 C44 122.0(16) . . ? C46 C45 H45A 119.0 . . ? C44 C45 H45A 119.0 . . ? C45 C46 C47 120.5(15) . . ? C45 C46 H46A 119.8 . . ? C47 C46 H46A 119.8 . . ? O11 C47 C48 117.5(14) . . ? O11 C47 C46 124.9(14) . . ? C48 C47 C46 117.3(14) . . ? C43 C48 O12 125.3(13) . . ? C43 C48 C47 123.5(13) . . ? O12 C48 C47 110.9(12) . . ? C18 C19 C24 124.2(12) . . ? C18 C19 C20 116.9(12) . . ? C24 C19 C20 118.8(11) . . ? C21 C20 C19 117.7(12) . . ? C21 C20 H20A 121.1 . . ? C19 C20 H20A 121.1 . . ? C20 C21 C22 124.4(14) . . ? C20 C21 H21A 117.8 . . ? C22 C21 H21A 117.8 . . ? C21 C22 C23 117.1(13) . . ? C21 C22 H22A 121.4 . . ? C23 C22 H22A 121.4 . . ? O05 C23 C24 118.8(11) . . ? O05 C23 C22 120.9(12) . . ? C24 C23 C22 120.1(12) . . ? O06 C24 C23 112.4(10) . . ? O06 C24 C19 125.8(10) . . ? C23 C24 C19 121.7(11) . . ? N01 C07 O03 120.4(15) . . ? N01 C07 C06 116.5(15) . . ? O03 C07 C06 123.0(16) . . ? C13 C08 C09 120.2(11) . . ? C13 C08 N01 121.3(10) . . ? C09 C08 N01 118.3(11) . . ? C10 C09 C08 118.7(11) . . ? C10 C09 H09A 120.6 . . ? C08 C09 H09A 120.6 . . ? C09 C10 C11 121.3(11) . . ? C09 C10 H10A 119.3 . . ? C11 C10 H10A 119.3 . . ? C12 C11 C10 119.5(11) . . ? C12 C11 H11A 120.2 . . ? C10 C11 H11A 120.2 . . ? C13 C12 C11 119.1(10) . . ? C13 C12 C17 120.3(10) . . ? C11 C12 C17 120.5(9) . . ? C12 C13 C08 120.6(10) . . ? C12 C13 C14 119.4(11) . . ? C08 C13 C14 119.6(10) . . ? C15 C14 C13 118.3(13) . . ? C15 C14 H14A 120.8 . . ? C13 C14 H14A 120.8 . . ? C16 C15 C14 123.0(13) . . ? C16 C15 H15A 118.5 . . ? C14 C15 H15A 118.5 . . ? C15 C16 C17 117.8(13) . . ? C15 C16 H16A 121.1 . . ? C17 C16 H16A 121.1 . . ? N02 C17 C16 119.6(10) . . ? N02 C17 C12 118.8(10) . . ? C16 C17 C12 121.0(11) . . ? O04 C18 N02 118.5(13) . . ? O04 C18 C19 122.7(15) . . ? N02 C18 C19 118.8(14) . . ? O09 C31 N03 119.8(13) . . ? O09 C31 C30 122.2(14) . . ? N03 C31 C30 117.9(14) . . ? C37 C32 N03 120.1(10) . . ? C37 C32 C33 121.8(11) . . ? N03 C32 C33 117.8(11) . . ? C34 C33 C32 117.2(12) . . ? C34 C33 H33A 121.4 . . ? C32 C33 H33A 121.4 . . ? C35 C34 C33 121.6(13) . . ? C35 C34 H34A 119.2 . . ? C33 C34 H34A 119.2 . . ? C34 C35 C36 120.6(12) . . ? C34 C35 H35A 119.7 . . ? C36 C35 H35A 119.7 . . ? C41 C36 C37 121.4(10) . . ? C41 C36 C35 119.2(10) . . ? C37 C36 C35 119.1(10) . . ? C32 C37 C36 119.4(10) . . ? C32 C37 C38 120.6(9) . . ? C36 C37 C38 120.0(10) . . ? C39 C38 C37 118.3(11) . . ? C39 C38 H38A 120.9 . . ? C37 C38 H38A 120.9 . . ? C38 C39 C40 121.8(12) . . ? C38 C39 H39A 119.1 . . ? C40 C39 H39A 119.1 . . ? C41 C40 C39 120.1(13) . . ? C41 C40 H40A 120.0 . . ? C39 C40 H40A 120.0 . . ? C36 C41 C40 118.4(12) . . ? C36 C41 N04 123.4(10) . 3 ? C40 C41 N04 117.9(11) . 3 ? O10 C42 N04 121.1(17) . . ? O10 C42 C43 119.9(18) . . ? N04 C42 C43 119.0(17) . . ? C54 N50 C50 114(2) . . ? C54 N50 C52 109(2) . . ? C50 N50 C52 113(2) . . ? C54 N50 C56 106(2) . . ? C50 N50 C56 108(2) . . ? C52 N50 C56 107(2) . . ? N50 C50 C51 113(3) . . ? N50 C50 H50A 108.9 . . ? C51 C50 H50A 108.9 . . ? N50 C50 H50B 108.9 . . ? C51 C50 H50B 108.9 . . ? H50A C50 H50B 107.7 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N50 C52 C53 121(3) . . ? N50 C52 H52A 107.0 . . ? C53 C52 H52A 107.0 . . ? N50 C52 H52B 107.0 . . ? C53 C52 H52B 107.0 . . ? H52A C52 H52B 106.8 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 N50 117(3) . . ? C55 C54 H54A 121.5 . . ? N50 C54 H54A 121.5 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C57 C56 N50 127(3) . . ? C57 C56 H56A 116.3 . . ? N50 C56 H56A 116.3 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C878 N60 C61 89.6(15) . 2 ? C878 N60 C61 89.6(15) . 3 ? C61 N60 C61 120.00(7) 2 3 ? C878 N60 C61 89.6(15) . . ? C61 N60 C61 120.00(7) 2 . ? C61 N60 C61 120.00(8) 3 . ? C878 N60 C63 147.4(15) . . ? C61 N60 C63 112(3) 2 . ? C61 N60 C63 100(4) 3 . ? C61 N60 C63 58.7(9) . . ? C878 N60 C63 147.4(16) . 2 ? C61 N60 C63 58.7(10) 2 2 ? C61 N60 C63 112(3) 3 2 ? C61 N60 C63 100(4) . 2 ? C63 N60 C63 56(3) . 2 ? C878 N60 C63 147.4(15) . 3 ? C61 N60 C63 100(4) 2 3 ? C61 N60 C63 58.7(9) 3 3 ? C61 N60 C63 112(3) . 3 ? C63 N60 C63 56(3) . 3 ? C63 N60 C63 56(3) 2 3 ? C62 C61 C63 115(4) . . ? C62 C61 N60 129(3) . . ? C63 C61 N60 60.9(10) . . ? C62 C61 C786 47(2) . . ? C63 C61 C786 109(4) . . ? N60 C61 C786 84(2) . . ? C62 C61 C878 105(2) . . ? C63 C61 C878 107(2) . . ? N60 C61 C878 46.8(16) . . ? C786 C61 C878 61.7(18) . . ? C786 C62 C61 84(3) . . ? C63 C63 C63 60.000(13) 2 3 ? C63 C63 C61 106(5) 2 . ? C63 C63 C61 120(2) 3 . ? C63 C63 C64 61.9(13) 2 . ? C63 C63 C64 61.9(13) 3 . ? C61 C63 C64 166(7) . . ? C63 C63 N60 62.2(13) 2 . ? C63 C63 N60 62.2(13) 3 . ? C61 C63 N60 60.4(10) . . ? C64 C63 N60 115(3) . . ? C63 C64 C63 56(3) 3 2 ? C63 C64 C63 56(3) 3 . ? C63 C64 C63 56(3) 2 . ? C62 C786 C61 48.4(18) . . ? C62 C786 C878 108(3) . . ? C61 C786 C878 64(2) . . ? N71 N71 N71 60.00(3) 3 2 ? N71 N71 C76 107(3) 3 . ? N71 N71 C76 74(3) 2 . ? N71 N71 C74 127(5) 3 . ? N71 N71 C74 142(3) 2 . ? C76 N71 C74 124(3) . . ? N71 N71 C72 161(3) 3 . ? N71 N71 C72 126(6) 2 . ? C76 N71 C72 62(2) . . ? C74 N71 C72 61.6(11) . . ? N71 N71 C76 70(3) 3 3 ? N71 N71 C76 105(3) 2 3 ? C76 N71 C76 71(3) . 3 ? C74 N71 C76 112(3) . 3 ? C72 N71 C76 91(3) . 3 ? N71 C72 C74 58.2(10) . . ? N71 C72 C73 113.3(19) . . ? C74 C72 C73 110(4) . . ? N71 C74 C75 117(2) . . ? N71 C74 C72 60.2(10) . . ? C75 C74 C72 106(4) . . ? N71 C76 C76 74.2(17) . 2 ? N71 C76 C76 53(2) 2 2 ? N71 C76 C76 55.2(19) . 3 ? N71 C76 C76 73.4(17) 2 3 ? C76 C76 C76 60.000(11) 2 3 ? C42 N04 C41 128.9(13) . 2 ? C42 N04 H04B 115.5 . . ? C41 N04 H04B 115.5 2 . ? N60 C878 C786 77(2) . 3 ? N60 C878 C786 77(2) . 2 ? C786 C878 C786 114.9(18) 3 2 ? N60 C878 C786 77(2) . . ? C786 C878 C786 114.9(18) 3 . ? C786 C878 C786 114.9(18) 2 . ? C786 C878 C61 54.2(19) 2 2 ? C786 C878 C61 120(4) . 2 ? C786 C878 C61 54.2(19) 3 3 ? C786 C878 C61 120(4) 2 3 ? C786 C878 C61 66(2) . 3 ? C61 C878 C61 73(2) 2 3 ? N60 C878 C61 43.6(14) . . ? C786 C878 C61 120(4) 3 . ? C786 C878 C61 66(2) 2 . ? C786 C878 C61 54.2(19) . . ? C61 C878 C61 73(2) 2 . ? C61 C878 C61 73(2) 3 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O02 Ti1 O01 C01 59.6(19) 3 . . . ? O02 Ti1 O01 C01 -81.9(8) 2 . . . ? O02 Ti1 O01 C01 7.6(8) . . . . ? O01 Ti1 O01 C01 -162.3(8) 2 . . . ? O01 Ti1 O01 C01 107.3(9) 3 . . . ? O02 Ti1 O02 C02 -175.1(9) 3 . . . ? O02 Ti1 O02 C02 93.9(10) 2 . . . ? O01 Ti1 O02 C02 -5.7(8) . . . . ? O01 Ti1 O02 C02 43(2) 2 . . . ? O01 Ti1 O02 C02 -94.5(9) 3 . . . ? O08 Ti2 O05 C23 100.0(11) . . . . ? O12 Ti2 O05 C23 -85.6(11) . . . . ? O11 Ti2 O05 C23 -165.5(11) . . . . ? O07 Ti2 O05 C23 64(2) . . . . ? O06 Ti2 O05 C23 0.8(10) . . . . ? O08 Ti2 O06 C24 -88.0(8) . . . . ? O05 Ti2 O06 C24 1.7(8) . . . . ? O12 Ti2 O06 C24 98.9(8) . . . . ? O11 Ti2 O06 C24 62.1(16) . . . . ? O07 Ti2 O06 C24 -169.3(8) . . . . ? O08 Ti2 O07 C25 5.9(8) . . . . ? O05 Ti2 O07 C25 42(2) . . . . ? O12 Ti2 O07 C25 -167.7(8) . . . . ? O11 Ti2 O07 C25 -87.7(9) . . . . ? O06 Ti2 O07 C25 104.7(8) . . . . ? O05 Ti2 O08 C26 -177.2(10) . . . . ? O11 Ti2 O08 C26 92.1(10) . . . . ? O07 Ti2 O08 C26 -3.1(10) . . . . ? O06 Ti2 O08 C26 -95.8(10) . . . . ? O08 Ti2 O11 C47 -172.6(11) . . . . ? O05 Ti2 O11 C47 96.3(11) . . . . ? O12 Ti2 O11 C47 -0.5(11) . . . . ? O07 Ti2 O11 C47 -91.4(11) . . . . ? O06 Ti2 O11 C47 37.0(19) . . . . ? O05 Ti2 O12 C48 -83.4(9) . . . . ? O11 Ti2 O12 C48 6.1(9) . . . . ? O07 Ti2 O12 C48 101.7(9) . . . . ? O06 Ti2 O12 C48 -164.3(9) . . . . ? Ti1 O01 C01 C06 171.5(11) . . . . ? Ti1 O01 C01 C02 -7.9(14) . . . . ? Ti1 O02 C02 C01 3.2(15) . . . . ? Ti1 O02 C02 C03 -172.2(12) . . . . ? O01 C01 C02 O02 3.2(17) . . . . ? C06 C01 C02 O02 -176.2(11) . . . . ? O01 C01 C02 C03 178.7(12) . . . . ? C06 C01 C02 C03 -1(2) . . . . ? O02 C02 C03 C04 175.8(14) . . . . ? C01 C02 C03 C04 1(2) . . . . ? C02 C03 C04 C05 -2(2) . . . . ? C03 C04 C05 C06 4(2) . . . . ? C04 C05 C06 C01 -4(2) . . . . ? C04 C05 C06 C07 177.7(13) . . . . ? O01 C01 C06 C05 -177.0(13) . . . . ? C02 C01 C06 C05 2.3(19) . . . . ? O01 C01 C06 C07 1(2) . . . . ? C02 C01 C06 C07 -179.3(13) . . . . ? Ti2 O07 C25 C26 -7.2(14) . . . . ? Ti2 O07 C25 C30 172.4(11) . . . . ? C30 C25 C26 C27 1(2) . . . . ? O07 C25 C26 O08 4.7(18) . . . . ? C30 C25 C26 O08 -175.0(12) . . . . ? Ti2 O08 C26 C27 -175.1(12) . . . . ? Ti2 O08 C26 C25 0.1(17) . . . . ? C25 C26 C27 C28 5(2) . . . . ? C26 C27 C28 C29 -6(2) . . . . ? C27 C28 C29 C30 3(2) . . . . ? O07 C25 C30 C31 -9(2) . . . . ? C26 C25 C30 C31 170.3(14) . . . . ? O07 C25 C30 C29 176.5(12) . . . . ? C26 C25 C30 C29 -4(2) . . . . ? C28 C29 C30 C25 2(2) . . . . ? C28 C29 C30 C31 -172.5(13) . . . . ? C48 C43 C44 C45 -3(3) . . . . ? C42 C43 C44 C45 -176.7(18) . . . . ? C43 C44 C45 C46 3(3) . . . . ? C44 C45 C46 C47 -3(3) . . . . ? Ti2 O11 C47 C48 -5.2(19) . . . . ? Ti2 O11 C47 C46 -178.1(14) . . . . ? C45 C46 C47 O11 175.4(17) . . . . ? C45 C46 C47 C48 2(3) . . . . ? C42 C43 C48 O12 -10(3) . . . . ? C44 C43 C48 O12 175.9(15) . . . . ? C42 C43 C48 C47 176.1(15) . . . . ? C44 C43 C48 C47 2(3) . . . . ? Ti2 O12 C48 C43 175.7(12) . . . . ? Ti2 O12 C48 C47 -10.1(16) . . . . ? O11 C47 C48 C43 -175.7(15) . . . . ? C46 C47 C48 C43 -2(3) . . . . ? O11 C47 C48 O12 10(2) . . . . ? C46 C47 C48 O12 -176.6(14) . . . . ? C18 C19 C20 C21 -178.1(13) . . . . ? C24 C19 C20 C21 2(2) . . . . ? C19 C20 C21 C22 -2(3) . . . . ? C20 C21 C22 C23 0(3) . . . . ? Ti2 O05 C23 C24 -3.2(17) . . . . ? C21 C22 C23 O05 178.6(15) . . . . ? Ti2 O06 C24 C23 -3.7(13) . . . . ? O05 C23 C24 O06 4.6(18) . . . . ? C22 C23 C24 C19 -3(2) . . . . ? C18 C19 C24 O06 -4(2) . . . . ? C20 C19 C24 O06 176.6(12) . . . . ? C20 C19 C24 C23 1(2) . . . . ? C08 N01 C07 O03 0(2) . . . . ? C08 N01 C07 C06 -175.1(11) . . . . ? C05 C06 C07 N01 177.4(12) . . . . ? C01 C06 C07 N01 -1(2) . . . . ? C05 C06 C07 O03 2(2) . . . . ? C01 C06 C07 O03 -176.0(14) . . . . ? C07 N01 C08 C13 143.4(14) . . . . ? C07 N01 C08 C09 -41.7(19) . . . . ? C13 C08 C09 C10 -7.0(19) . . . . ? N01 C08 C09 C10 178.0(11) . . . . ? C08 C09 C10 C11 4(2) . . . . ? C09 C10 C11 C12 -1(2) . . . . ? C10 C11 C12 C13 2.3(18) . . . . ? C10 C11 C12 C17 179.0(12) . . . . ? C11 C12 C13 C08 -5.8(18) . . . . ? C17 C12 C13 C08 177.6(12) . . . . ? C11 C12 C13 C14 -179.0(12) . . . . ? C17 C12 C13 C14 4.4(19) . . . . ? C09 C08 C13 C12 8.2(18) . . . . ? N01 C08 C13 C12 -177.0(11) . . . . ? C09 C08 C13 C14 -178.6(13) . . . . ? N01 C08 C13 C14 -3.8(19) . . . . ? C12 C13 C14 C15 -4(2) . . . . ? C08 C13 C14 C15 -177.1(13) . . . . ? C13 C14 C15 C16 1(3) . . . . ? C14 C15 C16 C17 1(3) . . . . ? C18 N02 C17 C16 -6(2) . . . . ? C18 N02 C17 C12 165.2(13) . . . . ? C15 C16 C17 N02 170.6(13) . . . . ? C15 C16 C17 C12 0(2) . . . . ? C13 C12 C17 N02 -173.2(11) . . . . ? C11 C12 C17 N02 10.1(18) . . . . ? C13 C12 C17 C16 -2.4(19) . . . . ? C11 C12 C17 C16 -179.0(13) . . . . ? C17 N02 C18 O04 5(2) . . . . ? C17 N02 C18 C19 -171.2(12) . . . . ? C24 C19 C18 O04 -176.6(13) . . . . ? C20 C19 C18 O04 3(2) . . . . ? C24 C19 C18 N02 0(2) . . . . ? C32 N03 C31 O09 8(2) . . . . ? C32 N03 C31 C30 -176.5(12) . . . . ? C25 C30 C31 O09 169.9(13) . . . . ? C29 C30 C31 O09 -15.6(19) . . . . ? C25 C30 C31 N03 -5(2) . . . . ? C29 C30 C31 N03 169.4(12) . . . . ? C31 N03 C32 C37 -166.8(13) . . . . ? C31 N03 C32 C33 19(2) . . . . ? C37 C32 C33 C34 4(2) . . . . ? N03 C32 C33 C34 178.2(12) . . . . ? C32 C33 C34 C35 -5(2) . . . . ? C33 C34 C35 C36 4(2) . . . . ? C34 C35 C36 C41 -176.2(15) . . . . ? C34 C35 C36 C37 -3(2) . . . . ? N03 C32 C37 C36 -176.9(11) . . . . ? C33 C32 C37 C36 -3.0(19) . . . . ? N03 C32 C37 C38 0.6(18) . . . . ? C33 C32 C37 C38 174.4(13) . . . . ? C41 C36 C37 C32 175.6(12) . . . . ? C35 C36 C37 C32 2.1(19) . . . . ? C41 C36 C37 C38 -1.9(19) . . . . ? C35 C36 C37 C38 -175.4(13) . . . . ? C36 C37 C38 C39 -1.4(19) . . . . ? C37 C38 C39 C40 3(2) . . . . ? C38 C39 C40 C41 -1(2) . . . . ? C37 C36 C41 C40 3(2) . . . . ? C35 C36 C41 C40 177.0(14) . . . . ? C37 C36 C41 N04 176.7(11) . . . 3 ? C35 C36 C41 N04 -10(2) . . . 3 ? C39 C40 C41 C36 -2(2) . . . . ? C39 C40 C41 N04 -175.5(13) . . . 3 ? C48 C43 C42 O10 -177.2(16) . . . . ? C44 C43 C42 O10 -4(3) . . . . ? C48 C43 C42 N04 2(2) . . . . ? C44 C43 C42 N04 175.9(16) . . . . ? C54 N50 C50 C51 -174(3) . . . . ? C52 N50 C50 C51 60(3) . . . . ? C56 N50 C50 C51 -57(3) . . . . ? C54 N50 C52 C53 -62(4) . . . . ? C50 N50 C52 C53 66(4) . . . . ? C56 N50 C52 C53 -176(3) . . . . ? C50 N50 C54 C55 171(3) . . . . ? C52 N50 C54 C55 -62(3) . . . . ? C56 N50 C54 C55 53(3) . . . . ? C54 N50 C56 C57 73(4) . . . . ? C50 N50 C56 C57 -49(4) . . . . ? C52 N50 C56 C57 -170(3) . . . . ? C878 N60 C61 C62 72(3) . . . . ? C61 N60 C61 C62 161(2) 2 . . . ? C61 N60 C61 C62 -17(6) 3 . . . ? C63 N60 C61 C62 -100(5) . . . . ? C63 N60 C61 C62 -139(3) 2 . . . ? C63 N60 C61 C62 -83(5) 3 . . . ? C878 N60 C61 C63 172(4) . . . . ? C61 N60 C61 C63 -99(4) 2 . . . ? C61 N60 C61 C63 83(5) 3 . . . ? C63 N60 C61 C63 -39(6) 2 . . . ? C63 N60 C61 C63 17(6) 3 . . . ? C878 N60 C61 C786 56.1(16) . . . . ? C61 N60 C61 C786 145(3) 2 . . . ? C61 N60 C61 C786 -33(3) 3 . . . ? C63 N60 C61 C786 -116(4) . . . . ? C63 N60 C61 C786 -155(2) 2 . . . ? C63 N60 C61 C786 -99(3) 3 . . . ? C61 N60 C61 C878 89(3) 2 . . . ? C61 N60 C61 C878 -89(3) 3 . . . ? C63 N60 C61 C878 -172(4) . . . . ? C63 N60 C61 C878 149(2) 2 . . . ? C63 N60 C61 C878 -155(3) 3 . . . ? C63 C61 C62 C786 -94(4) . . . . ? N60 C61 C62 C786 -22(4) . . . . ? C878 C61 C62 C786 24(3) . . . . ? C62 C61 C63 C63 167(6) . . . 2 ? N60 C61 C63 C63 44(5) . . . 2 ? C786 C61 C63 C63 115(7) . . . 2 ? C878 C61 C63 C63 50(8) . . . 2 ? C62 C61 C63 C63 102(8) . . . 3 ? N60 C61 C63 C63 -20(8) . . . 3 ? C786 C61 C63 C63 51(10) . . . 3 ? C878 C61 C63 C63 -14(11) . . . 3 ? C62 C61 C63 C64 -165(15) . . . . ? N60 C61 C63 C64 72(15) . . . . ? C62 C61 C63 N60 122(3) . . . . ? C786 C61 C63 N60 71(3) . . . . ? C878 C61 C63 N60 6(3) . . . . ? C878 N60 C63 C63 -145.6(4) . . . 2 ? C61 N60 C63 C63 110(6) 3 . . 2 ? C61 N60 C63 C63 -131(8) . . . 2 ? C63 N60 C63 C63 68.8(9) 3 . . 2 ? C878 N60 C63 C63 145.6(4) . . . 3 ? C61 N60 C63 C63 -87(7) 2 . . 3 ? C61 N60 C63 C63 41(6) 3 . . 3 ? C61 N60 C63 C63 160(8) . . . 3 ? C63 N60 C63 C63 -68.8(9) 2 . . 3 ? C878 N60 C63 C61 -15(8) . . . . ? C61 N60 C63 C61 112.8(17) 2 . . . ? C61 N60 C63 C61 -119(2) 3 . . . ? C63 N60 C63 C61 131(8) 2 . . . ? C63 N60 C63 C61 -160(8) 3 . . . ? C61 N60 C63 C64 -52(7) 2 . . . ? C61 N60 C63 C64 75(6) 3 . . . ? C61 N60 C63 C64 -165(8) . . . . ? C63 N60 C63 C64 -34.4(5) 2 . . . ? C63 N60 C63 C64 34.4(5) 3 . . . ? C63 C63 C64 C63 -69.0(10) 2 . . 3 ? N60 C63 C64 C63 -34.5(5) . . . 3 ? C63 C63 C64 C63 69.0(10) 3 . . 2 ? C61 C63 C64 C63 -31(13) . . . 2 ? N60 C63 C64 C63 34.5(5) . . . 2 ? C61 C62 C786 C878 -25(4) . . . . ? C63 C61 C786 C62 107(4) . . . . ? N60 C61 C786 C62 163(3) . . . . ? C878 C61 C786 C62 -153(4) . . . . ? C62 C61 C786 C878 153(4) . . . . ? C63 C61 C786 C878 -100(2) . . . . ? N60 C61 C786 C878 -43.4(18) . . . . ? C76 N71 C72 C74 177(3) . . . . ? C76 N71 C72 C74 -115(3) 3 . . . ? C76 N71 C72 C73 77(5) . . . . ? C74 N71 C72 C73 -100(5) . . . . ? C76 N71 C72 C73 145(5) 3 . . . ? C76 N71 C74 C75 -97(4) . . . . ? C72 N71 C74 C75 -94(5) . . . . ? C76 N71 C74 C75 -16(6) 3 . . . ? C76 N71 C74 C72 -3(3) . . . . ? C76 N71 C74 C72 78(4) 3 . . . ? C73 C72 C74 N71 105(3) . . . . ? N71 C72 C74 C75 112(3) . . . . ? C73 C72 C74 C75 -143(3) . . . . ? C74 N71 C76 N71 -143(6) . . . 2 ? O10 C42 N04 C41 -5(2) . . . 2 ? C43 C42 N04 C41 175.7(12) . . . 2 ? C61 N60 C878 C786 68.6(19) 2 . . 3 ? C61 N60 C878 C786 -51.4(19) 3 . . 3 ? C61 N60 C878 C786 -171.4(19) . . . 3 ? C63 N60 C878 C786 -159(7) . . . 3 ? C63 N60 C878 C786 81(7) 2 . . 3 ? C63 N60 C878 C786 -39(7) 3 . . 3 ? C61 N60 C878 C786 -51.4(18) 2 . . 2 ? C61 N60 C878 C786 -171.4(18) 3 . . 2 ? C61 N60 C878 C786 68.6(18) . . . 2 ? C63 N60 C878 C786 81(7) . . . 2 ? C63 N60 C878 C786 -39(7) 2 . . 2 ? C63 N60 C878 C786 -159(7) 3 . . 2 ? C61 N60 C878 C786 -171.4(18) 2 . . . ? C61 N60 C878 C786 68.6(18) 3 . . . ? C61 N60 C878 C786 -51.4(18) . . . . ? C63 N60 C878 C786 -39(7) . . . . ? C63 N60 C878 C786 -159(7) 2 . . . ? C63 N60 C878 C786 81(7) 3 . . . ? C61 N60 C878 C61 -120.000(2) 3 . . 2 ? C61 N60 C878 C61 120.000(1) . . . 2 ? C63 N60 C878 C61 133(7) . . . 2 ? C63 N60 C878 C61 13(7) 2 . . 2 ? C63 N60 C878 C61 -107(7) 3 . . 2 ? C61 N60 C878 C61 120.000(6) 2 . . 3 ? C61 N60 C878 C61 -120.000(4) . . . 3 ? C63 N60 C878 C61 -107(7) . . . 3 ? C63 N60 C878 C61 133(7) 2 . . 3 ? C63 N60 C878 C61 13(7) 3 . . 3 ? C61 N60 C878 C61 -120.000(16) 2 . . . ? C61 N60 C878 C61 120.000(15) 3 . . . ? C63 N60 C878 C61 13(7) . . . . ? C63 N60 C878 C61 -107(7) 2 . . . ? C63 N60 C878 C61 133(7) 3 . . . ? C62 C786 C878 N60 62(3) . . . . ? C61 C786 C878 N60 41.6(13) . . . . ? C62 C786 C878 C786 131(3) . . . 3 ? C61 C786 C878 C786 110(4) . . . 3 ? C62 C786 C878 C786 -6(6) . . . 2 ? C61 C786 C878 C786 -27(4) . . . 2 ? C62 C786 C878 C61 55(4) . . . 2 ? C61 C786 C878 C61 35(2) . . . 2 ? C62 C786 C878 C61 107(3) . . . 3 ? C61 C786 C878 C61 86(2) . . . 3 ? C62 C786 C878 C61 21(3) . . . . ? C62 C61 C878 N60 -130(3) . . . . ? C63 C61 C878 N60 -7(4) . . . . ? C786 C61 C878 N60 -110(2) . . . . ? C62 C61 C878 C786 -121(3) . . . 3 ? C63 C61 C878 C786 2(5) . . . 3 ? N60 C61 C878 C786 10(2) . . . 3 ? C786 C61 C878 C786 -100.6(12) . . . 3 ? C62 C61 C878 C786 134(3) . . . 2 ? C63 C61 C878 C786 -103(5) . . . 2 ? N60 C61 C878 C786 -96(2) . . . 2 ? C786 C61 C878 C786 153(3) . . . 2 ? C62 C61 C878 C786 -20(3) . . . . ? C63 C61 C878 C786 103(4) . . . . ? N60 C61 C878 C786 110(2) . . . . ? C62 C61 C878 C61 -169(3) . . . 2 ? C63 C61 C878 C61 -46(4) . . . 2 ? N60 C61 C878 C61 -38.6(7) . . . 2 ? C786 C61 C878 C61 -149(2) . . . 2 ? C62 C61 C878 C61 -92(3) . . . 3 ? C63 C61 C878 C61 31(4) . . . 3 ? N60 C61 C878 C61 38.6(7) . . . 3 ? C786 C61 C878 C61 -72(2) . . . 3 ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 19.32 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.836 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.113 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 972 227 ' ' 2 -0.333 0.333 0.083 1423 316 ' ' 3 0.333 0.667 0.167 975 228 ' ' 4 0.000 1.000 0.250 1422 315 ' ' 5 -0.333 0.333 0.333 975 228 ' ' 6 0.333 0.667 0.417 1422 316 ' ' 7 0.000 0.000 0.500 972 227 ' ' 8 -0.333 0.333 0.583 1423 316 ' ' 9 0.333 0.667 0.667 975 228 ' ' 10 0.000 0.000 0.750 1422 315 ' ' 11 -0.333 0.333 0.833 975 228 ' ' 12 0.333 0.667 0.917 1422 316 ' ' _platon_squeeze_details ; ; #===END data_Structure4 _publ_requested_journal ; test ; _publ_contact_author ; Kenneth N. Raymond Department of Chemistry University of California Berkeley, CA 94720-1460 ; _publ_contact_author_phone '510-642-7219' _publ_contact_author_fax '510-486-5283' _publ_contact_author_email 'raymond@socrates.berkeley.edu' loop_ _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, M., Giacovazzo, C., Guagliardi, A., Polidori, G. (1993). J. Appl. Cryst., 26, 343-350. Siemens Industrial Automation, Inc. (1995). SMART. Area Detector Software Package, Madison, WI, USA. Siemens Industrial Automation, Inc. (1995). SAINT. SAX Area Detector Integration Program (v. 4.024), Madison, WI, USA. Siemens Industrial Automation, Inc. (1993). SHELXL. SHELXTL Crystal Structure Determination Software Package, Madison, WI, USA. ; _audit_creation_method SHELXL _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement ; SMART (Siemens, 1995), SAINT (Siemens, 1995) ; _computing_data_reduction ; SAINT (Siemens, 1995), XPREP (Siemens, 1995) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------- _chemical_formula_sum 'C293 H265 Ga4 N27.50 O41.50' _chemical_formula_weight 5114.21 _chemical_compound_source synthetic loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ga' 'Ga' 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 26.7393(6) _cell_length_b 30.8317(2) _cell_length_c 38.5228(8) _cell_angle_alpha 90.00 _cell_angle_beta 109.8530(10) _cell_angle_gamma 90.00 _cell_volume 29871.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.55 _cell_measurement_theta_max 19.79 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour orange _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10686 _exptl_absorpt_coefficient_mu 0.426 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo Kalpha' _diffrn_radiation_source 'fine focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w-scans' _diffrn_reflns_number 71416 _diffrn_reflns_av_R_equivalents 0.0887 _diffrn_reflns_av_sigmaI/netI 0.1177 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 19.79 _reflns_number_total 26393 _reflns_number_observed 14441 _reflns_observed_criterion >2sigma(I) _refine_special_details ; Refinement on F^2^ for ALL reflections except for 22 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All Ga atoms were refined anisotropically. Hydrogen atoms were included, but not refined on all appropriate cluster atoms, ordered solvent and counterions. Final formula: (NMe3Bn)12[Ga4L6]*3.5DMF*1.5acetone*x(solvent) The large final maximum shift/esd corresponds to a thermal parameter of a partial occupancy carbon atom that is represented as "x(solvent)" in the chemical formula. This atoms is refined in the final block, 8, along with all other disordered solvent, counterions and the four metal centers. this large shift/esd could not be reduced even after 80 least squares cycles and is reported as is since these disordered solvent atoms have little bearing on the overall connectivity of the tetrahedral cluster. One batch (3) of the four batches collected had an anomalously large Rint so it was removed in Saint. This resulted in a significant lowering of the Rint for the merged data set. There is no obvious reason for this batch being bad, however. In addition, the possibility of the crystal being twinned in C2/c was investigated with a mathematically twinning law. After a least squares cycle it was determined that this twin could not be real. The likely reason for the reflections with large Fobs when Fcalc is near zero is that the crystal had a small "friend" contributing to the data. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.2418P)^2^+247.1206P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 26371 _refine_ls_number_parameters 1634 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.2046 _refine_ls_R_factor_obs 0.1238 _refine_ls_wR_factor_all 0.4101 _refine_ls_wR_factor_obs 0.3126 _refine_ls_goodness_of_fit_all 1.032 _refine_ls_goodness_of_fit_obs 1.067 _refine_ls_restrained_S_all 1.036 _refine_ls_restrained_S_obs 1.065 _refine_ls_shift/esd_max 5.647 _refine_ls_shift/esd_mean 0.081 _refine_diff_density_max 1.162 _refine_diff_density_min -1.611 _refine_diff_density_rms 0.151 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ga1 Ga -0.01932(7) 0.45966(5) 0.39375(4) 0.0373(5) Uani 1 d . . Ga2 Ga -0.33741(6) 0.47962(5) 0.05691(4) 0.0344(5) Uani 1 d . . Ga3 Ga -0.13059(7) 0.82058(5) 0.23518(4) 0.0390(5) Uani 1 d . . Ga4 Ga 0.15457(7) 0.55307(6) 0.13379(4) 0.0483(5) Uani 1 d . . O1 O 0.0491(4) 0.4442(3) 0.4310(3) 0.040(3) Uiso 1 d . . O2 O 0.0204(4) 0.5133(3) 0.3898(3) 0.039(2) Uiso 1 d . . O3 O 0.1223(4) 0.6222(3) 0.4116(3) 0.059(3) Uiso 1 d . . O4 O -0.2341(4) 0.6756(3) 0.2967(3) 0.061(3) Uiso 1 d . . O5 O -0.2023(4) 0.8425(3) 0.2283(2) 0.039(2) Uiso 1 d . . O6 O -0.1552(4) 0.7702(3) 0.2567(2) 0.037(2) Uiso 1 d . . O7 O -0.0483(4) 0.4032(3) 0.4000(3) 0.041(3) Uiso 1 d . . O8 O -0.0041(3) 0.4302(3) 0.3522(2) 0.035(2) Uiso 1 d . . O9 O 0.0198(4) 0.3435(3) 0.2752(3) 0.061(3) Uiso 1 d . . O10 O 0.2172(5) 0.5925(4) 0.2988(4) 0.085(4) Uiso 1 d . . O11 O 0.1607(4) 0.5674(3) 0.1853(3) 0.043(3) Uiso 1 d . . O12 O 0.2110(4) 0.5967(3) 0.1418(3) 0.055(3) Uiso 1 d . . O13 O -0.0473(4) 0.4840(3) 0.4302(2) 0.037(2) Uiso 1 d . . O14 O -0.0881(4) 0.4823(3) 0.3582(2) 0.037(2) Uiso 1 d . . O15 O -0.2482(4) 0.5177(3) 0.3054(3) 0.048(3) Uiso 1 d . . O16 O -0.1627(4) 0.3465(3) 0.1371(3) 0.051(3) Uiso 1 d . . O17 O -0.2785(3) 0.4425(3) 0.0891(2) 0.033(2) Uiso 1 d . . O18 O -0.3320(4) 0.4400(3) 0.0184(3) 0.040(2) Uiso 1 d . . O19 O -0.3882(4) 0.5166(3) 0.0198(2) 0.036(2) Uiso 1 d . . O20 O -0.2846(3) 0.5209(3) 0.0495(2) 0.034(2) Uiso 1 d . . O21 O -0.1928(4) 0.5933(3) 0.0011(3) 0.050(3) Uiso 1 d . . O22 O 0.0317(4) 0.3842(3) 0.1347(3) 0.062(3) Uiso 1 d . . O23 O 0.1056(4) 0.5041(3) 0.1341(3) 0.043(3) Uiso 1 d . . O24 O 0.2085(4) 0.5080(3) 0.1485(3) 0.053(3) Uiso 1 d . . O27 O -0.3933(4) 0.4450(3) 0.0653(2) 0.037(2) Uiso 1 d . . O28 O -0.3442(3) 0.5138(3) 0.0991(2) 0.033(2) Uiso 1 d . . O29 O -0.4043(4) 0.5845(3) 0.1701(3) 0.051(3) Uiso 1 d . . O30 O -0.1992(5) 0.7547(4) 0.0744(3) 0.072(3) Uiso 1 d . . O31 O -0.1537(4) 0.7905(3) 0.1859(3) 0.039(2) Uiso 1 d . . O32 O -0.1117(4) 0.8677(3) 0.2076(3) 0.042(3) Uiso 1 d . . O33 O -0.1007(4) 0.8535(3) 0.2813(3) 0.041(3) Uiso 1 d . . O34 O -0.0587(4) 0.7927(3) 0.2512(3) 0.042(3) Uiso 1 d . . O35 O 0.0972(5) 0.7500(4) 0.3065(3) 0.072(3) Uiso 1 d . . O36 O 0.0056(5) 0.7011(4) 0.0574(4) 0.081(4) Uiso 1 d . . O37 O 0.0958(4) 0.5949(3) 0.1141(3) 0.046(3) Uiso 1 d . . O38 O 0.1467(4) 0.5466(3) 0.0812(3) 0.048(3) Uiso 1 d . . O100 O 0.2768(7) 0.2677(6) 0.1302(5) 0.134(6) Uiso 1 d . . O101 O 0.0704(5) 0.7154(4) 0.4796(4) 0.090(4) Uiso 1 d . . O102 O 0.0744(8) 0.1124(6) 0.3839(6) 0.141(6) Uiso 1 d . . O103 O 0.2086(13) 0.2346(10) 0.0201(8) 0.082(8) Uiso 0.50 d P . O104 O -0.2913(10) 0.6001(8) 0.2896(8) 0.200(10) Uiso 1 d . . O106 O 0.2553(25) 0.2954(19) -0.0028(17) 0.210(29) Uiso 0.50 d P . O107 O -0.3550(16) 0.1519(13) -0.0733(12) 0.157(14) Uiso 0.50 d P . N1 N 0.0402(4) 0.5964(3) 0.3797(3) 0.036(3) Uiso 1 d . . H1A H 0.0221(4) 0.5727(3) 0.3741(3) 0.043 Uiso 1 calc R . N2 N -0.1580(5) 0.6966(4) 0.2878(3) 0.041(3) Uiso 1 d . . H2A H -0.1433(5) 0.7174(4) 0.2799(3) 0.049 Uiso 1 calc R . N3 N 0.0357(5) 0.4116(4) 0.2991(3) 0.044(3) Uiso 1 d . . H3A H 0.0273(5) 0.4290(4) 0.3136(3) 0.053 Uiso 1 calc R . N4 N 0.1581(5) 0.5554(4) 0.2520(4) 0.050(3) Uiso 1 d . . H4A H 0.1495(5) 0.5484(4) 0.2291(4) 0.060 Uiso 1 calc R . N5 N -0.1736(4) 0.4897(3) 0.2981(3) 0.035(3) Uiso 1 d . . H5A H -0.1419(4) 0.4807(3) 0.3097(3) 0.042 Uiso 1 calc R . N6 N -0.2053(4) 0.4069(3) 0.1467(3) 0.035(3) Uiso 1 d . . H6A H -0.2283(4) 0.4262(3) 0.1354(3) 0.041 Uiso 1 calc R . N7 N -0.1942(4) 0.5474(3) 0.0465(3) 0.038(3) Uiso 1 d . . H7A H -0.2138(4) 0.5323(3) 0.0556(3) 0.045 Uiso 1 calc R . N8 N 0.0199(5) 0.4558(4) 0.1212(3) 0.040(3) Uiso 1 d . . H8A H 0.0366(5) 0.4801(4) 0.1243(3) 0.048 Uiso 1 calc R . N9 N -0.3432(4) 0.5826(3) 0.1411(3) 0.038(3) Uiso 1 d . . H9A H -0.3321(4) 0.5668(3) 0.1268(3) 0.046 Uiso 1 calc R . N10 N -0.2009(5) 0.7360(4) 0.1316(3) 0.047(3) Uiso 1 d . . H10A H -0.1930(5) 0.7445(4) 0.1541(3) 0.056 Uiso 1 calc R . N11 N 0.0249(5) 0.7454(4) 0.2549(3) 0.045(3) Uiso 1 d . . H11A H -0.0077(5) 0.7533(4) 0.2451(3) 0.054 Uiso 1 calc R . N12 N 0.0371(5) 0.6657(4) 0.1118(3) 0.042(3) Uiso 1 d . . H12A H 0.0547(5) 0.6432(4) 0.1225(3) 0.051 Uiso 1 calc R . N13 N 0.0856(5) 0.4351(4) 0.0309(4) 0.056(4) Uiso 1 d . . N14 N 0.2710(6) 0.1493(5) 0.1213(4) 0.068(4) Uiso 1 d . . N15 N -0.0992(5) 0.6297(4) 0.2015(4) 0.059(4) Uiso 1 d . . N16 N -0.2059(5) 0.3755(4) 0.3657(3) 0.043(3) Uiso 1 d . . N17 N -0.0275(5) 0.3102(4) 0.1796(4) 0.058(4) Uiso 1 d . . N18 N -0.3407(5) 0.3321(4) 0.1404(3) 0.046(3) Uiso 1 d . . N19 N 0.2906(5) 0.5310(4) 0.0774(3) 0.044(3) Uiso 1 d . . N20 N 0.2211(12) 0.3503(10) 0.5180(8) 0.172(10) Uiso 1 d . . N21 N 0.0154(4) 0.0840(3) 0.4644(3) 0.036(3) Uiso 1 d . . N22 N -0.3707(5) 0.4720(4) 0.2502(3) 0.045(3) Uiso 1 d . . N23 N 0.0117(5) 0.6014(4) 0.4903(3) 0.045(3) Uiso 1 d . . N24 N -0.2936(9) 0.0632(7) -0.0977(7) 0.142(8) Uiso 1 d . . N100 N 0.3103(7) 0.3309(6) 0.1554(5) 0.092(5) Uiso 1 d . . N101 N 0.1107(7) 0.7503(6) 0.4446(5) 0.086(5) Uiso 1 d . . N102 N 0.0466(8) 0.1069(6) 0.3226(6) 0.101(6) Uiso 1 d . . N103 N 0.1342(27) 0.2725(20) -0.0196(18) 0.166(24) Uiso 0.50 d P . C1 C 0.0832(6) 0.4760(5) 0.4386(4) 0.043(4) Uiso 1 d . . C2 C 0.0686(6) 0.5147(4) 0.4159(4) 0.036(4) Uiso 1 d . . C3 C 0.1028(6) 0.5510(4) 0.4229(4) 0.040(4) Uiso 1 d . . C4 C 0.1517(6) 0.5478(5) 0.4525(4) 0.046(4) Uiso 1 d . . H4B H 0.1744(6) 0.5716(5) 0.4580(4) 0.055 Uiso 1 calc R . C5 C 0.1671(7) 0.5105(6) 0.4735(5) 0.069(5) Uiso 1 d . . H5B H 0.2000(7) 0.5090(6) 0.4922(5) 0.083 Uiso 1 calc R . C6 C 0.1324(6) 0.4755(5) 0.4661(5) 0.055(5) Uiso 1 d . . H6B H 0.1428(6) 0.4505(5) 0.4803(5) 0.066 Uiso 1 calc R . C7 C 0.0897(6) 0.5914(5) 0.4043(4) 0.042(4) Uiso 1 d . . C8 C 0.0128(6) 0.6338(4) 0.3615(4) 0.036(4) Uiso 1 d . . C9 C -0.0397(6) 0.6271(4) 0.3381(4) 0.037(4) Uiso 1 d . . C10 C -0.0633(6) 0.5866(5) 0.3277(4) 0.042(4) Uiso 1 d . . H10B H -0.0429(6) 0.5618(5) 0.3359(4) 0.050 Uiso 1 calc R . C11 C -0.1145(6) 0.5821(5) 0.3061(4) 0.046(4) Uiso 1 d . . H11B H -0.1289(6) 0.5546(5) 0.3000(4) 0.055 Uiso 1 calc R . C12 C -0.1466(6) 0.6192(5) 0.2927(4) 0.046(4) Uiso 1 d . . H12B H -0.1821(6) 0.6160(5) 0.2780(4) 0.055 Uiso 1 calc R . C13 C -0.1258(6) 0.6586(5) 0.3013(4) 0.049(4) Uiso 1 d . . C14 C -0.0712(6) 0.6650(4) 0.3238(4) 0.041(4) Uiso 1 d . . C15 C -0.0473(6) 0.7065(5) 0.3313(4) 0.045(4) Uiso 1 d . . H15A H -0.0672(6) 0.7311(5) 0.3216(4) 0.054 Uiso 1 calc R . C16 C 0.0033(6) 0.7102(5) 0.3522(4) 0.050(4) Uiso 1 d . . H16A H 0.0187(6) 0.7376(5) 0.3561(4) 0.060 Uiso 1 calc R . C17 C 0.0347(7) 0.6741(5) 0.3687(4) 0.054(5) Uiso 1 d . . H17A H 0.0697(7) 0.6778(5) 0.3841(4) 0.065 Uiso 1 calc R . C18 C -0.2079(6) 0.7030(5) 0.2862(4) 0.047(4) Uiso 1 d . . C19 C -0.2312(6) 0.7450(4) 0.2709(4) 0.038(4) Uiso 1 d . . C20 C -0.2841(6) 0.7538(5) 0.2700(4) 0.042(4) Uiso 1 d . . H20A H -0.3023(6) 0.7337(5) 0.2792(4) 0.051 Uiso 1 calc R . C21 C -0.3074(7) 0.7914(5) 0.2557(4) 0.051(4) Uiso 1 d . . H21A H -0.3418(7) 0.7971(5) 0.2550(4) 0.061 Uiso 1 calc R . C22 C -0.2808(6) 0.8221(5) 0.2417(4) 0.046(4) Uiso 1 d . . H22A H -0.2976(6) 0.8481(5) 0.2322(4) 0.056 Uiso 1 calc R . C23 C -0.2299(6) 0.8144(4) 0.2419(4) 0.039(4) Uiso 1 d . . C24 C -0.2051(5) 0.7750(4) 0.2567(4) 0.030(3) Uiso 1 d . . C25 C -0.0418(6) 0.3736(4) 0.3757(4) 0.037(4) Uiso 1 d . . C26 C -0.0169(6) 0.3890(4) 0.3503(4) 0.039(4) Uiso 1 d . . C27 C -0.0104(6) 0.3593(4) 0.3247(4) 0.038(4) Uiso 1 d . . C28 C -0.0269(6) 0.3169(5) 0.3245(5) 0.055(5) Uiso 1 d . . H28A H -0.0219(6) 0.2976(5) 0.3074(5) 0.067 Uiso 1 calc R . C29 C -0.0501(7) 0.3029(6) 0.3484(5) 0.067(5) Uiso 1 d . . H29A H -0.0619(7) 0.2744(6) 0.3471(5) 0.081 Uiso 1 calc R . C30 C -0.0568(6) 0.3314(5) 0.3759(5) 0.057(5) Uiso 1 d . . H30A H -0.0709(6) 0.3214(5) 0.3934(5) 0.068 Uiso 1 calc R . C31 C 0.0171(6) 0.3719(5) 0.2982(4) 0.044(4) Uiso 1 d . . C32 C 0.0668(6) 0.4302(5) 0.2801(4) 0.043(4) Uiso 1 d . . C33 C 0.0790(6) 0.4743(4) 0.2844(4) 0.037(4) Uiso 1 d . . C34 C 0.0612(6) 0.5018(5) 0.3075(4) 0.045(4) Uiso 1 d . . H34A H 0.0397(6) 0.4907(5) 0.3200(4) 0.054 Uiso 1 calc R . C35 C 0.0754(6) 0.5439(5) 0.3113(5) 0.055(5) Uiso 1 d . . H35A H 0.0629(6) 0.5614(5) 0.3263(5) 0.066 Uiso 1 calc R . C36 C 0.1082(6) 0.5626(5) 0.2936(4) 0.046(4) Uiso 1 d . . H36A H 0.1175(6) 0.5918(5) 0.2971(4) 0.056 Uiso 1 calc R . C37 C 0.1262(6) 0.5376(4) 0.2712(4) 0.037(4) Uiso 1 d . . C38 C 0.1123(6) 0.4933(4) 0.2661(4) 0.041(4) Uiso 1 d . . C39 C 0.1304(6) 0.4655(5) 0.2423(4) 0.053(5) Uiso 1 d . . H39A H 0.1519(6) 0.4770(5) 0.2301(4) 0.064 Uiso 1 calc R . C40 C 0.1167(7) 0.4245(5) 0.2379(5) 0.062(5) Uiso 1 d . . H40A H 0.1276(7) 0.4078(5) 0.2216(5) 0.074 Uiso 1 calc R . C41 C 0.0855(6) 0.4046(5) 0.2573(4) 0.055(5) Uiso 1 d . . H41A H 0.0778(6) 0.3751(5) 0.2546(4) 0.066 Uiso 1 calc R . C42 C 0.1989(7) 0.5813(5) 0.2648(5) 0.061(5) Uiso 1 d . . C43 C 0.2245(7) 0.5989(5) 0.2392(5) 0.056(5) Uiso 1 d . . C44 C 0.2717(8) 0.6227(6) 0.2539(6) 0.079(6) Uiso 1 d . . H44A H 0.2854(8) 0.6279(6) 0.2792(6) 0.095 Uiso 1 calc R . C45 C 0.2984(8) 0.6388(6) 0.2311(6) 0.082(6) Uiso 1 d . . H45A H 0.3292(8) 0.6553(6) 0.2405(6) 0.099 Uiso 1 calc R . C46 C 0.2763(8) 0.6287(6) 0.1925(5) 0.076(6) Uiso 1 d . . H46A H 0.2936(8) 0.6386(6) 0.1768(5) 0.091 Uiso 1 calc R . C47 C 0.2323(6) 0.6059(5) 0.1786(5) 0.054(5) Uiso 1 d . . C48 C 0.2042(6) 0.5904(5) 0.2009(4) 0.043(4) Uiso 1 d . . C49 C -0.0976(6) 0.4937(4) 0.4170(4) 0.036(4) Uiso 1 d . . C50 C -0.1221(5) 0.4940(4) 0.3757(4) 0.026(3) Uiso 1 d . . C51 C -0.1737(5) 0.5056(4) 0.3602(4) 0.032(4) Uiso 1 d . . C52 C -0.2056(6) 0.5161(4) 0.3809(4) 0.044(4) Uiso 1 d . . H52A H -0.2413(6) 0.5230(4) 0.3693(4) 0.052 Uiso 1 calc R . C53 C -0.1829(6) 0.5161(5) 0.4198(4) 0.046(4) Uiso 1 d . . H53A H -0.2033(6) 0.5239(5) 0.4342(4) 0.056 Uiso 1 calc R . C54 C -0.1305(6) 0.5045(4) 0.4364(4) 0.039(4) Uiso 1 d . . H54A H -0.1166(6) 0.5039(4) 0.4621(4) 0.047 Uiso 1 calc R . C55 C -0.2017(6) 0.5046(4) 0.3190(4) 0.037(4) Uiso 1 d . . C56 C -0.1910(5) 0.4873(4) 0.2592(4) 0.031(4) Uiso 1 d . . C57 C -0.1747(5) 0.4535(4) 0.2422(4) 0.032(4) Uiso 1 d . . C58 C -0.1375(5) 0.4227(4) 0.2628(4) 0.037(4) Uiso 1 d . . H58A H -0.1223(5) 0.4258(4) 0.2883(4) 0.045 Uiso 1 calc R . C59 C -0.1240(6) 0.3888(5) 0.2458(4) 0.047(4) Uiso 1 d . . H59A H -0.0986(6) 0.3692(5) 0.2598(4) 0.056 Uiso 1 calc R . C60 C -0.1475(5) 0.3821(4) 0.2072(4) 0.038(4) Uiso 1 d . . H60A H -0.1392(5) 0.3573(4) 0.1964(4) 0.045 Uiso 1 calc R . C61 C -0.1815(5) 0.4113(4) 0.1862(4) 0.033(4) Uiso 1 d . . C62 C -0.1960(5) 0.4488(4) 0.2023(4) 0.033(4) Uiso 1 d . . C63 C -0.2313(5) 0.4810(4) 0.1822(4) 0.035(4) Uiso 1 d . . H63A H -0.2455(5) 0.4787(4) 0.1567(4) 0.042 Uiso 1 calc R . C64 C -0.2453(6) 0.5156(5) 0.1990(4) 0.042(4) Uiso 1 d . . H64A H -0.2685(6) 0.5366(5) 0.1851(4) 0.050 Uiso 1 calc R . C65 C -0.2240(5) 0.5193(4) 0.2387(4) 0.037(4) Uiso 1 d . . H65A H -0.2324(5) 0.5432(4) 0.2504(4) 0.045 Uiso 1 calc R . C66 C -0.1951(6) 0.3754(5) 0.1254(4) 0.038(4) Uiso 1 d . . C67 C -0.2301(6) 0.3787(4) 0.0856(4) 0.038(4) Uiso 1 d . . C68 C -0.2668(5) 0.4106(4) 0.0701(4) 0.031(4) Uiso 1 d . . C69 C -0.2959(6) 0.4092(4) 0.0313(4) 0.036(4) Uiso 1 d . . C70 C -0.2871(6) 0.3774(5) 0.0097(4) 0.047(4) Uiso 1 d . . H70A H -0.3067(6) 0.3766(5) -0.0154(4) 0.056 Uiso 1 calc R . C71 C -0.2484(6) 0.3457(5) 0.0252(4) 0.051(4) Uiso 1 d . . H71A H -0.2424(6) 0.3242(5) 0.0102(4) 0.061 Uiso 1 calc R . C72 C -0.2194(6) 0.3459(5) 0.0622(4) 0.051(4) Uiso 1 d . . H72A H -0.1932(6) 0.3251(5) 0.0720(4) 0.061 Uiso 1 calc R . C73 C -0.3624(5) 0.5411(4) 0.0030(4) 0.032(4) Uiso 1 d . . C74 C -0.3069(5) 0.5443(4) 0.0185(3) 0.024(3) Uiso 1 d . . C75 C -0.2762(5) 0.5682(4) 0.0025(4) 0.030(3) Uiso 1 d . . C76 C -0.3055(6) 0.5923(4) -0.0309(4) 0.034(4) Uiso 1 d . . H76A H -0.2871(6) 0.6095(4) -0.0424(4) 0.041 Uiso 1 calc R . C77 C -0.3582(6) 0.5899(4) -0.0450(4) 0.042(4) Uiso 1 d . . H77A H -0.3756(6) 0.6053(4) -0.0664(4) 0.051 Uiso 1 calc R . C78 C -0.3885(6) 0.5652(4) -0.0290(4) 0.038(4) Uiso 1 d . . H78A H -0.4254(6) 0.5647(4) -0.0395(4) 0.046 Uiso 1 calc R . C79 C -0.2195(5) 0.5709(4) 0.0159(4) 0.032(4) Uiso 1 d . . C80 C -0.1386(6) 0.5454(4) 0.0651(4) 0.034(4) Uiso 1 d . . C81 C -0.1147(6) 0.5038(4) 0.0749(4) 0.038(4) Uiso 1 d . . C82 C -0.1447(6) 0.4655(5) 0.0650(4) 0.047(4) Uiso 1 d . . H82A H -0.1811(6) 0.4671(5) 0.0524(4) 0.056 Uiso 1 calc R . C83 C -0.1207(6) 0.4261(5) 0.0739(4) 0.049(4) Uiso 1 d . . H83A H -0.1412(6) 0.4011(5) 0.0672(4) 0.059 Uiso 1 calc R . C84 C -0.0670(6) 0.4225(5) 0.0924(4) 0.045(4) Uiso 1 d . . H84A H -0.0519(6) 0.3950(5) 0.0976(4) 0.054 Uiso 1 calc R . C85 C -0.0350(6) 0.4583(5) 0.1035(4) 0.046(4) Uiso 1 d . . C86 C -0.0584(6) 0.5001(4) 0.0934(4) 0.038(4) Uiso 1 d . . C87 C -0.0284(6) 0.5396(4) 0.1011(4) 0.041(4) Uiso 1 d . . H87A H 0.0083(6) 0.5385(4) 0.1125(4) 0.049 Uiso 1 calc R . C88 C -0.0524(6) 0.5782(5) 0.0922(4) 0.043(4) Uiso 1 d . . H88A H -0.0321(6) 0.6034(5) 0.0980(4) 0.052 Uiso 1 calc R . C89 C -0.1086(6) 0.5813(5) 0.0740(4) 0.046(4) Uiso 1 d . . H89A H -0.1245(6) 0.6084(5) 0.0682(4) 0.056 Uiso 1 calc R . C90 C 0.0513(6) 0.4200(5) 0.1343(4) 0.045(4) Uiso 1 d . . C91 C 0.1087(6) 0.4277(5) 0.1441(4) 0.042(4) Uiso 1 d . . C92 C 0.1321(6) 0.4673(4) 0.1435(4) 0.039(4) Uiso 1 d . . C93 C 0.1888(6) 0.4700(5) 0.1512(4) 0.043(4) Uiso 1 d . . C94 C 0.2174(7) 0.4316(5) 0.1592(4) 0.053(5) Uiso 1 d . . H94A H 0.2539(7) 0.4327(5) 0.1641(4) 0.064 Uiso 1 calc R . C95 C 0.1945(7) 0.3923(5) 0.1604(5) 0.060(5) Uiso 1 d . . H95A H 0.2152(7) 0.3673(5) 0.1662(5) 0.072 Uiso 1 calc R . C96 C 0.1413(7) 0.3903(5) 0.1529(4) 0.056(5) Uiso 1 d . . H96A H 0.1257(7) 0.3635(5) 0.1535(4) 0.067 Uiso 1 calc R . C97 C -0.4130(5) 0.4634(4) 0.0891(4) 0.031(4) Uiso 1 d . . C98 C -0.3854(6) 0.5019(4) 0.1081(4) 0.034(4) Uiso 1 d . . C99 C -0.4045(5) 0.5242(4) 0.1325(4) 0.033(4) Uiso 1 d . . C100 C -0.4505(6) 0.5066(4) 0.1386(4) 0.040(4) Uiso 1 d . . H10C H -0.4644(6) 0.5209(4) 0.1545(4) 0.048 Uiso 1 calc R . C101 C -0.4744(6) 0.4697(4) 0.1218(4) 0.041(4) Uiso 1 d . . H10D H -0.5037(6) 0.4588(4) 0.1267(4) 0.049 Uiso 1 calc R . C102 C -0.4555(6) 0.4485(4) 0.0976(4) 0.036(4) Uiso 1 d . . H10E H -0.4721(6) 0.4230(4) 0.0866(4) 0.044 Uiso 1 calc R . C103 C -0.3830(6) 0.5660(4) 0.1499(4) 0.037(4) Uiso 1 d . . C104 C -0.3163(6) 0.6225(4) 0.1519(4) 0.036(4) Uiso 1 d . . C105 C -0.2844(6) 0.6385(4) 0.1332(4) 0.039(4) Uiso 1 d . . C106 C -0.2738(7) 0.6134(6) 0.1059(5) 0.064(5) Uiso 1 d . . H10F H -0.2894(7) 0.5862(6) 0.0995(5) 0.077 Uiso 1 calc R . C107 C -0.2406(8) 0.6290(6) 0.0889(6) 0.080(6) Uiso 1 d . . H10G H -0.2340(8) 0.6121(6) 0.0710(6) 0.096 Uiso 1 calc R . C108 C -0.2154(8) 0.6703(6) 0.0975(5) 0.079(6) Uiso 1 d . . H10H H -0.1921(8) 0.6798(6) 0.0858(5) 0.095 Uiso 1 calc R . C109 C -0.2260(6) 0.6956(5) 0.1230(4) 0.043(4) Uiso 1 d . . C110 C -0.2579(6) 0.6793(5) 0.1416(4) 0.042(4) Uiso 1 d . . C111 C -0.2662(7) 0.7034(6) 0.1706(5) 0.063(5) Uiso 1 d . . H11C H -0.2511(7) 0.7308(6) 0.1766(5) 0.076 Uiso 1 calc R . C112 C -0.2962(8) 0.6864(7) 0.1896(6) 0.096(7) Uiso 1 d . . H11D H -0.3001(8) 0.7024(7) 0.2090(6) 0.115 Uiso 1 calc R . C113 C -0.3221(8) 0.6450(6) 0.1811(6) 0.082(6) Uiso 1 d . . H11E H -0.3420(8) 0.6339(6) 0.1948(6) 0.098 Uiso 1 calc R . C114 C -0.1877(7) 0.7631(5) 0.1088(5) 0.055(5) Uiso 1 d . . C115 C -0.1608(6) 0.8044(4) 0.1232(4) 0.038(4) Uiso 1 d . . C116 C -0.1456(5) 0.8156(4) 0.1611(4) 0.035(4) Uiso 1 d . . C117 C -0.1218(6) 0.8566(4) 0.1723(4) 0.038(4) Uiso 1 d . . C118 C -0.1106(6) 0.8843(5) 0.1473(4) 0.046(4) Uiso 1 d . . H11G H -0.0933(6) 0.9105(5) 0.1554(4) 0.055 Uiso 1 calc R . C119 C -0.1260(6) 0.8723(5) 0.1086(5) 0.056(5) Uiso 1 d . . H11H H -0.1188(6) 0.8902(5) 0.0914(5) 0.067 Uiso 1 calc R . C120 C -0.1513(6) 0.8335(5) 0.0985(4) 0.049(4) Uiso 1 d . . H12C H -0.1629(6) 0.8261(5) 0.0736(4) 0.059 Uiso 1 calc R . C121 C -0.0509(6) 0.8429(4) 0.2984(4) 0.037(4) Uiso 1 d . . C122 C -0.0261(6) 0.8101(4) 0.2836(4) 0.037(4) Uiso 1 d . . C123 C 0.0244(6) 0.7964(4) 0.3015(4) 0.038(4) Uiso 1 d . . C124 C 0.0542(7) 0.8175(5) 0.3352(4) 0.051(4) Uiso 1 d . . H12D H 0.0893(7) 0.8093(5) 0.3474(4) 0.061 Uiso 1 calc R . C125 C 0.0325(6) 0.8495(5) 0.3499(5) 0.053(4) Uiso 1 d . . H12E H 0.0524(6) 0.8626(5) 0.3720(5) 0.064 Uiso 1 calc R . C126 C -0.0198(6) 0.8625(5) 0.3317(4) 0.045(4) Uiso 1 d . . H12F H -0.0344(6) 0.8845(5) 0.3418(4) 0.054 Uiso 1 calc R . C127 C 0.0515(7) 0.7624(5) 0.2883(4) 0.050(4) Uiso 1 d . . C128 C 0.0439(6) 0.7161(5) 0.2340(4) 0.044(4) Uiso 1 d . . C129 C 0.0197(6) 0.7173(5) 0.1947(4) 0.048(4) Uiso 1 d . . C130 C -0.0222(7) 0.7451(5) 0.1777(5) 0.060(5) Uiso 1 d . . H13A H -0.0344(7) 0.7638(5) 0.1920(5) 0.072 Uiso 1 calc R . C131 C -0.0460(8) 0.7453(6) 0.1399(6) 0.081(6) Uiso 1 d . . H13B H -0.0750(8) 0.7632(6) 0.1289(6) 0.098 Uiso 1 calc R . C132 C -0.0263(7) 0.7180(6) 0.1175(5) 0.072(5) Uiso 1 d . . H13C H -0.0427(7) 0.7180(6) 0.0920(5) 0.086 Uiso 1 calc R . C133 C 0.0168(6) 0.6918(5) 0.1337(4) 0.049(4) Uiso 1 d . . C134 C 0.0399(6) 0.6900(4) 0.1721(4) 0.038(4) Uiso 1 d . . C135 C 0.0811(7) 0.6624(5) 0.1898(5) 0.063(5) Uiso 1 d . . H13D H 0.0952(7) 0.6448(5) 0.1758(5) 0.075 Uiso 1 calc R . C136 C 0.1019(8) 0.6600(6) 0.2275(5) 0.080(6) Uiso 1 d . . H13E H 0.1288(8) 0.6401(6) 0.2385(5) 0.096 Uiso 1 calc R . C137 C 0.0827(7) 0.6877(6) 0.2504(6) 0.074(6) Uiso 1 d . . H13F H 0.0970(7) 0.6859(6) 0.2760(6) 0.089 Uiso 1 calc R . C138 C 0.0326(7) 0.6714(5) 0.0759(5) 0.055(5) Uiso 1 d . . C139 C 0.0591(6) 0.6392(5) 0.0597(4) 0.043(4) Uiso 1 d . . C140 C 0.0886(6) 0.6052(5) 0.0785(4) 0.042(4) Uiso 1 d . . C141 C 0.1179(6) 0.5785(5) 0.0615(4) 0.048(4) Uiso 1 d . . C142 C 0.1126(6) 0.5866(5) 0.0243(4) 0.051(4) Uiso 1 d . . H14A H 0.1296(6) 0.5687(5) 0.0124(4) 0.061 Uiso 1 calc R . C143 C 0.0821(6) 0.6211(5) 0.0054(5) 0.062(5) Uiso 1 d . . H14B H 0.0788(6) 0.6265(5) -0.0190(5) 0.074 Uiso 1 calc R . C144 C 0.0569(6) 0.6475(5) 0.0233(5) 0.057(5) Uiso 1 d . . H14C H 0.0378(6) 0.6713(5) 0.0109(5) 0.068 Uiso 1 calc R . C145 C 0.0769(8) 0.4672(6) 0.0009(6) 0.095(7) Uiso 1 d . . H14D H 0.1032(8) 0.4632(6) -0.0107(6) 0.142 Uiso 1 calc R . H14E H 0.0799(8) 0.4960(6) 0.0109(6) 0.142 Uiso 1 calc R . H14F H 0.0421(8) 0.4632(6) -0.0170(6) 0.142 Uiso 1 calc R . C146 C 0.0444(7) 0.4429(6) 0.0476(6) 0.082(6) Uiso 1 d . . H14G H 0.0487(7) 0.4225(6) 0.0673(6) 0.122 Uiso 1 calc R . H14H H 0.0099(7) 0.4392(6) 0.0292(6) 0.122 Uiso 1 calc R . H14I H 0.0477(7) 0.4719(6) 0.0572(6) 0.122 Uiso 1 calc R . C147 C 0.1388(7) 0.4436(6) 0.0586(5) 0.080(6) Uiso 1 d . . H14J H 0.1656(7) 0.4386(6) 0.0477(5) 0.119 Uiso 1 calc R . H14K H 0.1444(7) 0.4245(6) 0.0793(5) 0.119 Uiso 1 calc R . H14L H 0.1406(7) 0.4731(6) 0.0668(5) 0.119 Uiso 1 calc R . C148 C 0.0816(7) 0.3904(5) 0.0146(4) 0.054(5) Uiso 1 d . . H14M H 0.0452(7) 0.3856(5) -0.0014(4) 0.064 Uiso 1 calc R . H14N H 0.1041(7) 0.3890(5) -0.0006(4) 0.064 Uiso 1 calc R . C149 C 0.0973(7) 0.3549(5) 0.0424(5) 0.062(5) Uiso 1 d . . C150 C 0.1468(8) 0.3403(6) 0.0553(5) 0.068(5) Uiso 1 d . . H15B H 0.1728(8) 0.3531(6) 0.0476(5) 0.082 Uiso 1 calc R . C151 C 0.1602(9) 0.3059(7) 0.0800(6) 0.094(7) Uiso 1 d . . H15C H 0.1950(9) 0.2957(7) 0.0886(6) 0.112 Uiso 1 calc R . C152 C 0.1224(9) 0.2869(7) 0.0918(6) 0.093(7) Uiso 1 d . . H15D H 0.1316(9) 0.2635(7) 0.1079(6) 0.112 Uiso 1 calc R . C153 C 0.0716(9) 0.3023(7) 0.0802(6) 0.098(7) Uiso 1 d . . H15E H 0.0463(9) 0.2897(7) 0.0887(6) 0.118 Uiso 1 calc R . C154 C 0.0577(8) 0.3373(6) 0.0552(6) 0.082(6) Uiso 1 d . . H15G H 0.0234(8) 0.3486(6) 0.0474(6) 0.099 Uiso 1 calc R . C155 C 0.3237(7) 0.1660(6) 0.1465(5) 0.069(5) Uiso 1 d . . C156 C 0.2279(9) 0.1633(7) 0.1381(6) 0.093(7) Uiso 1 d D . C157 C 0.2589(9) 0.1701(7) 0.0830(6) 0.094(7) Uiso 1 d . . C158 C 0.2739(8) 0.1011(6) 0.1182(5) 0.076(6) Uiso 1 d . . C159 C 0.1434(14) 0.1719(10) 0.0863(10) 0.098(14) Uiso 0.50 d PD . C160 C 0.1762(11) 0.1488(9) 0.1178(7) 0.067(10) Uiso 0.50 d PD . C161 C 0.1575(13) 0.1113(11) 0.1298(10) 0.091(13) Uiso 0.50 d PD . C162 C 0.0913(14) 0.1566(13) 0.0674(11) 0.119(17) Uiso 0.50 d PD . C163 C 0.1047(16) 0.0969(13) 0.1116(12) 0.137(19) Uiso 0.50 d PD . C164 C 0.0708(14) 0.1220(14) 0.0821(12) 0.131(19) Uiso 0.50 d PD . C165 C -0.1072(7) 0.6736(6) 0.2135(5) 0.075(6) Uiso 1 d . . H16B H -0.0752(7) 0.6902(6) 0.2183(5) 0.112 Uiso 1 calc R . H16C H -0.1160(7) 0.6718(6) 0.2357(5) 0.112 Uiso 1 calc R . H16D H -0.1357(7) 0.6875(6) 0.1945(5) 0.112 Uiso 1 calc R . C166 C -0.0875(7) 0.6324(5) 0.1652(5) 0.065(5) Uiso 1 d . . H16E H -0.0555(7) 0.6487(5) 0.1691(5) 0.097 Uiso 1 calc R . H16F H -0.1166(7) 0.6466(5) 0.1468(5) 0.097 Uiso 1 calc R . H16G H -0.0833(7) 0.6037(5) 0.1570(5) 0.097 Uiso 1 calc R . C167 C -0.1481(8) 0.6048(6) 0.1944(6) 0.087(6) Uiso 1 d . . H16H H -0.1431(8) 0.5761(6) 0.1865(6) 0.130 Uiso 1 calc R . H16I H -0.1765(8) 0.6188(6) 0.1754(6) 0.130 Uiso 1 calc R . H16J H -0.1568(8) 0.6031(6) 0.2165(6) 0.130 Uiso 1 calc R . C168 C -0.0539(7) 0.6072(6) 0.2304(5) 0.073(5) Uiso 1 d . . H16K H -0.0224(7) 0.6252(6) 0.2358(5) 0.087 Uiso 1 calc R . H16L H -0.0625(7) 0.6049(6) 0.2528(5) 0.087 Uiso 1 calc R . C169 C -0.0409(7) 0.5630(6) 0.2201(5) 0.065(5) Uiso 1 d . . C170 C -0.0015(7) 0.5579(6) 0.2045(5) 0.073(6) Uiso 1 d . . H17B H 0.0168(7) 0.5823(6) 0.2010(5) 0.088 Uiso 1 calc R . C171 C 0.0110(7) 0.5181(5) 0.1941(5) 0.063(5) Uiso 1 d . . H17C H 0.0379(7) 0.5150(5) 0.1840(5) 0.075 Uiso 1 calc R . C172 C -0.0170(8) 0.4830(6) 0.1990(5) 0.080(6) Uiso 1 d . . H17D H -0.0095(8) 0.4559(6) 0.1914(5) 0.096 Uiso 1 calc R . C173 C -0.0551(8) 0.4862(6) 0.2145(5) 0.075(6) Uiso 1 d . . H17E H -0.0727(8) 0.4613(6) 0.2179(5) 0.090 Uiso 1 calc R . C174 C -0.0684(7) 0.5258(5) 0.2254(5) 0.065(5) Uiso 1 d . . H17F H -0.0948(7) 0.5280(5) 0.2360(5) 0.078 Uiso 1 calc R . C175 C -0.1794(6) 0.3909(5) 0.3395(4) 0.054(5) Uiso 1 d . . H17G H -0.1457(6) 0.3766(5) 0.3449(4) 0.081 Uiso 1 calc R . H17H H -0.1739(6) 0.4217(5) 0.3422(4) 0.081 Uiso 1 calc R . H17I H -0.2015(6) 0.3844(5) 0.3147(4) 0.081 Uiso 1 calc R . C176 C -0.2568(6) 0.3977(5) 0.3569(4) 0.054(5) Uiso 1 d . . H17J H -0.2508(6) 0.4283(5) 0.3607(4) 0.080 Uiso 1 calc R . H17K H -0.2753(6) 0.3871(5) 0.3727(4) 0.080 Uiso 1 calc R . H17L H -0.2778(6) 0.3923(5) 0.3316(4) 0.080 Uiso 1 calc R . C177 C -0.2158(6) 0.3287(5) 0.3598(5) 0.056(5) Uiso 1 d . . H17M H -0.1825(6) 0.3137(5) 0.3655(5) 0.085 Uiso 1 calc R . H17N H -0.2370(6) 0.3236(5) 0.3345(5) 0.085 Uiso 1 calc R . H17O H -0.2344(6) 0.3184(5) 0.3755(5) 0.085 Uiso 1 calc R . C178 C -0.1693(6) 0.3866(5) 0.4043(4) 0.053(5) Uiso 1 d . . H17P H -0.1353(6) 0.3725(5) 0.4089(4) 0.064 Uiso 1 calc R . H17Q H -0.1633(6) 0.4177(5) 0.4060(4) 0.064 Uiso 1 calc R . C179 C -0.1919(7) 0.3729(6) 0.4336(5) 0.066(5) Uiso 1 d . . C180 C -0.2187(7) 0.4024(6) 0.4465(5) 0.077(6) Uiso 1 d . . H18A H -0.2221(7) 0.4308(6) 0.4378(5) 0.093 Uiso 1 calc R . C181 C -0.2421(9) 0.3896(8) 0.4740(7) 0.107(8) Uiso 1 d . . H18C H -0.2609(9) 0.4092(8) 0.4833(7) 0.129 Uiso 1 calc R . C182 C -0.2353(9) 0.3487(8) 0.4851(6) 0.099(7) Uiso 1 d . . H18B H -0.2507(9) 0.3405(8) 0.5024(6) 0.119 Uiso 1 calc R . C183 C -0.2113(8) 0.3209(7) 0.4752(6) 0.093(7) Uiso 1 d . . H18D H -0.2094(8) 0.2930(7) 0.4847(6) 0.112 Uiso 1 calc R . C184 C -0.1847(9) 0.3310(7) 0.4478(6) 0.094(7) Uiso 1 d . . H18E H -0.1645(9) 0.3105(7) 0.4406(6) 0.113 Uiso 1 calc R . C185 C -0.0609(7) 0.2849(6) 0.1960(5) 0.075(6) Uiso 1 d . . H18F H -0.0557(7) 0.2545(6) 0.1930(5) 0.113 Uiso 1 calc R . H18G H -0.0976(7) 0.2922(6) 0.1838(5) 0.113 Uiso 1 calc R . H18H H -0.0509(7) 0.2916(6) 0.2218(5) 0.113 Uiso 1 calc R . C186 C -0.0352(7) 0.3574(5) 0.1841(5) 0.069(5) Uiso 1 d . . H18I H -0.0135(7) 0.3737(5) 0.1734(5) 0.103 Uiso 1 calc R . H18J H -0.0252(7) 0.3642(5) 0.2098(5) 0.103 Uiso 1 calc R . H18K H -0.0719(7) 0.3648(5) 0.1719(5) 0.103 Uiso 1 calc R . C187 C -0.0437(8) 0.3017(6) 0.1382(5) 0.080(6) Uiso 1 d . . H18L H -0.0215(8) 0.3184(6) 0.1282(5) 0.120 Uiso 1 calc R . H18M H -0.0802(8) 0.3099(6) 0.1264(5) 0.120 Uiso 1 calc R . H18N H -0.0396(8) 0.2714(6) 0.1341(5) 0.120 Uiso 1 calc R . C188 C 0.0309(7) 0.3007(6) 0.1974(5) 0.070(5) Uiso 1 d . . H18O H 0.0507(7) 0.3199(6) 0.1869(5) 0.084 Uiso 1 calc R . H18P H 0.0412(7) 0.3072(6) 0.2235(5) 0.084 Uiso 1 calc R . C189 C 0.0465(7) 0.2548(6) 0.1932(5) 0.073(6) Uiso 1 d . . C190 C 0.0428(9) 0.2218(7) 0.2165(6) 0.097(7) Uiso 1 d . . H19A H 0.0290(9) 0.2275(7) 0.2351(6) 0.117 Uiso 1 calc R . C191 C 0.0599(10) 0.1799(9) 0.2121(8) 0.126(9) Uiso 1 d . . H19B H 0.0579(10) 0.1582(9) 0.2284(8) 0.151 Uiso 1 calc R . C192 C 0.0798(10) 0.1700(9) 0.1840(8) 0.126(9) Uiso 1 d . . H19C H 0.0893(10) 0.1418(9) 0.1804(8) 0.152 Uiso 1 calc R . C193 C 0.0850(9) 0.2035(8) 0.1616(7) 0.114(8) Uiso 1 d . . H19D H 0.0999(9) 0.1978(8) 0.1435(7) 0.136 Uiso 1 calc R . C194 C 0.0689(8) 0.2445(7) 0.1653(6) 0.098(7) Uiso 1 d . . H19E H 0.0725(8) 0.2662(7) 0.1496(6) 0.118 Uiso 1 calc R . C195 C -0.3228(7) 0.3669(5) 0.1691(5) 0.061(5) Uiso 1 d . . H19F H -0.3530(7) 0.3836(5) 0.1693(5) 0.092 Uiso 1 calc R . H19G H -0.2979(7) 0.3855(5) 0.1633(5) 0.092 Uiso 1 calc R . H19H H -0.3061(7) 0.3540(5) 0.1929(5) 0.092 Uiso 1 calc R . C196 C -0.3777(7) 0.3021(5) 0.1502(5) 0.061(5) Uiso 1 d . . H19I H -0.4087(7) 0.3178(5) 0.1501(5) 0.092 Uiso 1 calc R . H19J H -0.3601(7) 0.2902(5) 0.1743(5) 0.092 Uiso 1 calc R . H19K H -0.3879(7) 0.2790(5) 0.1324(5) 0.092 Uiso 1 calc R . C197 C -0.3666(6) 0.3544(5) 0.1039(4) 0.047(4) Uiso 1 d . . H19L H -0.3957(6) 0.3721(5) 0.1057(4) 0.057 Uiso 1 calc R . H19M H -0.3408(6) 0.3738(5) 0.0995(4) 0.057 Uiso 1 calc R . C198 C -0.2934(7) 0.3071(6) 0.1408(5) 0.074(6) Uiso 1 d . . H19N H -0.2691(7) 0.3259(6) 0.1346(5) 0.111 Uiso 1 calc R . H19O H -0.3041(7) 0.2840(6) 0.1231(5) 0.111 Uiso 1 calc R . H19P H -0.2763(7) 0.2951(6) 0.1649(5) 0.111 Uiso 1 calc R . C199 C -0.3880(6) 0.3247(5) 0.0711(4) 0.048(4) Uiso 1 d . . C200 C -0.4395(7) 0.3120(5) 0.0601(5) 0.064(5) Uiso 1 d . . H20B H -0.4615(7) 0.3208(5) 0.0730(5) 0.077 Uiso 1 calc R . C201 C -0.4604(8) 0.2840(6) 0.0274(5) 0.069(5) Uiso 1 d . . H20C H -0.4955(8) 0.2745(6) 0.0190(5) 0.083 Uiso 1 calc R . C202 C -0.4268(8) 0.2729(6) 0.0106(5) 0.074(6) Uiso 1 d . . H20D H -0.4394(8) 0.2547(6) -0.0097(5) 0.089 Uiso 1 calc R . C203 C -0.3764(8) 0.2856(6) 0.0203(5) 0.079(6) Uiso 1 d . . H20E H -0.3550(8) 0.2770(6) 0.0069(5) 0.095 Uiso 1 calc R . C204 C -0.3565(7) 0.3129(5) 0.0517(4) 0.056(5) Uiso 1 d . . H20F H -0.3216(7) 0.3226(5) 0.0590(4) 0.067 Uiso 1 calc R . C205 C 0.2890(6) 0.4948(5) 0.1032(4) 0.052(4) Uiso 1 d . . H20G H 0.2570(6) 0.4980(5) 0.1095(4) 0.062 Uiso 1 calc R . H20H H 0.2862(6) 0.4675(5) 0.0902(4) 0.062 Uiso 1 calc R . C206 C 0.3380(6) 0.5274(5) 0.0653(5) 0.054(5) Uiso 1 d . . H20I H 0.3383(6) 0.4994(5) 0.0545(5) 0.081 Uiso 1 calc R . H20J H 0.3698(6) 0.5309(5) 0.0863(5) 0.081 Uiso 1 calc R . H20K H 0.3364(6) 0.5495(5) 0.0475(5) 0.081 Uiso 1 calc R . C207 C 0.2898(7) 0.5738(6) 0.0940(5) 0.075(6) Uiso 1 d . . H20L H 0.3209(7) 0.5769(6) 0.1156(5) 0.112 Uiso 1 calc R . H20M H 0.2585(7) 0.5764(6) 0.1007(5) 0.112 Uiso 1 calc R . H20N H 0.2897(7) 0.5960(6) 0.0765(5) 0.112 Uiso 1 calc R . C208 C 0.2421(6) 0.5281(5) 0.0444(4) 0.058(5) Uiso 1 d . . H20O H 0.2411(6) 0.5005(5) 0.0327(4) 0.087 Uiso 1 calc R . H20P H 0.2424(6) 0.5509(5) 0.0274(4) 0.087 Uiso 1 calc R . H20Q H 0.2112(6) 0.5312(5) 0.0516(4) 0.087 Uiso 1 calc R . C209 C 0.3356(7) 0.4923(5) 0.1382(5) 0.053(5) Uiso 1 d . . C210 C 0.3782(7) 0.4665(6) 0.1405(5) 0.069(5) Uiso 1 d . . H21B H 0.3787(7) 0.4519(6) 0.1195(5) 0.082 Uiso 1 calc R . C211 C 0.4203(9) 0.4614(7) 0.1730(6) 0.088(6) Uiso 1 d . . H21C H 0.4482(9) 0.4428(7) 0.1744(6) 0.106 Uiso 1 calc R . C212 C 0.4195(10) 0.4850(7) 0.2033(7) 0.103(7) Uiso 1 d . . H21D H 0.4484(10) 0.4832(7) 0.2251(7) 0.124 Uiso 1 calc R . C213 C 0.3787(10) 0.5103(8) 0.2023(7) 0.110(8) Uiso 1 d . . H21E H 0.3786(10) 0.5242(8) 0.2237(7) 0.132 Uiso 1 calc R . C214 C 0.3364(8) 0.5162(6) 0.1700(6) 0.084(6) Uiso 1 d . . H21F H 0.3091(8) 0.5354(6) 0.1690(6) 0.101 Uiso 1 calc R . C215 C 0.1909(13) 0.3740(10) 0.5351(10) 0.178(13) Uiso 1 d . . H21G H 0.2050(13) 0.4029(10) 0.5404(10) 0.266 Uiso 1 calc R . H21H H 0.1925(13) 0.3600(10) 0.5577(10) 0.266 Uiso 1 calc R . H21I H 0.1546(13) 0.3754(10) 0.5190(10) 0.266 Uiso 1 calc R . C216 C 0.2199(14) 0.3699(12) 0.4804(11) 0.199(15) Uiso 1 d . . H21J H 0.2411(14) 0.3523(12) 0.4702(11) 0.298 Uiso 1 calc R . H21K H 0.2339(14) 0.3988(12) 0.4842(11) 0.298 Uiso 1 calc R . H21L H 0.1839(14) 0.3706(12) 0.4637(11) 0.298 Uiso 1 calc R . C217 C 0.1944(15) 0.3069(12) 0.5119(11) 0.214(16) Uiso 1 d . . H21M H 0.2122(15) 0.2879(12) 0.5001(11) 0.322 Uiso 1 calc R . H21N H 0.1579(15) 0.3102(12) 0.4964(11) 0.322 Uiso 1 calc R . H21O H 0.1959(15) 0.2948(12) 0.5352(11) 0.322 Uiso 1 calc R . C218 C 0.2800(12) 0.3421(11) 0.5348(10) 0.177(13) Uiso 1 d D . H21P H 0.2996(12) 0.3688(11) 0.5357(10) 0.213 Uiso 1 calc R . H21Q H 0.2912(12) 0.3211(11) 0.5202(10) 0.213 Uiso 1 calc R . C219 C 0.2911(9) 0.3235(13) 0.5764(9) 0.220(17) Uiso 1 d D . C220 C 0.2915(12) 0.2795(12) 0.5795(9) 0.202(15) Uiso 1 d D . H22B H 0.2859(12) 0.2620(12) 0.5589(9) 0.243 Uiso 1 calc R . C221 C 0.3003(16) 0.2611(9) 0.6140(11) 0.250(20) Uiso 1 d D . H22C H 0.3001(16) 0.2311(9) 0.6165(11) 0.300 Uiso 1 calc R . C222 C 0.3092(13) 0.2868(11) 0.6439(8) 0.176(13) Uiso 1 d D . H22D H 0.3150(13) 0.2743(11) 0.6669(8) 0.211 Uiso 1 calc R . C223 C 0.3099(15) 0.3314(12) 0.6409(9) 0.228(18) Uiso 1 d D . H22E H 0.3188(15) 0.3486(12) 0.6620(9) 0.273 Uiso 1 calc R . C224 C 0.2973(15) 0.3499(9) 0.6067(11) 0.227(18) Uiso 1 d D . H22F H 0.2930(15) 0.3798(9) 0.6039(11) 0.273 Uiso 1 calc R . C225 C 0.0339(8) 0.0432(6) 0.4532(5) 0.079(6) Uiso 1 d . . H22G H 0.0438(8) 0.0482(6) 0.4318(5) 0.118 Uiso 1 calc R . H22H H 0.0060(8) 0.0221(6) 0.4475(5) 0.118 Uiso 1 calc R . H22I H 0.0642(8) 0.0327(6) 0.4730(5) 0.118 Uiso 1 calc R . C226 C -0.0322(7) 0.1008(5) 0.4313(5) 0.059(5) Uiso 1 d . . H22J H -0.0203(7) 0.1043(5) 0.4104(5) 0.071 Uiso 1 calc R . H22R H -0.0595(7) 0.0786(5) 0.4249(5) 0.071 Uiso 1 calc R . C227 C 0.0604(7) 0.1148(5) 0.4741(5) 0.068(5) Uiso 1 d . . H22K H 0.0713(7) 0.1192(5) 0.4530(5) 0.101 Uiso 1 calc R . H22L H 0.0895(7) 0.1032(5) 0.4941(5) 0.101 Uiso 1 calc R . H22M H 0.0495(7) 0.1420(5) 0.4814(5) 0.101 Uiso 1 calc R . C228 C -0.0001(7) 0.0782(6) 0.4965(5) 0.074(6) Uiso 1 d . . H22N H -0.0120(7) 0.1054(6) 0.5030(5) 0.110 Uiso 1 calc R . H22O H 0.0299(7) 0.0680(6) 0.5167(5) 0.110 Uiso 1 calc R . H22P H -0.0283(7) 0.0574(6) 0.4911(5) 0.110 Uiso 1 calc R . C229 C -0.1255(14) 0.1777(11) 0.4540(9) 0.167(12) Uiso 1 d . . H22Q H -0.1542(14) 0.1775(11) 0.4624(9) 0.201 Uiso 1 calc R . C230 C -0.0568(7) 0.1420(5) 0.4368(5) 0.056(5) Uiso 1 d . . C231 C -0.0374(10) 0.1790(8) 0.4259(7) 0.121(9) Uiso 1 d . . H23A H -0.0093(10) 0.1795(8) 0.4168(7) 0.145 Uiso 1 calc R . C232 C -0.0981(9) 0.1410(8) 0.4492(6) 0.104(7) Uiso 1 d . . H23C H -0.1091(9) 0.1141(8) 0.4548(6) 0.125 Uiso 1 calc R . C233 C -0.1053(12) 0.2113(10) 0.4453(8) 0.140(10) Uiso 1 d . . H23D H -0.1204(12) 0.2363(10) 0.4511(8) 0.168 Uiso 1 calc R . C234 C -0.0698(12) 0.2210(10) 0.4307(8) 0.146(10) Uiso 1 d . . H23B H -0.0638(12) 0.2489(10) 0.4239(8) 0.176 Uiso 1 calc R . C235 C -0.3267(7) 0.4435(5) 0.2484(5) 0.061(5) Uiso 1 d . . H23E H -0.2932(7) 0.4559(5) 0.2628(5) 0.091 Uiso 1 calc R . H23F H -0.3283(7) 0.4407(5) 0.2232(5) 0.091 Uiso 1 calc R . H23G H -0.3302(7) 0.4154(5) 0.2580(5) 0.091 Uiso 1 calc R . C236 C -0.4223(6) 0.4534(5) 0.2282(4) 0.055(5) Uiso 1 d . . H23H H -0.4503(6) 0.4721(5) 0.2296(4) 0.083 Uiso 1 calc R . H23I H -0.4262(6) 0.4254(5) 0.2378(4) 0.083 Uiso 1 calc R . H23J H -0.4243(6) 0.4507(5) 0.2030(4) 0.083 Uiso 1 calc R . C237 C -0.3674(6) 0.4747(5) 0.2903(4) 0.049(4) Uiso 1 d . . H23K H -0.3711(6) 0.4457(5) 0.2989(4) 0.059 Uiso 1 calc R . H23L H -0.3324(6) 0.4853(5) 0.3049(4) 0.059 Uiso 1 calc R . C238 C -0.3629(6) 0.5152(5) 0.2351(4) 0.052(4) Uiso 1 d . . H23M H -0.3290(6) 0.5268(5) 0.2497(4) 0.078 Uiso 1 calc R . H23N H -0.3906(6) 0.5346(5) 0.2358(4) 0.078 Uiso 1 calc R . H23O H -0.3641(6) 0.5118(5) 0.2100(4) 0.078 Uiso 1 calc R . C239 C -0.4078(7) 0.5030(5) 0.2968(5) 0.060(5) Uiso 1 d . . C240 C -0.4555(7) 0.4854(6) 0.2974(5) 0.074(6) Uiso 1 d . . H24A H -0.4621(7) 0.4559(6) 0.2933(5) 0.088 Uiso 1 calc R . C241 C -0.4939(8) 0.5121(7) 0.3043(6) 0.084(6) Uiso 1 d . . H24B H -0.5257(8) 0.5000(7) 0.3045(6) 0.101 Uiso 1 calc R . C242 C -0.4853(10) 0.5536(7) 0.3103(6) 0.100(7) Uiso 1 d . . H24C H -0.5115(10) 0.5707(7) 0.3143(6) 0.120 Uiso 1 calc R . C243 C -0.4381(9) 0.5725(8) 0.3108(6) 0.102(7) Uiso 1 d . . H24D H -0.4326(9) 0.6021(8) 0.3153(6) 0.122 Uiso 1 calc R . C244 C -0.3993(8) 0.5474(6) 0.3046(5) 0.084(6) Uiso 1 d . . H24E H -0.3672(8) 0.5600(6) 0.3055(5) 0.101 Uiso 1 calc R . C245 C 0.0055(7) 0.6379(5) 0.5132(4) 0.057(5) Uiso 1 d . . H24F H -0.0298(7) 0.6496(5) 0.5028(4) 0.085 Uiso 1 calc R . H24G H 0.0310(7) 0.6600(5) 0.5138(4) 0.085 Uiso 1 calc R . H24H H 0.0111(7) 0.6278(5) 0.5378(4) 0.085 Uiso 1 calc R . C246 C 0.0653(6) 0.5828(5) 0.5054(5) 0.059(5) Uiso 1 d . . H24I H 0.0687(6) 0.5592(5) 0.4901(5) 0.089 Uiso 1 calc R . H24J H 0.0713(6) 0.5725(5) 0.5300(5) 0.089 Uiso 1 calc R . H24K H 0.0912(6) 0.6047(5) 0.5060(5) 0.089 Uiso 1 calc R . C247 C -0.0269(6) 0.5663(5) 0.4907(4) 0.047(4) Uiso 1 d . . H24L H -0.0625(6) 0.5774(5) 0.4809(4) 0.070 Uiso 1 calc R . H24M H -0.0199(6) 0.5567(5) 0.5156(4) 0.070 Uiso 1 calc R . H24N H -0.0230(6) 0.5424(5) 0.4759(4) 0.070 Uiso 1 calc R . C248 C 0.0018(6) 0.6151(5) 0.4504(4) 0.043(4) Uiso 1 d . . H24O H 0.0293(6) 0.6356(5) 0.4504(4) 0.051 Uiso 1 calc R . H24P H 0.0062(6) 0.5897(5) 0.4368(4) 0.051 Uiso 1 calc R . C249 C -0.0500(6) 0.6347(5) 0.4300(4) 0.048(4) Uiso 1 d . . C250 C -0.0919(6) 0.6090(5) 0.4067(4) 0.051(4) Uiso 1 d . . H25A H -0.0866(6) 0.5794(5) 0.4047(4) 0.061 Uiso 1 calc R . C251 C -0.1408(7) 0.6274(5) 0.3868(5) 0.055(5) Uiso 1 d . . H25B H -0.1682(7) 0.6099(5) 0.3722(5) 0.066 Uiso 1 calc R . C252 C -0.1487(8) 0.6707(6) 0.3886(5) 0.072(6) Uiso 1 d . . H25C H -0.1809(8) 0.6830(6) 0.3743(5) 0.086 Uiso 1 calc R . C253 C -0.1088(7) 0.6964(6) 0.4116(5) 0.074(6) Uiso 1 d . . H25D H -0.1148(7) 0.7259(6) 0.4134(5) 0.088 Uiso 1 calc R . C254 C -0.0607(7) 0.6791(5) 0.4317(5) 0.056(5) Uiso 1 d . . H25E H -0.0344(7) 0.6971(5) 0.4468(5) 0.067 Uiso 1 calc R . C255 C -0.3073(16) 0.0114(13) -0.1215(12) 0.085(12) Uiso 0.50 d P . C257 C -0.3568(17) 0.0789(14) -0.1165(11) 0.082(12) Uiso 0.50 d P . C259 C 0.2871(27) 0.3120(21) 0.2643(20) 0.169(24) Uiso 0.50 d P . C260 C 0.2208(30) 0.3081(25) 0.2316(22) 0.186(28) Uiso 0.50 d P . C261 C 0.2211(28) 0.2593(23) 0.2211(20) 0.171(25) Uiso 0.50 d P . C262 C 0.2807(38) 0.2497(30) 0.2534(28) 0.249(39) Uiso 0.50 d P . C300 C 0.3409(9) 0.3566(7) 0.1897(7) 0.117(8) Uiso 1 d . . H30B H 0.3470(9) 0.3855(7) 0.1827(7) 0.175 Uiso 1 calc R . H30C H 0.3743(9) 0.3427(7) 0.2020(7) 0.175 Uiso 1 calc R . H30D H 0.3206(9) 0.3579(7) 0.2060(7) 0.175 Uiso 1 calc R . C301 C 0.3011(8) 0.3541(6) 0.1208(6) 0.091(7) Uiso 1 d . . H30E H 0.3142(8) 0.3833(6) 0.1260(6) 0.136 Uiso 1 calc R . H30F H 0.2636(8) 0.3548(6) 0.1071(6) 0.136 Uiso 1 calc R . H30G H 0.3193(8) 0.3396(6) 0.1065(6) 0.136 Uiso 1 calc R . C302 C 0.2962(10) 0.2898(8) 0.1565(8) 0.116(8) Uiso 1 d . . H30H H 0.3018(10) 0.2774(8) 0.1796(8) 0.139 Uiso 1 calc R . C303 C 0.0897(11) 0.7917(9) 0.4472(8) 0.144(10) Uiso 1 d . . H30I H 0.1028(11) 0.8123(9) 0.4337(8) 0.217 Uiso 1 calc R . H30J H 0.1003(11) 0.8002(9) 0.4726(8) 0.217 Uiso 1 calc R . H30K H 0.0516(11) 0.7906(9) 0.4369(8) 0.217 Uiso 1 calc R . C304 C 0.1409(10) 0.7456(8) 0.4203(7) 0.122(9) Uiso 1 d . . H30L H 0.1460(10) 0.7736(8) 0.4110(7) 0.183 Uiso 1 calc R . H30M H 0.1222(10) 0.7270(8) 0.4001(7) 0.183 Uiso 1 calc R . H30N H 0.1749(10) 0.7331(8) 0.4336(7) 0.183 Uiso 1 calc R . C305 C 0.0984(8) 0.7150(7) 0.4612(6) 0.083(6) Uiso 1 d . . H30O H 0.1129(8) 0.6885(7) 0.4580(6) 0.099 Uiso 1 calc R . C306 C 0.0050(10) 0.0914(8) 0.2880(8) 0.135(9) Uiso 1 d . . H30P H 0.0147(10) 0.0994(8) 0.2671(8) 0.202 Uiso 1 calc R . H30Q H -0.0286(10) 0.1043(8) 0.2860(8) 0.202 Uiso 1 calc R . H30R H 0.0022(10) 0.0604(8) 0.2889(8) 0.202 Uiso 1 calc R . C307 C 0.0921(11) 0.1288(9) 0.3192(8) 0.138(10) Uiso 1 d . . H30S H 0.0883(11) 0.1311(9) 0.2936(8) 0.207 Uiso 1 calc R . H30T H 0.1236(11) 0.1126(9) 0.3320(8) 0.207 Uiso 1 calc R . H30U H 0.0946(11) 0.1573(9) 0.3297(8) 0.207 Uiso 1 calc R . C308 C 0.0415(12) 0.0995(9) 0.3541(9) 0.136(10) Uiso 1 d . . H30V H 0.0121(12) 0.0839(9) 0.3547(9) 0.163 Uiso 1 calc R . C309 C 0.2315(29) 0.2947(22) 0.0048(17) 0.102(19) Uiso 0.50 d P . C310 C 0.1845(22) 0.2633(14) 0.0003(12) 0.066(13) Uiso 0.50 d P . C311 C 0.1432(21) 0.2943(17) -0.0240(14) 0.095(16) Uiso 0.50 d P . C312 C 0.3425(19) 0.4972(15) 0.6004(15) 0.100(15) Uiso 0.50 d P . C313 C 0.3218(21) 0.4873(16) 0.5457(15) 0.180(15) Uiso 0.50 d P . C314 C 0.2962(16) 0.4514(13) 0.5489(11) 0.085(12) Uiso 0.50 d P . C315 C -0.5458(17) 0.3844(14) 0.2985(12) 0.076(12) Uiso 0.50 d P . C316 C -0.5318(17) 0.3699(14) 0.3310(13) 0.091(13) Uiso 0.50 d P . C317 C -0.5261(16) 0.3687(13) 0.2716(11) 0.075(11) Uiso 0.50 d P . C318 C -0.0213(22) 0.2054(16) 0.2731(15) 0.115(16) Uiso 0.50 d P . C319 C -0.0564(20) 0.1874(16) 0.3187(17) 0.115(17) Uiso 0.50 d P . C320 C -0.0588(28) 0.1950(22) 0.2904(26) 0.135(25) Uiso 0.50 d P . C321 C -0.7239(15) 0.4919(12) 0.2438(11) 0.072(11) Uiso 0.50 d P . C322 C -0.6733(33) 0.5058(24) 0.2845(21) 0.169(25) Uiso 0.50 d P . C323 C -0.6280(27) 0.5287(21) 0.3089(19) 0.156(22) Uiso 0.50 d P . C324 C 0.2039(16) 0.6653(13) 0.0823(12) 0.085(12) Uiso 0.50 d P . C326 C 0.1978(38) 0.7092(33) 0.1039(29) 0.251(40) Uiso 0.50 d P . C327 C 0.2124(34) 0.7655(29) 0.1122(25) 0.223(35) Uiso 0.50 d P . C328 C 0.1749(24) 0.7056(21) 0.1381(18) 0.150(21) Uiso 0.50 d P . C329 C 0.1696(28) 0.7443(25) 0.1521(21) 0.183(27) Uiso 0.50 d P . C400 C -0.3215(44) 0.2917(31) -0.0757(29) 0.253(42) Uiso 0.50 d P . C401 C -0.5430(28) 0.3493(25) 0.2878(21) 0.170(26) Uiso 0.50 d P . C402 C -0.3705(33) 0.2911(23) -0.0775(20) 0.168(25) Uiso 0.50 d P . C403 C -0.4097(28) 0.2588(24) -0.0969(21) 0.169(25) Uiso 0.50 d P . C404 C -0.5883(39) 0.4049(30) 0.2864(27) 0.228(38) Uiso 0.50 d P . C405 C 0.4347(34) 0.2378(24) 0.5458(22) 0.183(27) Uiso 0.50 d P . C406 C 0.3549(32) 0.2461(25) 0.4992(25) 0.191(29) Uiso 0.50 d P . C407 C -0.0979(24) 0.1723(20) 0.2518(15) 0.098(15) Uiso 0.50 d P . C408 C -0.0705(24) 0.1949(17) 0.2692(19) 0.087(16) Uiso 0.50 d P . C409 C -0.1211(22) 0.1484(18) 0.2471(14) 0.108(17) Uiso 0.50 d P . C410 C 0.2249(23) 0.0799(18) 0.0974(16) 0.133(19) Uiso 0.50 d P . C411 C 0.1382(39) 0.0348(32) 0.0476(30) 0.257(42) Uiso 0.50 d P . C412 C 0.1851(30) 0.0742(24) 0.0380(22) 0.195(29) Uiso 0.50 d P . C413 C 0.4604(27) 0.2648(22) 0.5133(20) 0.177(26) Uiso 0.50 d P . C414 C -0.3584(40) 0.2213(33) -0.1959(30) 0.257(42) Uiso 0.50 d P . C415 C -0.3253(35) 0.1772(29) -0.1734(26) 0.227(35) Uiso 0.50 d P . C416 C -0.4175(32) 0.2219(27) -0.0716(24) 0.209(32) Uiso 0.50 d P . C417 C -0.2767(18) 0.5983(14) 0.3200(14) 0.091(13) Uiso 0.50 d P . C418 C -0.3688(26) 0.1119(23) -0.1105(19) 0.160(24) Uiso 0.50 d P . C420 C 0.2134(30) 0.2741(25) 0.0084(16) 0.102(20) Uiso 0.50 d P . C421 C 0.1733(25) 0.2285(18) 0.0143(16) 0.119(18) Uiso 0.50 d P . C422 C 0.4145(34) 0.3473(27) 0.5582(26) 0.224(34) Uiso 0.50 d P . C423 C 0.4433(31) 0.3346(25) 0.6046(24) 0.198(30) Uiso 0.50 d P . C424 C -0.2516(21) 0.0841(17) -0.1119(15) 0.124(17) Uiso 0.50 d P . C425 C -0.2937(28) 0.0548(23) -0.1466(22) 0.181(27) Uiso 0.50 d P . C426 C 0.0501(24) 0.1893(20) -0.0478(18) 0.145(21) Uiso 0.50 d P . C427 C 0.0802(51) 0.1528(42) -0.0192(37) 0.307(55) Uiso 0.50 d P . C428 C 0.1223(29) 0.1244(23) -0.0076(20) 0.167(24) Uiso 0.50 d P . C429 C -0.6990(51) 0.4770(37) 0.2813(35) 0.255(49) Uiso 0.50 d P . C430 C -0.4142(10) 0.1396(8) -0.0574(7) 0.121(9) Uiso 1 d . . C431 C -0.6619(38) 0.4581(31) 0.2676(26) 0.291(37) Uiso 0.50 d P . C432 C 0.1371(30) -0.0866(26) 0.0247(23) 0.200(30) Uiso 0.50 d P . C433 C -0.5155(40) 0.4778(33) 0.4002(30) 0.269(44) Uiso 0.50 d P . C434 C 0.4586(33) 0.2860(27) 0.5750(25) 0.221(33) Uiso 0.50 d P . C435 C -0.0700(32) 0.1866(25) 0.2306(25) 0.203(30) Uiso 0.50 d P . C436 C 0.1685(43) -0.1324(36) 0.0501(33) 0.289(48) Uiso 0.50 d P . C437 C -0.3722(64) 0.2096(54) -0.0970(48) 0.398(79) Uiso 0.50 d P . C438 C 0.3445(41) 0.4894(33) 0.5637(33) 0.132(45) Uiso 0.50 d P . C439 C 0.3851(43) 0.2313(30) 0.5326(30) 0.224(37) Uiso 0.50 d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.0510(12) 0.0479(10) 0.0102(8) 0.0022(7) 0.0068(8) -0.0014(9) Ga2 0.0409(11) 0.0484(10) 0.0088(8) 0.0011(7) 0.0020(8) -0.0005(8) Ga3 0.0518(12) 0.0422(10) 0.0208(9) -0.0035(8) 0.0092(8) 0.0018(9) Ga4 0.0526(13) 0.0738(13) 0.0227(9) -0.0008(9) 0.0180(9) 0.0079(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 O13 1.952(9) . ? Ga1 O7 1.953(9) . ? Ga1 O1 1.963(9) . ? Ga1 O8 1.998(9) . ? Ga1 O2 1.999(9) . ? Ga1 O14 2.009(9) . ? Ga2 O27 1.952(9) . ? Ga2 O18 1.963(9) . ? Ga2 O19 1.968(9) . ? Ga2 O20 1.993(9) . ? Ga2 O28 1.996(9) . ? Ga2 O17 2.002(9) . ? Ga3 O32 1.964(9) . ? Ga3 O5 1.965(9) . ? Ga3 O33 1.965(9) . ? Ga3 O6 1.975(9) . ? Ga3 O34 2.002(9) . ? Ga3 O31 2.014(9) . ? Ga4 O24 1.943(10) . ? Ga4 O12 1.967(10) . ? Ga4 O38 1.974(10) . ? Ga4 O37 1.976(9) . ? Ga4 O11 1.984(9) . ? Ga4 O23 2.001(9) . ? O1 C1 1.30(2) . ? O2 C2 1.34(2) . ? O3 C7 1.25(2) . ? O4 C18 1.25(2) . ? O5 C23 1.35(2) . ? O6 C24 1.342(14) . ? O7 C25 1.36(2) . ? O8 C26 1.312(15) . ? O9 C31 1.27(2) . ? O10 C42 1.28(2) . ? O11 C48 1.32(2) . ? O12 C47 1.37(2) . ? O13 C49 1.301(15) . ? O14 C50 1.351(14) . ? O15 C55 1.240(15) . ? O16 C66 1.216(15) . ? O17 C68 1.325(14) . ? O18 C69 1.325(15) . ? O19 C73 1.330(15) . ? O20 C74 1.348(14) . ? O21 C79 1.260(15) . ? O22 C90 1.22(2) . ? O23 C92 1.32(2) . ? O24 C93 1.31(2) . ? O27 C97 1.327(15) . ? O28 C98 1.314(14) . ? O29 C103 1.247(15) . ? O30 C114 1.28(2) . ? O31 C116 1.302(15) . ? O32 C117 1.34(2) . ? O33 C121 1.31(2) . ? O34 C122 1.37(2) . ? O35 C127 1.25(2) . ? O36 C138 1.23(2) . ? O37 C140 1.36(2) . ? O38 C141 1.32(2) . ? O100 C302 1.18(3) . ? O101 C305 1.19(2) . ? O102 C308 1.25(3) . ? O103 C421 0.91(6) . ? O103 C310 1.20(5) . ? O103 C420 1.32(7) . ? O104 C417 1.10(5) . ? O106 C309 0.78(8) . ? O106 C420 1.48(9) . ? O107 C437 1.98(16) . ? O107 C418 1.83(7) . ? O107 C430 1.92(4) . ? N1 C7 1.35(2) . ? N1 C8 1.42(2) . ? N2 C18 1.33(2) . ? N2 C13 1.44(2) . ? N3 C31 1.32(2) . ? N3 C32 1.40(2) . ? N4 C42 1.31(2) . ? N4 C37 1.42(2) . ? N5 C55 1.36(2) . ? N5 C56 1.41(2) . ? N6 C66 1.36(2) . ? N6 C61 1.44(2) . ? N7 C79 1.35(2) . ? N7 C80 1.42(2) . ? N8 C90 1.37(2) . ? N8 C85 1.40(2) . ? N9 C103 1.33(2) . ? N9 C104 1.42(2) . ? N10 C114 1.34(2) . ? N10 C109 1.40(2) . ? N11 C127 1.35(2) . ? N11 C128 1.41(2) . ? N12 C138 1.36(2) . ? N12 C133 1.40(2) . ? N13 C146 1.47(2) . ? N13 C145 1.48(2) . ? N13 C147 1.48(2) . ? N13 C148 1.50(2) . ? N14 C158 1.49(2) . ? N14 C155 1.51(2) . ? N14 C157 1.54(2) . ? N14 C156 1.56(2) . ? N15 C167 1.46(2) . ? N15 C165 1.47(2) . ? N15 C168 1.51(2) . ? N15 C166 1.53(2) . ? N16 C176 1.46(2) . ? N16 C177 1.47(2) . ? N16 C175 1.49(2) . ? N16 C178 1.52(2) . ? N17 C185 1.48(2) . ? N17 C186 1.49(2) . ? N17 C188 1.50(2) . ? N17 C187 1.52(2) . ? N18 C198 1.48(2) . ? N18 C196 1.49(2) . ? N18 C195 1.50(2) . ? N18 C197 1.51(2) . ? N19 C207 1.47(2) . ? N19 C208 1.48(2) . ? N19 C206 1.50(2) . ? N19 C205 1.51(2) . ? N20 C215 1.41(3) . ? N20 C217 1.50(4) . ? N20 C218 1.50(3) . ? N20 C216 1.56(4) . ? N21 C228 1.44(2) . ? N21 C225 1.47(2) . ? N21 C227 1.48(2) . ? N21 C226 1.55(2) . ? N22 C236 1.47(2) . ? N22 C235 1.49(2) . ? N22 C238 1.50(2) . ? N22 C237 1.52(2) . ? N23 C246 1.47(2) . ? N23 C245 1.47(2) . ? N23 C247 1.50(2) . ? N23 C248 1.53(2) . ? N24 C424 1.55(5) . ? N24 C257 1.67(4) . ? N24 C255 1.82(4) . ? N24 C425 1.90(8) . ? N100 C302 1.33(3) . ? N100 C301 1.46(2) . ? N100 C300 1.52(3) . ? N101 C305 1.36(2) . ? N101 C303 1.41(3) . ? N101 C304 1.44(2) . ? N102 C308 1.29(3) . ? N102 C307 1.43(3) . ? N102 C306 1.49(3) . ? N103 C311 0.75(7) . ? N103 C310 1.33(6) . ? N103 C421 1.93(9) . ? C1 C6 1.38(2) . ? C1 C2 1.45(2) . ? C2 C3 1.41(2) . ? C3 C4 1.42(2) . ? C3 C7 1.42(2) . ? C4 C5 1.39(2) . ? C5 C6 1.39(2) . ? C8 C17 1.36(2) . ? C8 C9 1.40(2) . ? C9 C10 1.39(2) . ? C9 C14 1.44(2) . ? C10 C11 1.35(2) . ? C11 C12 1.42(2) . ? C12 C13 1.33(2) . ? C13 C14 1.44(2) . ? C14 C15 1.42(2) . ? C15 C16 1.32(2) . ? C16 C17 1.41(2) . ? C18 C19 1.47(2) . ? C19 C24 1.38(2) . ? C19 C20 1.43(2) . ? C20 C21 1.34(2) . ? C21 C22 1.40(2) . ? C22 C23 1.38(2) . ? C23 C24 1.41(2) . ? C25 C30 1.36(2) . ? C25 C26 1.44(2) . ? C26 C27 1.40(2) . ? C27 C28 1.38(2) . ? C27 C31 1.50(2) . ? C28 C29 1.34(2) . ? C29 C30 1.44(2) . ? C32 C41 1.39(2) . ? C32 C33 1.39(2) . ? C33 C34 1.43(2) . ? C33 C38 1.43(2) . ? C34 C35 1.35(2) . ? C35 C36 1.40(2) . ? C36 C37 1.36(2) . ? C37 C38 1.41(2) . ? C38 C39 1.45(2) . ? C39 C40 1.31(2) . ? C40 C41 1.43(2) . ? C42 C43 1.48(2) . ? C43 C44 1.40(2) . ? C43 C48 1.41(2) . ? C44 C45 1.40(2) . ? C45 C46 1.43(3) . ? C46 C47 1.32(2) . ? C47 C48 1.40(2) . ? C49 C54 1.38(2) . ? C49 C50 1.50(2) . ? C50 C51 1.35(2) . ? C51 C52 1.39(2) . ? C51 C55 1.51(2) . ? C52 C53 1.41(2) . ? C53 C54 1.38(2) . ? C56 C65 1.38(2) . ? C56 C57 1.38(2) . ? C57 C58 1.41(2) . ? C57 C62 1.45(2) . ? C58 C59 1.35(2) . ? C59 C60 1.42(2) . ? C60 C61 1.34(2) . ? C61 C62 1.43(2) . ? C62 C63 1.41(2) . ? C63 C64 1.37(2) . ? C64 C65 1.44(2) . ? C66 C67 1.50(2) . ? C67 C68 1.37(2) . ? C67 C72 1.45(2) . ? C68 C69 1.43(2) . ? C69 C70 1.36(2) . ? C70 C71 1.40(2) . ? C71 C72 1.37(2) . ? C73 C74 1.40(2) . ? C73 C78 1.41(2) . ? C74 C75 1.39(2) . ? C75 C79 1.43(2) . ? C75 C76 1.46(2) . ? C76 C77 1.33(2) . ? C77 C78 1.40(2) . ? C80 C89 1.34(2) . ? C80 C81 1.43(2) . ? C81 C82 1.40(2) . ? C81 C86 1.43(2) . ? C82 C83 1.36(2) . ? C83 C84 1.37(2) . ? C84 C85 1.37(2) . ? C85 C86 1.43(2) . ? C86 C87 1.43(2) . ? C87 C88 1.34(2) . ? C88 C89 1.43(2) . ? C90 C91 1.47(2) . ? C91 C92 1.38(2) . ? C91 C96 1.42(2) . ? C92 C93 1.44(2) . ? C93 C94 1.38(2) . ? C94 C95 1.36(2) . ? C95 C96 1.35(2) . ? C97 C102 1.37(2) . ? C97 C98 1.46(2) . ? C98 C99 1.40(2) . ? C99 C100 1.43(2) . ? C99 C103 1.48(2) . ? C100 C101 1.36(2) . ? C101 C102 1.37(2) . ? C104 C113 1.38(2) . ? C104 C105 1.38(2) . ? C105 C106 1.41(2) . ? C105 C110 1.43(2) . ? C106 C107 1.36(2) . ? C107 C108 1.43(2) . ? C108 C109 1.36(2) . ? C109 C110 1.38(2) . ? C110 C111 1.42(2) . ? C111 C112 1.36(2) . ? C112 C113 1.44(3) . ? C114 C115 1.48(2) . ? C115 C120 1.39(2) . ? C115 C116 1.42(2) . ? C116 C117 1.42(2) . ? C117 C118 1.39(2) . ? C118 C119 1.46(2) . ? C119 C120 1.36(2) . ? C121 C126 1.41(2) . ? C121 C122 1.43(2) . ? C122 C123 1.36(2) . ? C123 C124 1.43(2) . ? C123 C127 1.46(2) . ? C124 C125 1.36(2) . ? C125 C126 1.39(2) . ? C128 C137 1.34(2) . ? C128 C129 1.43(2) . ? C129 C130 1.39(2) . ? C129 C134 1.44(2) . ? C130 C131 1.38(2) . ? C131 C132 1.43(2) . ? C132 C133 1.37(2) . ? C133 C134 1.40(2) . ? C134 C135 1.38(2) . ? C135 C136 1.37(2) . ? C136 C137 1.44(2) . ? C138 C139 1.48(2) . ? C139 C140 1.36(2) . ? C139 C144 1.41(2) . ? C140 C141 1.44(2) . ? C141 C142 1.41(2) . ? C142 C143 1.38(2) . ? C143 C144 1.38(2) . ? C148 C149 1.49(2) . ? C149 C150 1.33(2) . ? C149 C154 1.42(2) . ? C150 C151 1.39(2) . ? C151 C152 1.37(3) . ? C152 C153 1.36(3) . ? C153 C154 1.41(3) . ? C156 C160 1.41(3) . ? C158 C410 1.44(6) . ? C159 C162 1.42(2) . ? C159 C160 1.42(2) . ? C160 C161 1.40(2) . ? C161 C163 1.42(2) . ? C162 C164 1.40(2) . ? C163 C164 1.42(2) . ? C168 C169 1.49(2) . ? C169 C170 1.39(2) . ? C169 C174 1.41(2) . ? C170 C171 1.37(2) . ? C171 C172 1.36(2) . ? C172 C173 1.35(2) . ? C173 C174 1.38(2) . ? C178 C179 1.51(2) . ? C179 C180 1.35(2) . ? C179 C184 1.39(2) . ? C180 C181 1.46(3) . ? C181 C182 1.32(3) . ? C182 C183 1.21(3) . ? C183 C184 1.49(3) . ? C188 C189 1.50(2) . ? C189 C190 1.38(3) . ? C189 C194 1.43(3) . ? C190 C191 1.40(3) . ? C191 C192 1.39(3) . ? C192 C193 1.38(3) . ? C193 C194 1.36(3) . ? C197 C199 1.51(2) . ? C199 C204 1.35(2) . ? C199 C200 1.36(2) . ? C200 C201 1.47(2) . ? C201 C202 1.32(2) . ? C202 C203 1.33(2) . ? C203 C204 1.42(2) . ? C205 C209 1.49(2) . ? C209 C210 1.37(2) . ? C209 C214 1.43(2) . ? C210 C211 1.38(3) . ? C211 C212 1.38(3) . ? C212 C213 1.33(3) . ? C213 C214 1.38(3) . ? C218 C219 1.63(4) . ? C219 C220 1.36(2) . ? C219 C224 1.39(2) . ? C220 C221 1.39(2) . ? C221 C222 1.35(2) . ? C222 C223 1.38(2) . ? C223 C224 1.37(2) . ? C226 C230 1.48(2) . ? C229 C233 1.27(4) . ? C229 C232 1.39(3) . ? C230 C232 1.34(2) . ? C230 C231 1.38(3) . ? C231 C234 1.60(3) . ? C233 C234 1.29(3) . ? C237 C239 1.48(2) . ? C239 C240 1.40(2) . ? C239 C244 1.40(2) . ? C240 C241 1.41(2) . ? C241 C242 1.31(3) . ? C242 C243 1.39(3) . ? C243 C244 1.38(3) . ? C248 C249 1.47(2) . ? C249 C254 1.40(2) . ? C249 C250 1.42(2) . ? C250 C251 1.39(2) . ? C251 C252 1.36(2) . ? C252 C253 1.38(2) . ? C253 C254 1.36(2) . ? C255 C425 1.76(8) . ? C257 C418 1.11(6) . ? C259 C260 1.79(9) . ? C259 C262 1.96(10) . ? C260 C261 1.56(8) . ? C261 C262 1.68(10) . ? C309 C420 0.84(8) . ? C309 C310 1.55(9) . ? C310 C420 0.80(7) . ? C310 C421 1.28(6) . ? C310 C311 1.52(7) . ? C311 C420 1.97(8) . ? C312 C438 1.45(11) . ? C312 C313 2.01(10) . ? C313 C438 0.75(12) . ? C313 C314 1.33(9) . ? C314 C438 1.69(11) . ? C315 C401 1.17(7) . ? C315 C404 1.25(9) . ? C315 C316 1.26(5) . ? C315 C317 1.40(5) . ? C316 C401 1.71(8) . ? C317 C401 1.07(7) . ? C318 C408 1.31(7) . ? C318 C320 1.42(9) . ? C318 C435 1.81(9) . ? C319 C320 1.09(8) . ? C319 C408 1.83(8) . ? C320 C408 0.77(8) . ? C320 C407 1.65(9) . ? C321 C429 1.45(12) . ? C321 C322 1.74(9) . ? C321 C431 1.91(12) . ? C322 C429 1.10(12) . ? C322 C323 1.44(8) . ? C322 C431 1.68(12) . ? C324 C326 1.63(10) . ? C326 C328 1.63(10) . ? C326 C327 1.79(11) . ? C328 C329 1.34(8) . ? C400 C402 1.29(10) . ? C402 C403 1.45(8) . ? C403 C416 1.56(9) . ? C403 C437 1.82(16) . ? C405 C439 1.26(10) . ? C405 C413 1.82(9) . ? C405 C434 1.84(10) . ? C406 C439 1.35(10) . ? C407 C409 0.94(6) . ? C407 C408 1.07(6) . ? C407 C435 1.36(9) . ? C408 C435 1.51(10) . ? C408 C409 1.95(8) . ? C411 C412 1.87(11) . ? C414 C415 1.69(11) . ? C416 C437 1.84(16) . ? C420 C421 1.83(10) . ? C422 C423 1.73(11) . ? C423 C434 2.01(11) . ? C424 C425 1.69(8) . ? C426 C427 1.59(13) . ? C427 C428 1.38(12) . ? C429 C431 1.40(13) . ? C432 C436 1.76(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O13 Ga1 O7 89.4(4) . . ? O13 Ga1 O1 93.3(4) . . ? O7 Ga1 O1 90.2(4) . . ? O13 Ga1 O8 169.5(4) . . ? O7 Ga1 O8 83.7(4) . . ? O1 Ga1 O8 94.8(4) . . ? O13 Ga1 O2 94.6(4) . . ? O7 Ga1 O2 171.8(4) . . ? O1 Ga1 O2 82.5(4) . . ? O8 Ga1 O2 93.2(4) . . ? O13 Ga1 O14 82.6(4) . . ? O7 Ga1 O14 94.8(4) . . ? O1 Ga1 O14 173.5(4) . . ? O8 Ga1 O14 90.0(4) . . ? O2 Ga1 O14 92.8(4) . . ? O27 Ga2 O18 92.4(4) . . ? O27 Ga2 O19 93.4(4) . . ? O18 Ga2 O19 91.2(4) . . ? O27 Ga2 O20 173.5(4) . . ? O18 Ga2 O20 92.9(4) . . ? O19 Ga2 O20 82.8(4) . . ? O27 Ga2 O28 82.3(4) . . ? O18 Ga2 O28 173.4(4) . . ? O19 Ga2 O28 93.2(4) . . ? O20 Ga2 O28 92.6(4) . . ? O27 Ga2 O17 94.0(4) . . ? O18 Ga2 O17 82.4(4) . . ? O19 Ga2 O17 170.4(4) . . ? O20 Ga2 O17 90.4(3) . . ? O28 Ga2 O17 93.8(3) . . ? O32 Ga3 O5 95.2(4) . . ? O32 Ga3 O33 90.4(4) . . ? O5 Ga3 O33 91.3(4) . . ? O32 Ga3 O6 172.7(4) . . ? O5 Ga3 O6 83.0(4) . . ? O33 Ga3 O6 96.7(4) . . ? O32 Ga3 O34 95.0(4) . . ? O5 Ga3 O34 168.6(4) . . ? O33 Ga3 O34 83.6(4) . . ? O6 Ga3 O34 87.5(4) . . ? O32 Ga3 O31 83.3(4) . . ? O5 Ga3 O31 93.3(4) . . ? O33 Ga3 O31 172.5(4) . . ? O6 Ga3 O31 89.7(4) . . ? O34 Ga3 O31 92.8(4) . . ? O24 Ga4 O12 89.4(4) . . ? O24 Ga4 O38 92.1(4) . . ? O12 Ga4 O38 92.2(4) . . ? O24 Ga4 O37 173.8(4) . . ? O12 Ga4 O37 94.6(4) . . ? O38 Ga4 O37 83.0(4) . . ? O24 Ga4 O11 93.8(4) . . ? O12 Ga4 O11 83.9(4) . . ? O38 Ga4 O11 172.8(4) . . ? O37 Ga4 O11 91.3(4) . . ? O24 Ga4 O23 83.2(4) . . ? O12 Ga4 O23 169.9(4) . . ? O38 Ga4 O23 95.0(4) . . ? O37 Ga4 O23 93.3(4) . . ? O11 Ga4 O23 89.7(4) . . ? C1 O1 Ga1 112.8(9) . . ? C2 O2 Ga1 111.8(8) . . ? C23 O5 Ga3 111.2(8) . . ? C24 O6 Ga3 112.7(8) . . ? C25 O7 Ga1 111.4(8) . . ? C26 O8 Ga1 111.4(8) . . ? C48 O11 Ga4 109.6(8) . . ? C47 O12 Ga4 109.3(10) . . ? C49 O13 Ga1 113.9(8) . . ? C50 O14 Ga1 111.5(8) . . ? C68 O17 Ga2 111.5(8) . . ? C69 O18 Ga2 113.2(8) . . ? C73 O19 Ga2 109.7(8) . . ? C74 O20 Ga2 110.3(8) . . ? C92 O23 Ga4 111.0(9) . . ? C93 O24 Ga4 112.7(9) . . ? C97 O27 Ga2 112.7(8) . . ? C98 O28 Ga2 112.5(8) . . ? C116 O31 Ga3 110.1(8) . . ? C117 O32 Ga3 111.0(8) . . ? C121 O33 Ga3 111.0(8) . . ? C122 O34 Ga3 111.2(8) . . ? C140 O37 Ga4 111.2(8) . . ? C141 O38 Ga4 110.7(9) . . ? C421 O103 C310 73.1(46) . . ? C421 O103 C420 108.6(56) . . ? C310 O103 C420 36.7(30) . . ? C309 O106 C420 24.9(64) . . ? C437 O107 C418 106.9(60) . . ? C437 O107 C430 103.7(54) . . ? C418 O107 C430 98.5(29) . . ? C7 N1 C8 131.2(12) . . ? C18 N2 C13 127.2(13) . . ? C31 N3 C32 130.7(13) . . ? C42 N4 C37 127.9(14) . . ? C55 N5 C56 126.8(12) . . ? C66 N6 C61 126.7(11) . . ? C79 N7 C80 126.2(12) . . ? C90 N8 C85 129.2(13) . . ? C103 N9 C104 129.2(12) . . ? C114 N10 C109 127.6(13) . . ? C127 N11 C128 128.1(13) . . ? C138 N12 C133 128.2(13) . . ? C146 N13 C145 107.0(14) . . ? C146 N13 C147 109.5(14) . . ? C145 N13 C147 107.7(14) . . ? C146 N13 C148 111.8(13) . . ? C145 N13 C148 108.4(13) . . ? C147 N13 C148 112.2(13) . . ? C158 N14 C155 109.2(14) . . ? C158 N14 C157 109.8(14) . . ? C155 N14 C157 108.8(14) . . ? C158 N14 C156 111.9(14) . . ? C155 N14 C156 107.3(14) . . ? C157 N14 C156 109.7(14) . . ? C167 N15 C165 109.0(14) . . ? C167 N15 C168 109.9(14) . . ? C165 N15 C168 111.0(13) . . ? C167 N15 C166 107.7(14) . . ? C165 N15 C166 109.5(13) . . ? C168 N15 C166 109.7(13) . . ? C176 N16 C177 108.7(12) . . ? C176 N16 C175 108.2(11) . . ? C177 N16 C175 108.0(11) . . ? C176 N16 C178 111.1(12) . . ? C177 N16 C178 113.4(12) . . ? C175 N16 C178 107.2(11) . . ? C185 N17 C186 109.7(13) . . ? C185 N17 C188 112.6(13) . . ? C186 N17 C188 107.5(13) . . ? C185 N17 C187 110.9(13) . . ? C186 N17 C187 106.8(13) . . ? C188 N17 C187 109.1(13) . . ? C198 N18 C196 108.2(12) . . ? C198 N18 C195 108.0(13) . . ? C196 N18 C195 109.5(12) . . ? C198 N18 C197 111.5(12) . . ? C196 N18 C197 112.6(12) . . ? C195 N18 C197 106.9(11) . . ? C207 N19 C208 106.9(12) . . ? C207 N19 C206 109.9(12) . . ? C208 N19 C206 108.5(12) . . ? C207 N19 C205 111.7(12) . . ? C208 N19 C205 108.1(11) . . ? C206 N19 C205 111.5(11) . . ? C215 N20 C217 102.6(28) . . ? C215 N20 C218 124.6(31) . . ? C217 N20 C218 107.0(28) . . ? C215 N20 C216 113.5(28) . . ? C217 N20 C216 109.9(30) . . ? C218 N20 C216 98.8(26) . . ? C228 N21 C225 111.6(13) . . ? C228 N21 C227 108.0(13) . . ? C225 N21 C227 107.2(12) . . ? C228 N21 C226 110.6(12) . . ? C225 N21 C226 108.0(12) . . ? C227 N21 C226 111.4(11) . . ? C236 N22 C235 110.3(12) . . ? C236 N22 C238 110.6(12) . . ? C235 N22 C238 107.0(11) . . ? C236 N22 C237 108.9(11) . . ? C235 N22 C237 107.7(12) . . ? C238 N22 C237 112.3(11) . . ? C246 N23 C245 110.7(12) . . ? C246 N23 C247 107.3(11) . . ? C245 N23 C247 108.9(11) . . ? C246 N23 C248 108.7(11) . . ? C245 N23 C248 112.0(11) . . ? C247 N23 C248 109.1(11) . . ? C424 N24 C257 118.4(28) . . ? C424 N24 C255 103.6(27) . . ? C257 N24 C255 92.0(23) . . ? C424 N24 C425 57.6(28) . . ? C257 N24 C425 87.1(29) . . ? C255 N24 C425 56.5(25) . . ? C302 N100 C301 122.5(21) . . ? C302 N100 C300 123.1(21) . . ? C301 N100 C300 114.3(17) . . ? C305 N101 C303 121.7(20) . . ? C305 N101 C304 120.4(19) . . ? C303 N101 C304 117.5(20) . . ? C308 N102 C307 122.3(25) . . ? C308 N102 C306 119.8(24) . . ? C307 N102 C306 117.9(21) . . ? C311 N103 C310 89.0(82) . . ? C311 N103 C421 129.8(93) . . ? C310 N103 C421 41.5(33) . . ? O1 C1 C6 125.0(14) . . ? O1 C1 C2 117.4(13) . . ? C6 C1 C2 117.6(14) . . ? O2 C2 C3 124.5(12) . . ? O2 C2 C1 114.7(12) . . ? C3 C2 C1 120.7(13) . . ? C2 C3 C4 117.4(13) . . ? C2 C3 C7 124.4(14) . . ? C4 C3 C7 118.0(13) . . ? C5 C4 C3 122.6(15) . . ? C4 C5 C6 118.7(17) . . ? C1 C6 C5 123.0(16) . . ? O3 C7 N1 120.8(13) . . ? O3 C7 C3 121.1(14) . . ? N1 C7 C3 118.0(13) . . ? C17 C8 C9 122.2(14) . . ? C17 C8 N1 121.9(13) . . ? C9 C8 N1 115.7(12) . . ? C10 C9 C8 125.0(13) . . ? C10 C9 C14 118.0(13) . . ? C8 C9 C14 117.1(12) . . ? C11 C10 C9 122.3(14) . . ? C10 C11 C12 120.4(15) . . ? C13 C12 C11 119.6(15) . . ? C12 C13 C14 122.0(14) . . ? C12 C13 N2 120.2(14) . . ? C14 C13 N2 117.9(13) . . ? C15 C14 C13 122.8(14) . . ? C15 C14 C9 119.5(13) . . ? C13 C14 C9 117.7(13) . . ? C16 C15 C14 119.9(15) . . ? C15 C16 C17 122.5(15) . . ? C8 C17 C16 118.7(15) . . ? O4 C18 N2 123.3(14) . . ? O4 C18 C19 121.1(14) . . ? N2 C18 C19 115.7(13) . . ? C24 C19 C20 119.4(13) . . ? C24 C19 C18 123.1(13) . . ? C20 C19 C18 117.4(13) . . ? C21 C20 C19 119.5(14) . . ? C20 C21 C22 121.3(15) . . ? C23 C22 C21 120.7(14) . . ? O5 C23 C22 123.6(13) . . ? O5 C23 C24 117.8(12) . . ? C22 C23 C24 118.7(13) . . ? O6 C24 C19 124.2(12) . . ? O6 C24 C23 115.2(12) . . ? C19 C24 C23 120.5(13) . . ? O7 C25 C30 122.0(13) . . ? O7 C25 C26 116.2(12) . . ? C30 C25 C26 121.7(14) . . ? O8 C26 C27 125.5(13) . . ? O8 C26 C25 117.0(12) . . ? C27 C26 C25 117.4(12) . . ? C28 C27 C26 120.5(14) . . ? C28 C27 C31 118.1(13) . . ? C26 C27 C31 121.3(13) . . ? C29 C28 C27 121.4(16) . . ? C28 C29 C30 120.9(17) . . ? C25 C30 C29 118.0(15) . . ? O9 C31 N3 123.3(14) . . ? O9 C31 C27 117.2(13) . . ? N3 C31 C27 119.4(13) . . ? C41 C32 C33 120.4(14) . . ? C41 C32 N3 120.1(13) . . ? C33 C32 N3 119.5(13) . . ? C32 C33 C34 122.6(13) . . ? C32 C33 C38 120.0(13) . . ? C34 C33 C38 117.3(13) . . ? C35 C34 C33 119.9(15) . . ? C34 C35 C36 123.1(15) . . ? C37 C36 C35 119.1(14) . . ? C36 C37 C38 120.3(13) . . ? C36 C37 N4 121.0(13) . . ? C38 C37 N4 118.6(12) . . ? C37 C38 C33 120.3(13) . . ? C37 C38 C39 122.0(13) . . ? C33 C38 C39 117.7(13) . . ? C40 C39 C38 120.9(16) . . ? C39 C40 C41 122.0(17) . . ? C32 C41 C40 118.9(15) . . ? O10 C42 N4 122.0(16) . . ? O10 C42 C43 118.7(16) . . ? N4 C42 C43 119.2(16) . . ? C44 C43 C48 119.5(16) . . ? C44 C43 C42 118.6(16) . . ? C48 C43 C42 121.7(15) . . ? C45 C44 C43 120.9(19) . . ? C44 C45 C46 117.1(19) . . ? C47 C46 C45 122.4(19) . . ? C46 C47 O12 122.3(16) . . ? C46 C47 C48 121.3(17) . . ? O12 C47 C48 116.4(14) . . ? O11 C48 C47 118.4(13) . . ? O11 C48 C43 122.8(14) . . ? C47 C48 C43 118.7(14) . . ? O13 C49 C54 127.6(13) . . ? O13 C49 C50 115.9(12) . . ? C54 C49 C50 116.5(13) . . ? O14 C50 C51 127.5(12) . . ? O14 C50 C49 113.7(11) . . ? C51 C50 C49 118.7(12) . . ? C50 C51 C52 122.9(13) . . ? C50 C51 C55 121.7(12) . . ? C52 C51 C55 115.3(12) . . ? C51 C52 C53 118.8(14) . . ? C54 C53 C52 119.7(15) . . ? C49 C54 C53 123.3(14) . . ? O15 C55 N5 122.6(13) . . ? O15 C55 C51 120.3(13) . . ? N5 C55 C51 117.1(12) . . ? C65 C56 C57 120.8(13) . . ? C65 C56 N5 119.2(12) . . ? C57 C56 N5 120.0(12) . . ? C56 C57 C58 121.1(12) . . ? C56 C57 C62 120.3(12) . . ? C58 C57 C62 118.6(12) . . ? C59 C58 C57 120.2(14) . . ? C58 C59 C60 121.8(14) . . ? C61 C60 C59 120.2(13) . . ? C60 C61 C62 120.7(13) . . ? C60 C61 N6 122.7(12) . . ? C62 C61 N6 116.6(11) . . ? C63 C62 C61 124.2(12) . . ? C63 C62 C57 117.4(12) . . ? C61 C62 C57 118.3(12) . . ? C64 C63 C62 122.1(13) . . ? C63 C64 C65 119.4(14) . . ? C56 C65 C64 119.8(13) . . ? O16 C66 N6 124.3(13) . . ? O16 C66 C67 123.1(13) . . ? N6 C66 C67 112.5(12) . . ? C68 C67 C72 119.4(13) . . ? C68 C67 C66 126.7(13) . . ? C72 C67 C66 113.6(12) . . ? O17 C68 C67 124.0(12) . . ? O17 C68 C69 116.9(12) . . ? C67 C68 C69 119.2(12) . . ? O18 C69 C70 123.0(13) . . ? O18 C69 C68 116.0(12) . . ? C70 C69 C68 120.9(13) . . ? C69 C70 C71 119.9(15) . . ? C72 C71 C70 121.2(15) . . ? C71 C72 C67 119.2(15) . . ? O19 C73 C74 118.9(12) . . ? O19 C73 C78 122.7(12) . . ? C74 C73 C78 118.4(12) . . ? O20 C74 C75 121.6(11) . . ? O20 C74 C73 115.2(11) . . ? C75 C74 C73 123.2(12) . . ? C74 C75 C79 125.9(12) . . ? C74 C75 C76 115.9(12) . . ? C79 C75 C76 118.2(12) . . ? C77 C76 C75 120.5(13) . . ? C76 C77 C78 123.1(14) . . ? C77 C78 C73 118.9(14) . . ? O21 C79 N7 119.8(13) . . ? O21 C79 C75 124.3(12) . . ? N7 C79 C75 115.9(12) . . ? C89 C80 N7 121.9(13) . . ? C89 C80 C81 120.0(14) . . ? N7 C80 C81 118.2(12) . . ? C82 C81 C80 121.3(13) . . ? C82 C81 C86 118.5(13) . . ? C80 C81 C86 120.1(13) . . ? C83 C82 C81 120.3(15) . . ? C82 C83 C84 121.5(15) . . ? C85 C84 C83 121.9(15) . . ? C84 C85 N8 123.4(14) . . ? C84 C85 C86 118.1(14) . . ? N8 C85 C86 118.3(13) . . ? C85 C86 C81 119.6(13) . . ? C85 C86 C87 123.2(13) . . ? C81 C86 C87 117.2(13) . . ? C88 C87 C86 121.0(14) . . ? C87 C88 C89 121.1(14) . . ? C80 C89 C88 120.6(14) . . ? O22 C90 N8 121.3(14) . . ? O22 C90 C91 123.7(14) . . ? N8 C90 C91 114.8(13) . . ? C92 C91 C96 118.7(14) . . ? C92 C91 C90 125.4(14) . . ? C96 C91 C90 115.7(13) . . ? O23 C92 C91 124.2(14) . . ? O23 C92 C93 115.8(12) . . ? C91 C92 C93 119.9(13) . . ? O24 C93 C94 125.3(14) . . ? O24 C93 C92 117.3(13) . . ? C94 C93 C92 117.3(14) . . ? C95 C94 C93 123.1(16) . . ? C96 C95 C94 119.0(17) . . ? C95 C96 C91 122.0(16) . . ? O27 C97 C102 125.3(12) . . ? O27 C97 C98 116.3(12) . . ? C102 C97 C98 118.3(12) . . ? O28 C98 C99 124.9(12) . . ? O28 C98 C97 115.0(12) . . ? C99 C98 C97 120.1(12) . . ? C98 C99 C100 117.1(12) . . ? C98 C99 C103 124.1(12) . . ? C100 C99 C103 118.6(12) . . ? C101 C100 C99 121.9(14) . . ? C100 C101 C102 120.3(14) . . ? C101 C102 C97 122.2(13) . . ? O29 C103 N9 124.1(13) . . ? O29 C103 C99 119.5(13) . . ? N9 C103 C99 116.2(12) . . ? C113 C104 C105 120.6(14) . . ? C113 C104 N9 119.4(14) . . ? C105 C104 N9 120.0(12) . . ? C104 C105 C106 120.7(13) . . ? C104 C105 C110 122.9(13) . . ? C106 C105 C110 116.3(14) . . ? C107 C106 C105 119.6(17) . . ? C106 C107 C108 122.8(19) . . ? C109 C108 C107 118.8(18) . . ? C108 C109 C110 118.9(15) . . ? C108 C109 N10 118.8(15) . . ? C110 C109 N10 122.1(13) . . ? C109 C110 C111 120.3(14) . . ? C109 C110 C105 123.3(13) . . ? C111 C110 C105 116.4(14) . . ? C112 C111 C110 119.9(17) . . ? C111 C112 C113 123.1(21) . . ? C104 C113 C112 117.0(18) . . ? O30 C114 N10 121.8(15) . . ? O30 C114 C115 118.5(14) . . ? N10 C114 C115 119.7(14) . . ? C120 C115 C116 119.5(13) . . ? C120 C115 C114 118.7(13) . . ? C116 C115 C114 121.8(13) . . ? O31 C116 C117 118.4(12) . . ? O31 C116 C115 123.3(12) . . ? C117 C116 C115 118.2(13) . . ? O32 C117 C118 121.8(12) . . ? O32 C117 C116 117.0(12) . . ? C118 C117 C116 121.1(13) . . ? C117 C118 C119 120.0(14) . . ? C120 C119 C118 117.1(15) . . ? C119 C120 C115 124.0(15) . . ? O33 C121 C126 122.4(13) . . ? O33 C121 C122 120.4(12) . . ? C126 C121 C122 117.2(13) . . ? C123 C122 O34 123.9(12) . . ? C123 C122 C121 122.2(13) . . ? O34 C122 C121 113.7(12) . . ? C122 C123 C124 118.1(13) . . ? C122 C123 C127 124.8(14) . . ? C124 C123 C127 117.1(14) . . ? C125 C124 C123 121.5(15) . . ? C124 C125 C126 119.9(16) . . ? C125 C126 C121 121.0(14) . . ? O35 C127 N11 121.2(15) . . ? O35 C127 C123 122.0(14) . . ? N11 C127 C123 116.8(14) . . ? C137 C128 N11 121.4(15) . . ? C137 C128 C129 120.9(15) . . ? N11 C128 C129 117.7(13) . . ? C130 C129 C128 121.2(15) . . ? C130 C129 C134 118.9(14) . . ? C128 C129 C134 119.8(14) . . ? C131 C130 C129 120.7(17) . . ? C130 C131 C132 120.2(19) . . ? C133 C132 C131 120.0(18) . . ? C132 C133 C134 120.4(15) . . ? C132 C133 N12 120.2(15) . . ? C134 C133 N12 119.4(14) . . ? C135 C134 C133 122.8(14) . . ? C135 C134 C129 117.5(14) . . ? C133 C134 C129 119.6(13) . . ? C136 C135 C134 121.9(17) . . ? C135 C136 C137 121.0(19) . . ? C128 C137 C136 118.7(18) . . ? O36 C138 N12 121.2(15) . . ? O36 C138 C139 121.6(15) . . ? N12 C138 C139 117.1(14) . . ? C140 C139 C144 119.3(14) . . ? C140 C139 C138 124.5(14) . . ? C144 C139 C138 115.9(14) . . ? O37 C140 C139 125.1(13) . . ? O37 C140 C141 114.5(12) . . ? C139 C140 C141 120.4(14) . . ? O38 C141 C142 123.7(14) . . ? O38 C141 C140 117.9(13) . . ? C142 C141 C140 118.4(14) . . ? C143 C142 C141 120.5(15) . . ? C144 C143 C142 119.4(16) . . ? C143 C144 C139 121.9(16) . . ? C149 C148 N13 114.2(13) . . ? C150 C149 C154 120.6(18) . . ? C150 C149 C148 121.3(17) . . ? C154 C149 C148 118.1(16) . . ? C149 C150 C151 120.5(19) . . ? C152 C151 C150 120.4(21) . . ? C153 C152 C151 120.5(22) . . ? C152 C153 C154 119.5(22) . . ? C153 C154 C149 118.4(20) . . ? C160 C156 N14 113.8(15) . . ? C410 C158 N14 115.6(26) . . ? C162 C159 C160 119.1(14) . . ? C161 C160 C156 118.1(24) . . ? C161 C160 C159 120.7(15) . . ? C156 C160 C159 121.2(24) . . ? C160 C161 C163 120.2(15) . . ? C164 C162 C159 119.7(15) . . ? C164 C163 C161 118.9(15) . . ? C162 C164 C163 120.5(15) . . ? C169 C168 N15 115.3(15) . . ? C170 C169 C174 118.7(17) . . ? C170 C169 C168 119.7(17) . . ? C174 C169 C168 121.5(17) . . ? C171 C170 C169 121.6(18) . . ? C172 C171 C170 118.1(18) . . ? C173 C172 C171 122.4(20) . . ? C172 C173 C174 120.8(19) . . ? C173 C174 C169 118.4(18) . . ? C179 C178 N16 112.4(13) . . ? C180 C179 C184 120.2(19) . . ? C180 C179 C178 118.7(16) . . ? C184 C179 C178 121.1(17) . . ? C179 C180 C181 119.8(19) . . ? C182 C181 C180 116.5(23) . . ? C183 C182 C181 127.1(27) . . ? C182 C183 C184 120.5(23) . . ? C179 C184 C183 115.7(20) . . ? C189 C188 N17 114.8(15) . . ? C190 C189 C194 117.6(19) . . ? C190 C189 C188 122.7(18) . . ? C194 C189 C188 119.6(18) . . ? C189 C190 C191 120.4(23) . . ? C192 C191 C190 121.3(27) . . ? C193 C192 C191 118.0(27) . . ? C194 C193 C192 121.7(26) . . ? C193 C194 C189 120.9(23) . . ? C199 C197 N18 115.4(12) . . ? C204 C199 C200 120.3(16) . . ? C204 C199 C197 119.9(15) . . ? C200 C199 C197 119.7(15) . . ? C199 C200 C201 119.2(17) . . ? C202 C201 C200 116.7(18) . . ? C201 C202 C203 125.5(20) . . ? C202 C203 C204 117.6(19) . . ? C199 C204 C203 120.6(17) . . ? C209 C205 N19 115.6(13) . . ? C210 C209 C214 118.3(17) . . ? C210 C209 C205 120.7(16) . . ? C214 C209 C205 120.9(16) . . ? C209 C210 C211 122.2(19) . . ? C210 C211 C212 117.6(21) . . ? C213 C212 C211 122.1(25) . . ? C212 C213 C214 121.0(25) . . ? C213 C214 C209 118.5(20) . . ? N20 C218 C219 107.2(22) . . ? C220 C219 C224 120.9(15) . . ? C220 C219 C218 115.6(32) . . ? C224 C219 C218 123.4(32) . . ? C219 C220 C221 119.1(15) . . ? C222 C221 C220 119.8(15) . . ? C221 C222 C223 121.3(15) . . ? C224 C223 C222 119.3(15) . . ? C223 C224 C219 119.1(15) . . ? C230 C226 N21 116.7(13) . . ? C233 C229 C232 109.8(33) . . ? C232 C230 C231 124.7(20) . . ? C232 C230 C226 119.3(18) . . ? C231 C230 C226 115.9(18) . . ? C230 C231 C234 111.0(22) . . ? C230 C232 C229 124.1(26) . . ? C229 C233 C234 138.3(36) . . ? C233 C234 C231 111.8(29) . . ? C239 C237 N22 114.4(13) . . ? C240 C239 C244 117.3(17) . . ? C240 C239 C237 120.0(15) . . ? C244 C239 C237 122.7(16) . . ? C239 C240 C241 120.4(18) . . ? C242 C241 C240 120.7(21) . . ? C241 C242 C243 121.3(24) . . ? C244 C243 C242 119.8(22) . . ? C243 C244 C239 120.5(20) . . ? C249 C248 N23 117.4(12) . . ? C254 C249 C250 116.4(15) . . ? C254 C249 C248 123.2(14) . . ? C250 C249 C248 120.4(13) . . ? C251 C250 C249 120.9(15) . . ? C252 C251 C250 120.4(17) . . ? C251 C252 C253 119.8(18) . . ? C254 C253 C252 120.8(18) . . ? C253 C254 C249 121.7(17) . . ? C425 C255 N24 64.1(28) . . ? C418 C257 N24 119.7(50) . . ? C260 C259 C262 77.9(46) . . ? C261 C260 C259 99.1(54) . . ? C260 C261 C262 93.7(59) . . ? C261 C262 C259 88.7(54) . . ? O100 C302 N100 124.5(27) . . ? O101 C305 N101 124.9(20) . . ? O102 C308 N102 122.8(29) . . ? O106 C309 C420 131.9(100) . . ? O106 C309 C310 134.6(91) . . ? C420 C309 C310 18.7(60) . . ? C420 C310 O103 79.7(70) . . ? C420 C310 C421 121.1(82) . . ? O103 C310 C421 43.0(29) . . ? C420 C310 N103 141.8(83) . . ? O103 C310 N103 137.7(57) . . ? C421 C310 N103 94.9(55) . . ? C420 C310 C311 112.4(73) . . ? O103 C310 C311 167.0(57) . . ? C421 C310 C311 124.1(58) . . ? N103 C310 C311 29.6(32) . . ? C420 C310 C309 19.6(61) . . ? O103 C310 C309 98.6(48) . . ? C421 C310 C309 140.7(56) . . ? N103 C310 C309 123.5(47) . . ? C311 C310 C309 93.9(37) . . ? N103 C311 C310 61.4(70) . . ? N103 C311 C420 83.3(77) . . ? C310 C311 C420 22.1(27) . . ? C438 C312 C313 17.0(49) . . ? C438 C313 C314 105.7(100) . . ? C438 C313 C312 34.4(96) . . ? C314 C313 C312 89.9(51) . . ? C313 C314 C438 25.3(46) . . ? C401 C315 C404 119.9(70) . . ? C401 C315 C316 89.4(52) . . ? C404 C315 C316 118.4(63) . . ? C401 C315 C317 48.4(40) . . ? C404 C315 C317 115.1(60) . . ? C316 C315 C317 123.8(44) . . ? C315 C316 C401 43.0(31) . . ? C401 C317 C315 54.4(44) . . ? C408 C318 C320 32.5(36) . . ? C408 C318 C435 55.3(42) . . ? C320 C318 C435 86.9(52) . . ? C320 C319 C408 9.4(51) . . ? C408 C320 C319 157.3(100) . . ? C408 C320 C318 66.2(84) . . ? C319 C320 C318 134.8(82) . . ? C408 C320 C407 30.6(64) . . ? C319 C320 C407 127.6(72) . . ? C318 C320 C407 90.2(61) . . ? C429 C321 C322 39.2(52) . . ? C429 C321 C431 46.8(53) . . ? C322 C321 C431 54.5(39) . . ? C429 C322 C323 144.9(100) . . ? C429 C322 C431 55.9(74) . . ? C323 C322 C431 117.4(76) . . ? C429 C322 C321 55.9(74) . . ? C323 C322 C321 158.9(65) . . ? C431 C322 C321 67.9(56) . . ? C324 C326 C328 119.1(70) . . ? C324 C326 C327 147.9(76) . . ? C328 C326 C327 92.3(66) . . ? C329 C328 C326 112.7(67) . . ? C317 C401 C315 77.2(60) . . ? C317 C401 C316 113.2(65) . . ? C315 C401 C316 47.6(38) . . ? C400 C402 C403 125.5(83) . . ? C402 C403 C416 114.0(67) . . ? C402 C403 C437 105.7(71) . . ? C416 C403 C437 65.4(60) . . ? C439 C405 C413 112.7(79) . . ? C439 C405 C434 118.2(77) . . ? C413 C405 C434 85.3(48) . . ? C409 C407 C408 154.4(83) . . ? C409 C407 C435 127.0(80) . . ? C408 C407 C435 76.3(62) . . ? C409 C407 C320 132.8(69) . . ? C408 C407 C320 21.6(43) . . ? C435 C407 C320 95.4(67) . . ? C320 C408 C407 127.8(100) . . ? C320 C408 C318 81.3(89) . . ? C407 C408 C318 133.0(67) . . ? C320 C408 C435 155.3(99) . . ? C407 C408 C435 60.5(51) . . ? C318 C408 C435 79.1(49) . . ? C320 C408 C319 13.3(74) . . ? C407 C408 C319 115.3(51) . . ? C318 C408 C319 93.9(50) . . ? C435 C408 C319 159.4(48) . . ? C320 C408 C409 115.9(87) . . ? C407 C408 C409 12.0(39) . . ? C318 C408 C409 138.5(48) . . ? C435 C408 C409 71.7(47) . . ? C319 C408 C409 103.3(31) . . ? C407 C409 C408 13.6(45) . . ? C403 C416 C437 64.2(62) . . ? C257 C418 O107 141.5(62) . . ? C310 C420 C309 141.7(100) . . ? C310 C420 O103 63.6(69) . . ? C309 C420 O103 152.2(98) . . ? C310 C420 O106 142.4(77) . . ? C309 C420 O106 23.2(62) . . ? O103 C420 O106 132.8(54) . . ? C310 C420 C421 36.9(57) . . ? C309 C420 C421 177.6(94) . . ? O103 C420 C421 28.2(28) . . ? O106 C420 C421 155.3(54) . . ? C310 C420 C311 45.5(55) . . ? C309 C420 C311 97.8(77) . . ? O103 C420 C311 109.0(57) . . ? O106 C420 C311 109.0(47) . . ? C421 C420 C311 81.3(42) . . ? O103 C421 C310 63.9(46) . . ? O103 C421 C420 43.2(37) . . ? C310 C421 C420 22.0(31) . . ? O103 C421 N103 107.5(54) . . ? C310 C421 N103 43.6(33) . . ? C420 C421 N103 65.2(34) . . ? C422 C423 C434 71.8(48) . . ? N24 C424 C425 71.8(34) . . ? C424 C425 C255 100.3(46) . . ? C424 C425 N24 50.7(28) . . ? C255 C425 N24 59.4(28) . . ? C428 C427 C426 147.4(100) . . ? C322 C429 C321 85.0(97) . . ? C322 C429 C431 83.3(89) . . ? C321 C429 C431 84.3(81) . . ? C429 C431 C322 40.8(56) . . ? C429 C431 C321 48.9(55) . . ? C322 C431 C321 57.6(53) . . ? C405 C434 C423 148.5(59) . . ? C407 C435 C408 43.2(38) . . ? C407 C435 C318 86.2(57) . . ? C408 C435 C318 45.6(36) . . ? O107 C437 C416 91.9(81) . . ? O107 C437 C403 142.1(100) . . ? C416 C437 C403 50.4(54) . . ? C313 C438 C312 128.6(100) . . ? C313 C438 C314 49.0(84) . . ? C312 C438 C314 99.5(67) . . ? C405 C439 C406 122.5(99) . . ? #===END data_Structure5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Ti4L6 cluster' _chemical_melting_point 'not measured' _chemical_formula_moiety ; 'C179.75 H96 Co2.50 N16 O56.50 Ti4' ; _chemical_formula_sum 'C179.75 H96 Co2.50 N16 O56.50 Ti4' _chemical_formula_weight 3722.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2780 0.4460 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3490 0.9720 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 20.5378(7) _cell_length_b 20.5378(7) _cell_length_c 169.966(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 62087(5) _cell_formula_units_Z 12 _cell_measurement_temperature 178(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 22724 _exptl_absorpt_coefficient_mu 0.420 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8738 _exptl_absorpt_correction_T_max 0.9513 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 178(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 42016 _diffrn_reflns_av_R_equivalents 0.0933 _diffrn_reflns_av_sigmaI/netI 0.0487 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -141 _diffrn_reflns_limit_l_max 141 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 17.25 _reflns_number_total 4201 _reflns_number_gt 2811 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v.5.054d' _computing_cell_refinement 'SAINT v.7.07' _computing_data_reduction 'SAINT v.7.07' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 v.1.08, POV-Ray v3.6.1c.icl8.win32' _computing_publication_material 'ORTEP-3 v.1.08, POV-Ray v3.6.1c.icl8.win32' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Ti and Co atoms as well as the N and O atoms in the assembly were refined anisotropically. Hydrogen atoms were included on the ligand and the ordered Cp2Co+ on the exterior of the assembly in calculated positions and their positions were refined using the riding model. Hydrogen atoms were not included on any of the solvent or ammonium cations in the asymmetric unit. The bond distances of the catechol and naphthalene rings were modeled separately as standard aromatic rings using typical bond length restraints. Similarly, the bond distances for the methanol and NEt4+ cations were modeled using standard C-C and C-N bond length restraints. The Cp2Co+ molecule on the interior of the assembly was modeled as a rigid body using a known structure of Cp2Co+ (CSD-182/808) at 1/3 occupancy due to the fact that the Co sits on a 3-fold rotation axis. The Cp2Co+ molecule on the exterior of the assembly was found to be ordered and exhibited D5d symmetry as a consequence of its position on a 2-fold axis, but was modeled using the known structure of Cp2Co+ due to elongated thermal ellipsoids on the cyclopentadienyl rings and atom position instability. A small pocket of disordered solvent was located in the asymmetric (O1s to O11s) unit and modeled as water by keeping the thermal parameters of the oxygen atoms constant while refining the occupancy. The total occupancy of the oxygen atoms in the disordered area equated to 4.6 water molecules corresponding to 13.8 waters per assembly in the lattice. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4201 _refine_ls_number_parameters 440 _refine_ls_number_restraints 275 _refine_ls_R_factor_all 0.1923 _refine_ls_R_factor_gt 0.1569 _refine_ls_wR_factor_ref 0.4484 _refine_ls_wR_factor_gt 0.4246 _refine_ls_goodness_of_fit_ref 1.836 _refine_ls_restrained_S_all 2.009 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C01 C 0.8664(12) -0.1350(13) 0.41854(13) 0.088(6) Uiso 1 1 d DU . . C02 C 0.8977(14) -0.1439(14) 0.42552(13) 0.090(7) Uiso 1 1 d DU . . C03 C 0.8617(13) -0.2036(13) 0.43067(14) 0.111(8) Uiso 1 1 d DU . . H03A H 0.8859 -0.2090 0.4352 0.133 Uiso 1 1 calc R . . C04 C 0.7879(13) -0.2549(15) 0.42876(14) 0.125(8) Uiso 1 1 d DU . . H04A H 0.7598 -0.2957 0.4322 0.149 Uiso 1 1 calc R . . C05 C 0.7535(15) -0.2494(14) 0.42202(13) 0.117(8) Uiso 1 1 d DU . . H05A H 0.7028 -0.2865 0.4209 0.140 Uiso 1 1 calc R . . C06 C 0.7924(13) -0.1898(12) 0.41679(14) 0.106(7) Uiso 1 1 d DU . . C08 C 0.7663(12) -0.1071(12) 0.39812(15) 0.101(7) Uiso 1 1 d DU . . C09 C 0.6985(13) -0.1571(14) 0.39450(13) 0.109(8) Uiso 1 1 d DU . . H09A H 0.6691 -0.2072 0.3964 0.131 Uiso 1 1 calc R . . C10 C 0.6746(14) -0.1323(12) 0.38807(13) 0.111(8) Uiso 1 1 d DU . . H10A H 0.6291 -0.1672 0.3855 0.133 Uiso 1 1 calc R . . C11 C 0.7136(11) -0.0597(11) 0.38520(13) 0.093(7) Uiso 1 1 d DU . . H11A H 0.6947 -0.0440 0.3810 0.111 Uiso 1 1 calc R . . C12 C 0.7824(12) -0.0101(12) 0.38882(12) 0.095(7) Uiso 1 1 d DU . . C13 C 0.8095(12) -0.0371(13) 0.39488(13) 0.098(7) Uiso 1 1 d DU . . C14 C 0.8821(13) 0.0099(14) 0.39794(15) 0.122(8) Uiso 1 1 d DU . . H14A H 0.9021 -0.0088 0.4018 0.147 Uiso 1 1 calc R . . C15 C 0.9248(17) 0.0842(15) 0.39529(16) 0.127(13) Uiso 0.90(6) 1 d PDU . . H15A H 0.9731 0.1172 0.3974 0.152 Uiso 1 1 calc R . . C16 C 0.8943(13) 0.1084(15) 0.38941(14) 0.117(8) Uiso 1 1 d DU . . H16A H 0.9239 0.1581 0.3874 0.140 Uiso 1 1 calc R . . C17 C 0.8229(12) 0.0635(12) 0.38631(14) 0.090(6) Uiso 1 1 d DU . . C19 C 0.7560(12) 0.1762(13) 0.37529(14) 0.083(6) Uiso 1 1 d U . . C20 C 0.7617(14) 0.2478(15) 0.37607(15) 0.116(8) Uiso 1 1 d U . . H20A H 0.7884 0.2821 0.3802 0.139 Uiso 1 1 calc R . . C21 C 0.7252(13) 0.2618(14) 0.37029(15) 0.106(8) Uiso 1 1 d U . . H21A H 0.7269 0.3087 0.3708 0.127 Uiso 1 1 calc R . . C22 C 0.6874(14) 0.2215(14) 0.36409(15) 0.108(8) Uiso 1 1 d U . . H22A H 0.6661 0.2390 0.3603 0.130 Uiso 1 1 calc R . . C23 C 0.6816(14) 0.1490(14) 0.36370(15) 0.087(7) Uiso 1 1 d U . . C24 C 0.7170(12) 0.1328(13) 0.36914(13) 0.081(6) Uiso 1 1 d U . . C34 C 0.5793(12) -0.1329(12) 0.36731(11) 0.058(5) Uiso 1 1 d U . . C35 C 0.5294(13) -0.1076(14) 0.36798(13) 0.084(6) Uiso 1 1 d U . . C36 C 0.4584(14) -0.1514(14) 0.37226(14) 0.107(8) Uiso 1 1 d U . . H36A H 0.4230 -0.1347 0.3726 0.128 Uiso 1 1 calc R . . C37 C 0.4448(14) -0.2168(14) 0.37573(14) 0.105(8) Uiso 1 1 d U . . H37A H 0.4017 -0.2441 0.3790 0.126 Uiso 1 1 calc R . . C38 C 0.4937(13) -0.2430(13) 0.37454(12) 0.089(7) Uiso 1 1 d U . . H38A H 0.4823 -0.2903 0.3767 0.106 Uiso 1 1 calc R . . C39 C 0.5587(12) -0.2025(12) 0.37031(12) 0.071(6) Uiso 1 1 d U . . C25 C 0.7102(12) 0.0081(11) 0.34443(14) 0.070(6) Uiso 1 1 d U . . C26 C 0.6295(14) -0.0295(13) 0.34310(16) 0.088(6) Uiso 1 1 d U . . C27 C 0.6033(15) -0.0513(14) 0.33548(15) 0.112(8) Uiso 1 1 d U . . H27A H 0.5512 -0.0727 0.3343 0.134 Uiso 1 1 calc R . . C28 C 0.6535(16) -0.0417(15) 0.32956(18) 0.133(9) Uiso 1 1 d U . . H28A H 0.6340 -0.0628 0.3245 0.159 Uiso 1 1 calc R . . C29 C 0.7317(15) -0.0024(14) 0.33057(15) 0.113(8) Uiso 1 1 d U . . H29A H 0.7647 0.0084 0.3262 0.136 Uiso 1 1 calc R . . C30 C 0.7595(12) 0.0205(11) 0.33823(12) 0.072(6) Uiso 1 1 d U . . C41 C 0.7244(11) -0.2225(11) 0.36396(12) 0.067(5) Uiso 1 1 d U . . C42 C 0.7302(12) -0.2721(12) 0.36872(13) 0.089(7) Uiso 1 1 d U . . H42A H 0.7019 -0.2895 0.3735 0.107 Uiso 1 1 calc R . . C43 C 0.7804(13) -0.2972(12) 0.36634(13) 0.092(7) Uiso 1 1 d U . . H43A H 0.7847 -0.3327 0.3696 0.110 Uiso 1 1 calc R . . C44 C 0.8223(12) -0.2730(11) 0.35974(12) 0.080(6) Uiso 1 1 d U . . H44A H 0.8517 -0.2948 0.3582 0.095 Uiso 1 1 calc R . . C45 C 0.8231(10) -0.2154(10) 0.35502(11) 0.060(6) Uiso 1 1 d U . . C46 C 0.7724(11) -0.1895(11) 0.35729(11) 0.065(6) Uiso 1 1 d U . . Ti2 Ti 1.0000 0.0000 0.42055(4) 0.092(3) Uani 1 3 d S . . C32 C 0.9466(12) 0.1347(12) 0.34842(12) 0.068(6) Uiso 1 1 d U . . C47 C 0.7690(12) -0.1344(11) 0.35227(12) 0.078(6) Uiso 1 1 d U . . H47A H 0.7345 -0.1178 0.3535 0.094 Uiso 1 1 calc R . . O12 O 0.5847(8) -0.3028(9) 0.37194(9) 0.100(5) Uani 1 1 d U . . C33 C 1.0057(14) 0.1362(13) 0.34376(14) 0.101(8) Uiso 1 1 d U . . Co2 Co 0.7228(3) 0.0561(3) 0.4167 0.131(2) Uani 1 2 d SG . . C205 C 0.7174(12) -0.0375(6) 0.41277(8) 0.158(10) Uiso 1 1 d GU . . H205 H 0.6873 -0.0867 0.4148 0.189 Uiso 1 1 calc R . . C201 C 0.7920(10) 0.0151(12) 0.41511(10) 0.151(10) Uiso 1 1 d GU . . H201 H 0.8205 0.0072 0.4190 0.182 Uiso 1 1 calc R . . C202 C 0.8164(6) 0.0816(10) 0.41062(11) 0.161(10) Uiso 1 1 d GU . . H202 H 0.8641 0.1260 0.4110 0.193 Uiso 1 1 calc R . . C203 C 0.7569(12) 0.0700(12) 0.40548(4) 0.147(10) Uiso 1 1 d GU . . H203 H 0.7580 0.1053 0.4018 0.176 Uiso 1 1 calc R . . C204 C 0.6958(10) -0.0036(12) 0.40681(5) 0.157(10) Uiso 1 1 d GU . . H204 H 0.6487 -0.0262 0.4042 0.189 Uiso 1 1 calc R . . C48 C 0.8132(13) -0.1067(13) 0.34599(14) 0.096(7) Uiso 1 1 d U . . H48A H 0.8105 -0.0696 0.3429 0.144 Uiso 1 1 calc R . . Ti1 Ti 0.6430(2) 0.0028(2) 0.35899(2) 0.0727(17) Uani 1 1 d . . . O06 O 0.7107(7) 0.0620(7) 0.36762(7) 0.072(4) Uani 1 1 d U . . O07 O 0.7278(6) 0.0245(7) 0.35205(7) 0.062(4) Uani 1 1 d U . . O10 O 0.6390(6) -0.0885(7) 0.36332(7) 0.060(4) Uani 1 1 d U . . O05 O 0.6433(7) 0.0990(8) 0.35779(9) 0.088(5) Uani 1 1 d U . . O08 O 0.5896(8) -0.0372(9) 0.34940(9) 0.097(5) Uani 1 1 d U . . O09 O 0.8814(8) 0.0668(8) 0.33318(8) 0.089(5) Uani 1 1 d U . . O02 O 0.9637(9) -0.0886(9) 0.42719(7) 0.094(5) Uani 1 1 d U . . O11 O 0.5488(7) -0.0397(8) 0.36477(8) 0.084(4) Uani 1 1 d U . . O01 O 0.9107(8) -0.0740(8) 0.41423(7) 0.090(5) Uani 1 1 d U . . N04 N 0.6725(9) -0.1974(9) 0.36595(8) 0.064(4) Uani 1 1 d U . . H04B H 0.6853 -0.1510 0.3647 0.077 Uiso 1 1 calc R . . N03 N 0.8700(9) 0.0858(8) 0.34591(9) 0.064(4) Uani 1 1 d U . . H40B H 0.8364 0.0710 0.3497 0.077 Uiso 1 1 calc R . . N02 N 0.7932(10) 0.0962(12) 0.38134(12) 0.108(6) Uani 1 1 d U . . H02B H 0.7713 0.0674 0.3772 0.129 Uiso 1 1 calc R . . O03 O 0.6850(12) -0.2380(11) 0.40817(11) 0.157(8) Uani 1 1 d U . . O04 O 0.8286(11) 0.2026(12) 0.38730(10) 0.142(7) Uani 1 1 d U . . C31 C 0.8416(13) 0.0594(11) 0.33881(15) 0.066(6) Uiso 1 1 d U . . C18 C 0.7885(16) 0.1593(17) 0.38105(19) 0.112(7) Uiso 1 1 d U . . N01 N 0.7895(11) -0.1285(11) 0.40473(10) 0.102(6) Uani 1 1 d U . . H01B H 0.8364 -0.0982 0.4061 0.123 Uiso 1 1 calc R . . C07 C 0.7485(17) -0.1924(17) 0.40959(16) 0.106(7) Uiso 1 1 d U . . C40 C 0.6085(13) -0.2375(14) 0.36945(12) 0.067(6) Uiso 1 1 d U . . Co1 Co 1.0000 0.0000 0.37136(3) 0.095(2) Uani 1 3 d SGD . . C101 C 0.9044(9) -0.0517(17) 0.37648(18) 0.117(10) Uiso 0.33 1 d PGDU . . C102 C 0.9077(11) 0.000(2) 0.37070(16) 0.117(10) Uiso 0.33 1 d PGDU . . C103 C 0.966(2) 0.0726(16) 0.3728(2) 0.117(10) Uiso 0.33 1 d PGDU . . C104 C 0.9991(18) 0.0662(18) 0.37993(17) 0.117(10) Uiso 0.33 1 d PGDU . . C105 C 0.9609(17) -0.011(2) 0.38218(7) 0.117(10) Uiso 0.33 1 d PGDU . . C106 C 1.023(2) -0.0828(15) 0.3666(2) 0.117(10) Uiso 0.33 1 d PGDU . . C107 C 1.0220(18) -0.035(2) 0.36054(11) 0.117(10) Uiso 0.33 1 d PGDU . . C108 C 1.0783(15) 0.040(2) 0.36227(14) 0.117(10) Uiso 0.33 1 d PGDU . . C109 C 1.1142(5) 0.039(2) 0.36939(19) 0.117(10) Uiso 0.33 1 d PGDU . . C110 C 1.0801(18) -0.037(2) 0.37206(19) 0.117(10) Uiso 0.33 1 d PGDU . . C10S C 1.0000 0.0000 0.3240(3) 0.131(16) Uiso 1 3 d SDU . . C12S C 0.865(6) -0.084(6) 0.3150(6) 0.49(4) Uiso 1 1 d U . . O12S O 0.795(4) -0.090(3) 0.3186(4) 0.46(3) Uiso 1 1 d U . . C7S C 0.769(5) 0.156(4) 0.3137(4) 0.40(3) Uiso 1 1 d DU . . C11S C 1.0000 0.0000 0.3080(3) 0.171(19) Uiso 1 3 d SDU . . C8S C 0.735(3) 0.140(3) 0.3027(3) 0.28(2) Uiso 1 1 d DU . . N2S N 0.769(3) 0.104(3) 0.3075(4) 0.35(2) Uiso 1 1 d DU . . N3S N 0.983(6) -0.036(3) 0.3160(3) 0.154(19) Uiso 0.33 1 d PDU A -1 O1S O 0.5277(16) 0.0419(14) 0.38958(15) 0.173(9) Uiso 0.96(4) 1 d PU . . O2S O 0.548(3) 0.027(2) 0.4015(3) 0.173(9) Uiso 0.50(3) 1 d PU . . O3S O 0.598(4) 0.163(4) 0.3897(4) 0.173(9) Uiso 0.34(3) 1 d P . . O4S O 0.651(4) -0.300(4) 0.4438(4) 0.173(9) Uiso 0.33(3) 1 d PU . . O5S O 0.719(4) -0.253(4) 0.4494(4) 0.173(9) Uiso 0.33(3) 1 d PU . . O6S O 0.3333 -0.3333 0.3921(8) 0.173(9) Uiso 0.28(6) 3 d SP . . O7S O 1.0000 0.0000 0.4441(5) 0.173(9) Uiso 0.45(6) 3 d SP . . O8S O 0.909(2) 0.098(2) 0.3180(2) 0.173(9) Uiso 0.51(4) 1 d P . . O9S O 0.584(3) 0.075(3) 0.3944(3) 0.173(9) Uiso 0.49(4) 1 d PU . . O10S O 0.582(3) 0.019(3) 0.3862(3) 0.173(9) Uiso 0.40(3) 1 d PU . . O11S O 0.778(3) -0.435(3) 0.3426(3) 0.173(9) Uiso 0.43(4) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti2 0.116(4) 0.116(4) 0.043(5) 0.000 0.000 0.058(2) O12 0.079(11) 0.087(12) 0.141(13) 0.029(10) 0.016(9) 0.046(9) Co2 0.129(4) 0.129(4) 0.136(5) -0.0278(19) 0.0278(19) 0.065(4) Ti1 0.057(3) 0.079(3) 0.086(3) 0.014(2) -0.002(2) 0.038(2) O06 0.068(9) 0.073(9) 0.082(9) 0.023(7) 0.022(7) 0.040(7) O07 0.061(8) 0.083(9) 0.049(8) 0.010(7) 0.008(7) 0.041(7) O10 0.051(8) 0.056(8) 0.078(9) 0.027(7) 0.022(7) 0.032(7) O05 0.073(9) 0.106(11) 0.103(11) 0.058(9) 0.029(8) 0.059(9) O08 0.065(9) 0.137(12) 0.084(10) 0.040(9) 0.010(8) 0.046(9) O09 0.068(10) 0.094(11) 0.081(10) 0.003(9) 0.016(9) 0.024(9) O02 0.122(12) 0.120(11) 0.052(8) 0.013(8) 0.024(8) 0.069(10) O11 0.070(9) 0.097(10) 0.104(10) 0.039(8) 0.026(8) 0.055(8) O01 0.098(10) 0.115(11) 0.055(8) 0.019(8) 0.018(8) 0.052(9) N04 0.066(9) 0.068(9) 0.066(9) 0.020(8) 0.021(8) 0.040(8) N03 0.064(10) 0.061(9) 0.067(10) 0.021(8) 0.014(8) 0.031(8) N02 0.088(11) 0.113(12) 0.108(11) 0.022(10) 0.039(10) 0.040(10) O03 0.129(16) 0.137(16) 0.135(15) 0.021(12) -0.030(13) 0.014(14) O04 0.146(15) 0.186(17) 0.111(13) -0.046(13) -0.001(12) 0.095(14) N01 0.115(11) 0.115(12) 0.082(11) 0.012(10) 0.011(10) 0.061(10) Co1 0.106(3) 0.106(3) 0.074(4) 0.000 0.000 0.0530(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C01 O01 1.34(2) . ? C01 C06 1.398(13) . ? C01 C02 1.403(13) . ? C02 O02 1.29(2) . ? C02 C03 1.382(13) . ? C03 C04 1.384(13) . ? C03 H03A 0.9500 . ? C04 C05 1.381(13) . ? C04 H04A 0.9500 . ? C05 C06 1.396(13) . ? C05 H05A 0.9500 . ? C06 C07 1.50(3) . ? C08 C13 1.373(14) . ? C08 N01 1.37(3) . ? C08 C09 1.394(13) . ? C09 C10 1.396(13) . ? C09 H09A 0.9500 . ? C10 C11 1.381(13) . ? C10 H10A 0.9500 . ? C11 C12 1.405(13) . ? C11 H11A 0.9500 . ? C12 C17 1.380(14) . ? C12 C13 1.409(13) . ? C13 C14 1.409(13) . ? C14 C15 1.402(13) . ? C14 H14A 0.9500 . ? C15 C16 1.397(13) . ? C15 H15A 0.9500 . ? C16 C17 1.388(14) . ? C16 H16A 0.9500 . ? C17 N02 1.40(3) . ? C19 C18 1.32(3) . ? C19 C24 1.35(3) . ? C19 C20 1.42(3) . ? C20 C21 1.35(3) . ? C20 H20A 0.9500 . ? C21 C22 1.33(3) . ? C21 H21A 0.9500 . ? C22 C23 1.43(3) . ? C22 H22A 0.9500 . ? C23 O05 1.37(2) . ? C23 C24 1.32(3) . ? C24 O06 1.42(2) . ? C34 O10 1.29(2) . ? C34 C39 1.37(2) . ? C34 C35 1.37(2) . ? C35 O11 1.36(2) . ? C35 C36 1.47(3) . ? C36 C37 1.36(3) . ? C36 H36A 0.9500 . ? C37 C38 1.37(3) . ? C37 H37A 0.9500 . ? C38 C39 1.37(3) . ? C38 H38A 0.9500 . ? C39 C40 1.52(3) . ? C25 O07 1.34(2) . ? C25 C30 1.39(3) . ? C25 C26 1.45(3) . ? C26 O08 1.31(2) . ? C26 C27 1.39(3) . ? C27 C28 1.38(3) . ? C27 H27A 0.9500 . ? C28 C29 1.40(3) . ? C28 H28A 0.9500 . ? C29 C30 1.41(3) . ? C29 H29A 0.9500 . ? C30 C31 1.47(3) . ? C41 C42 1.35(2) . ? C41 C46 1.43(2) . ? C41 N04 1.44(2) . ? C42 C43 1.42(3) . ? C42 H42A 0.9500 . ? C43 C44 1.35(3) . ? C43 H43A 0.9500 . ? C44 C45 1.42(2) . ? C44 H44A 0.9500 . ? C45 C32 1.36(2) 2_645 ? C45 C46 1.44(2) . ? C46 C47 1.45(2) . ? Ti2 O02 1.945(15) . ? Ti2 O02 1.945(15) 2_645 ? Ti2 O02 1.945(15) 3_765 ? Ti2 O01 2.010(15) 3_765 ? Ti2 O01 2.010(15) 2_645 ? Ti2 O01 2.010(15) . ? C32 C45 1.36(2) 3_765 ? C32 C33 1.44(3) . ? C32 N03 1.44(2) . ? C47 C48 1.33(3) . ? C47 H47A 0.9500 . ? O12 C40 1.25(2) . ? C33 C48 1.40(3) 3_765 ? Co2 C205 1.984(19) 10_545 ? Co2 C205 1.984(6) . ? Co2 C204 1.986(11) 10_545 ? Co2 C204 1.985(5) . ? Co2 C203 1.997(9) 10_545 ? Co2 C203 1.9967 . ? Co2 C201 1.998(4) . ? Co2 C201 1.998(8) 10_545 ? Co2 C202 2.005(17) 10_545 ? Co2 C202 2.0044(17) . ? C205 C201 1.4193(11) . ? C205 C204 1.420(3) . ? C205 H205 0.9500 . ? C201 C202 1.418(3) . ? C201 H201 0.9500 . ? C202 C203 1.4213(13) . ? C202 H202 0.9500 . ? C203 C204 1.4196 . ? C203 H203 0.9500 . ? C204 H204 0.9500 . ? C48 C33 1.40(3) 2_645 ? C48 H48A 0.9500 . ? Ti1 O08 1.908(15) . ? Ti1 O11 1.944(13) . ? Ti1 O06 1.968(14) . ? Ti1 O07 1.962(12) . ? Ti1 O10 1.976(12) . ? Ti1 O05 1.984(14) . ? O09 C31 1.22(2) . ? N04 C40 1.30(2) . ? N04 H04B 0.8800 . ? N03 C31 1.33(2) . ? N03 H40B 0.8800 . ? N02 C18 1.35(3) . ? N02 H02B 0.8800 . ? O03 C07 1.19(3) . ? O04 C18 1.37(3) . ? N01 C07 1.42(3) . ? N01 H01B 0.8800 . ? Co1 C102 1.90(4) 3_765 ? Co1 C102 1.90(3) 2_645 ? Co1 C102 1.8978 . ? Co1 C101 1.9126 . ? Co1 C101 1.91(3) 3_765 ? Co1 C101 1.91(3) 2_645 ? Co1 C103 1.95(3) 3_765 ? Co1 C103 1.9512 . ? Co1 C103 1.95(3) 2_645 ? Co1 C105 1.9745 . ? Co1 C105 1.97(2) 3_765 ? Co1 C105 1.975(17) 2_645 ? C101 C110 0.918(2) 3_765 ? C101 C104 1.00(5) 2_645 ? C101 C105 1.4198 . ? C101 C102 1.4202 . ? C101 C103 1.55(6) 2_645 ? C102 C106 0.81(3) 3_765 ? C102 C109 1.40(4) 2_645 ? C102 C103 1.4184(16) . ? C102 C110 1.47(4) 3_765 ? C103 C109 0.598(13) 2_645 ? C103 C110 1.28(4) 2_645 ? C103 C104 1.4235 . ? C103 C101 1.55(6) 3_765 ? C104 C101 1.00(5) 3_765 ? C104 C105 1.07(7) 3_765 ? C104 C105 1.4198 . ? C104 C110 1.635(4) 2_645 ? C105 C104 1.07(5) 2_645 ? C106 C102 0.81(3) 2_645 ? C106 C110 1.4211(13) . ? C106 C107 1.4218 . ? C106 C108 1.51(6) 3_765 ? C107 C108 1.15(5) 3_765 ? C107 C108 1.4192(17) . ? C108 C107 1.15(6) 2_645 ? C108 C109 1.4228 . ? C108 C106 1.51(6) 2_645 ? C109 C103 0.598(3) 3_765 ? C109 C102 1.40(5) 3_765 ? C109 C110 1.4205 . ? C110 C101 0.92(4) 2_645 ? C110 C103 1.28(6) 3_765 ? C110 C102 1.47(5) 2_645 ? C110 C104 1.63(5) 3_765 ? C10S N3S 1.50(2) 2_645 ? C10S N3S 1.50(2) 3_765 ? C10S N3S 1.50(2) . ? C12S O12S 1.52(10) . ? C7S N2S 1.50(2) . ? C11S N3S 1.50(2) . ? C11S N3S 1.50(2) 2_645 ? C11S N3S 1.50(2) 3_765 ? C8S N2S 1.50(2) . ? O1S O9S 1.30(5) . ? O1S O10S 1.53(6) . ? O2S O9S 1.51(5) . ? O4S O5S 1.57(8) . ? O9S O10S 1.79(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O01 C01 C06 126(2) . . ? O01 C01 C02 116(2) . . ? C06 C01 C02 117(2) . . ? O02 C02 C03 120(2) . . ? O02 C02 C01 115(2) . . ? C03 C02 C01 125(3) . . ? C02 C03 C04 115(2) . . ? C02 C03 H03A 122.5 . . ? C04 C03 H03A 122.5 . . ? C05 C04 C03 123(3) . . ? C05 C04 H04A 118.6 . . ? C03 C04 H04A 118.6 . . ? C04 C05 C06 120(3) . . ? C04 C05 H05A 119.8 . . ? C06 C05 H05A 119.8 . . ? C01 C06 C05 119(2) . . ? C01 C06 C07 126(2) . . ? C05 C06 C07 115(2) . . ? C13 C08 N01 121(2) . . ? C13 C08 C09 119(2) . . ? N01 C08 C09 120(2) . . ? C08 C09 C10 119(2) . . ? C08 C09 H09A 120.6 . . ? C10 C09 H09A 120.6 . . ? C11 C10 C09 123(2) . . ? C11 C10 H10A 118.3 . . ? C09 C10 H10A 118.3 . . ? C10 C11 C12 117(2) . . ? C10 C11 H11A 121.3 . . ? C12 C11 H11A 121.3 . . ? C17 C12 C13 121(2) . . ? C17 C12 C11 119.7(19) . . ? C13 C12 C11 119(2) . . ? C08 C13 C12 122(2) . . ? C08 C13 C14 118(2) . . ? C12 C13 C14 119(2) . . ? C15 C14 C13 120(3) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C16 C15 C14 118(3) . . ? C16 C15 H15A 121.0 . . ? C14 C15 H15A 121.0 . . ? C15 C16 C17 123(3) . . ? C15 C16 H16A 118.4 . . ? C17 C16 H16A 118.4 . . ? C12 C17 C16 118(2) . . ? C12 C17 N02 123(2) . . ? C16 C17 N02 119(2) . . ? C18 C19 C24 128(3) . . ? C18 C19 C20 114(3) . . ? C24 C19 C20 118(2) . . ? C21 C20 C19 113(3) . . ? C21 C20 H20A 123.7 . . ? C19 C20 H20A 123.7 . . ? C20 C21 C22 131(3) . . ? C20 C21 H21A 114.3 . . ? C22 C21 H21A 114.3 . . ? C21 C22 C23 114(3) . . ? C21 C22 H22A 123.1 . . ? C23 C22 H22A 123.1 . . ? O05 C23 C24 121(2) . . ? O05 C23 C22 122(2) . . ? C24 C23 C22 117(3) . . ? C23 C24 O06 111(2) . . ? C23 C24 C19 127(3) . . ? O06 C24 C19 123(2) . . ? O10 C34 C39 128.2(19) . . ? O10 C34 C35 114(2) . . ? C39 C34 C35 118(2) . . ? O11 C35 C34 118(2) . . ? O11 C35 C36 121(2) . . ? C34 C35 C36 121(2) . . ? C37 C36 C35 118(2) . . ? C37 C36 H36A 121.0 . . ? C35 C36 H36A 121.0 . . ? C38 C37 C36 120(3) . . ? C38 C37 H37A 120.2 . . ? C36 C37 H37A 120.2 . . ? C37 C38 C39 121(2) . . ? C37 C38 H38A 119.3 . . ? C39 C38 H38A 119.3 . . ? C34 C39 C38 122(2) . . ? C34 C39 C40 122(2) . . ? C38 C39 C40 116(2) . . ? O07 C25 C30 127.1(19) . . ? O07 C25 C26 112.1(19) . . ? C30 C25 C26 121(2) . . ? O08 C26 C27 127(2) . . ? O08 C26 C25 115(2) . . ? C27 C26 C25 118(2) . . ? C28 C27 C26 119(3) . . ? C28 C27 H27A 120.3 . . ? C26 C27 H27A 120.3 . . ? C27 C28 C29 124(3) . . ? C27 C28 H28A 118.2 . . ? C29 C28 H28A 118.2 . . ? C28 C29 C30 118(3) . . ? C28 C29 H29A 121.2 . . ? C30 C29 H29A 121.2 . . ? C25 C30 C29 120(2) . . ? C25 C30 C31 126(2) . . ? C29 C30 C31 114(2) . . ? C42 C41 C46 122(2) . . ? C42 C41 N04 119.3(19) . . ? C46 C41 N04 118.3(18) . . ? C41 C42 C43 117(2) . . ? C41 C42 H42A 121.5 . . ? C43 C42 H42A 121.5 . . ? C44 C43 C42 123(2) . . ? C44 C43 H43A 118.4 . . ? C42 C43 H43A 118.4 . . ? C43 C44 C45 121(2) . . ? C43 C44 H44A 119.5 . . ? C45 C44 H44A 119.5 . . ? C32 C45 C44 123(2) 2_645 . ? C32 C45 C46 120.0(19) 2_645 . ? C44 C45 C46 116.5(18) . . ? C41 C46 C45 119.4(18) . . ? C41 C46 C47 123.1(19) . . ? C45 C46 C47 117.3(18) . . ? O02 Ti2 O02 89.7(6) . 2_645 ? O02 Ti2 O02 89.7(6) . 3_765 ? O02 Ti2 O02 89.7(6) 2_645 3_765 ? O02 Ti2 O01 167.3(6) . 3_765 ? O02 Ti2 O01 97.5(6) 2_645 3_765 ? O02 Ti2 O01 79.9(6) 3_765 3_765 ? O02 Ti2 O01 97.5(6) . 2_645 ? O02 Ti2 O01 79.9(6) 2_645 2_645 ? O02 Ti2 O01 167.3(7) 3_765 2_645 ? O01 Ti2 O01 94.1(5) 3_765 2_645 ? O02 Ti2 O01 79.9(6) . . ? O02 Ti2 O01 167.3(6) 2_645 . ? O02 Ti2 O01 97.5(6) 3_765 . ? O01 Ti2 O01 94.1(5) 3_765 . ? O01 Ti2 O01 94.1(5) 2_645 . ? C45 C32 C33 122(2) 3_765 . ? C45 C32 N03 120.4(19) 3_765 . ? C33 C32 N03 117.9(19) . . ? C48 C47 C46 121(2) . . ? C48 C47 H47A 119.4 . . ? C46 C47 H47A 119.4 . . ? C48 C33 C32 118(2) 3_765 . ? C205 Co2 C205 118.4(3) 10_545 . ? C205 Co2 C204 41.9(2) 10_545 10_545 ? C205 Co2 C204 106.5(8) . 10_545 ? C205 Co2 C204 106.5(8) 10_545 . ? C205 Co2 C204 41.9(2) . . ? C204 Co2 C204 126.7(4) 10_545 . ? C205 Co2 C203 70.5(6) 10_545 10_545 ? C205 Co2 C203 126.0(8) . 10_545 ? C204 Co2 C203 41.8(2) 10_545 10_545 ? C204 Co2 C203 165.3(6) . 10_545 ? C205 Co2 C203 126.0(12) 10_545 . ? C205 Co2 C203 70.5(3) . . ? C204 Co2 C203 165.4(9) 10_545 . ? C204 Co2 C203 41.77(6) . . ? C203 Co2 C203 151.4(4) 10_545 . ? C205 Co2 C201 153.4(9) 10_545 . ? C205 Co2 C201 41.76(11) . . ? C204 Co2 C201 117.7(13) 10_545 . ? C204 Co2 C201 70.5(2) . . ? C203 Co2 C201 105.5(9) 10_545 . ? C203 Co2 C201 70.2(2) . . ? C205 Co2 C201 41.8(6) 10_545 10_545 ? C205 Co2 C201 153.4(4) . 10_545 ? C204 Co2 C201 70.4(9) 10_545 10_545 ? C204 Co2 C201 117.7(8) . 10_545 ? C203 Co2 C201 70.2(3) 10_545 10_545 ? C203 Co2 C201 105.5(9) . 10_545 ? C201 Co2 C201 163.35(19) . 10_545 ? C205 Co2 C202 70.3(4) 10_545 10_545 ? C205 Co2 C202 164.1(10) . 10_545 ? C204 Co2 C202 70.3(7) 10_545 10_545 ? C204 Co2 C202 152.1(11) . 10_545 ? C203 Co2 C202 41.6(7) 10_545 10_545 ? C203 Co2 C202 116.5(9) . 10_545 ? C201 Co2 C202 124.9(8) . 10_545 ? C201 Co2 C202 41.5(7) 10_545 10_545 ? C205 Co2 C202 164.1(11) 10_545 . ? C205 Co2 C202 70.30(18) . . ? C204 Co2 C202 152.1(12) 10_545 . ? C204 Co2 C202 70.35(12) . . ? C203 Co2 C202 116.5(6) 10_545 . ? C203 Co2 C202 41.62(6) . . ? C201 Co2 C202 41.49(13) . . ? C201 Co2 C202 124.9(5) 10_545 . ? C202 Co2 C202 104.9(6) 10_545 . ? C201 C205 C204 108.03(7) . . ? C201 C205 Co2 69.65(6) . . ? C204 C205 Co2 69.08(13) . . ? C201 C205 H205 126.0 . . ? C204 C205 H205 126.0 . . ? Co2 C205 H205 126.8 . . ? C202 C201 C205 108.06(6) . . ? C202 C201 Co2 69.50(11) . . ? C205 C201 Co2 68.59(13) . . ? C202 C201 H201 126.0 . . ? C205 C201 H201 126.0 . . ? Co2 C201 H201 127.5 . . ? C201 C202 C203 107.97(18) . . ? C201 C202 Co2 69.01(16) . . ? C203 C202 Co2 68.9 . . ? C201 C202 H202 126.0 . . ? C203 C202 H202 126.0 . . ? Co2 C202 H202 127.6 . . ? C204 C203 C202 108.01(14) . . ? C204 C203 Co2 68.7(2) . . ? C202 C203 Co2 69.48(7) . . ? C204 C203 H203 126.0 . . ? C202 C203 H203 126.0 . . ? Co2 C203 H203 127.4 . . ? C203 C204 C205 107.92(11) . . ? C203 C204 Co2 69.55(13) . . ? C205 C204 Co2 68.98(15) . . ? C203 C204 H204 126.0 . . ? C205 C204 H204 126.0 . . ? Co2 C204 H204 127.0 . . ? C47 C48 C33 122(2) . 2_645 ? C47 C48 H48A 118.9 . . ? C33 C48 H48A 118.9 2_645 . ? O08 Ti1 O11 90.5(6) . . ? O08 Ti1 O06 168.5(6) . . ? O11 Ti1 O06 97.9(6) . . ? O08 Ti1 O07 80.7(6) . . ? O11 Ti1 O07 167.7(6) . . ? O06 Ti1 O07 92.0(5) . . ? O08 Ti1 O10 99.7(6) . . ? O11 Ti1 O10 80.0(5) . . ? O06 Ti1 O10 89.5(5) . . ? O07 Ti1 O10 93.0(5) . . ? O08 Ti1 O05 93.1(7) . . ? O11 Ti1 O05 90.3(5) . . ? O06 Ti1 O05 79.2(6) . . ? O07 Ti1 O05 98.7(5) . . ? O10 Ti1 O05 164.0(6) . . ? C24 O06 Ti1 116.3(12) . . ? C25 O07 Ti1 115.2(12) . . ? C34 O10 Ti1 116.0(11) . . ? C23 O05 Ti1 112.7(13) . . ? C26 O08 Ti1 117.1(14) . . ? C02 O02 Ti2 115.9(14) . . ? C35 O11 Ti1 112.3(13) . . ? C01 O01 Ti2 110.5(12) . . ? C40 N04 C41 125.4(18) . . ? C40 N04 H04B 117.3 . . ? C41 N04 H04B 117.3 . . ? C31 N03 C32 130.7(18) . . ? C31 N03 H40B 114.6 . . ? C32 N03 H40B 114.6 . . ? C18 N02 C17 138(3) . . ? C18 N02 H02B 111.0 . . ? C17 N02 H02B 111.0 . . ? O09 C31 N03 122(2) . . ? O09 C31 C30 122(2) . . ? N03 C31 C30 116(2) . . ? N02 C18 C19 124(3) . . ? N02 C18 O04 107(3) . . ? C19 C18 O04 129(3) . . ? C08 N01 C07 129(2) . . ? C08 N01 H01B 115.4 . . ? C07 N01 H01B 115.4 . . ? O03 C07 N01 121(3) . . ? O03 C07 C06 127(3) . . ? N01 C07 C06 112(2) . . ? O12 C40 N04 124(2) . . ? O12 C40 C39 119(2) . . ? N04 C40 C39 117(2) . . ? C102 Co1 C102 119.66(8) 3_765 2_645 ? C102 Co1 C102 119.7(17) 3_765 . ? C102 Co1 C102 119.7(17) 2_645 . ? C102 Co1 C101 144.6(12) 3_765 . ? C102 Co1 C101 89.2(15) 2_645 . ? C102 Co1 C101 43.8 . . ? C102 Co1 C101 43.8(6) 3_765 3_765 ? C102 Co1 C101 144.6(8) 2_645 3_765 ? C102 Co1 C101 89.2(18) . 3_765 ? C101 Co1 C101 100.9(15) . 3_765 ? C102 Co1 C101 89.2(12) 3_765 2_645 ? C102 Co1 C101 43.8(8) 2_645 2_645 ? C101 Co1 C101 100.9(19) . 2_645 ? C101 Co1 C101 100.9(3) 3_765 2_645 ? C102 Co1 C103 43.2(4) 3_765 3_765 ? C102 Co1 C103 78.6(4) 2_645 3_765 ? C102 Co1 C103 161.6(19) . 3_765 ? C101 Co1 C103 142.8(6) . 3_765 ? C101 Co1 C103 73.0(6) 3_765 3_765 ? C101 Co1 C103 47.4(9) 2_645 3_765 ? C102 Co1 C103 78.6(17) 3_765 . ? C102 Co1 C103 161.6(17) 2_645 . ? C102 Co1 C103 43.2 . . ? C101 Co1 C103 73.0 . . ? C101 Co1 C103 47.4(17) 3_765 . ? C101 Co1 C103 142.8(6) 2_645 . ? C103 Co1 C103 118.4(19) 3_765 . ? C102 Co1 C103 161.6(2) 3_765 2_645 ? C102 Co1 C103 43.2(3) 2_645 2_645 ? C102 Co1 C103 78.6(18) . 2_645 ? C101 Co1 C103 47.4(16) . 2_645 ? C101 Co1 C103 142.8(5) 3_765 2_645 ? C101 Co1 C103 73.0(10) 2_645 2_645 ? C103 Co1 C103 118.4(2) 3_765 2_645 ? C103 Co1 C103 118.4(18) . 2_645 ? C102 Co1 C105 108.2(4) 3_765 . ? C102 Co1 C105 98.5(5) 2_645 . ? C102 Co1 C105 72.8 . . ? C101 Co1 C105 42.8 . . ? C101 Co1 C105 69.3(10) 3_765 . ? C101 Co1 C105 79.3(10) 2_645 . ? C103 Co1 C105 104.04(16) 3_765 . ? C103 Co1 C105 71.7 . . ? C103 Co1 C105 73.5(7) 2_645 . ? C102 Co1 C105 72.8(14) 3_765 3_765 ? C102 Co1 C105 98.5(18) . 3_765 ? C101 Co1 C105 79.3(14) . 3_765 ? C101 Co1 C105 42.8(15) 3_765 3_765 ? C101 Co1 C105 69.3(16) 2_645 3_765 ? C103 Co1 C105 71.7(13) 3_765 3_765 ? C103 Co1 C105 104.0(16) 2_645 3_765 ? C105 Co1 C105 36.8(14) . 3_765 ? C102 Co1 C105 72.8(14) 2_645 2_645 ? C102 Co1 C105 108.2(19) . 2_645 ? C101 Co1 C105 79.3(13) 3_765 2_645 ? C101 Co1 C105 42.8(9) 2_645 2_645 ? C103 Co1 C105 73.5(19) 3_765 2_645 ? C103 Co1 C105 104.0(13) . 2_645 ? C105 Co1 C105 36.8(16) . 2_645 ? C105 Co1 C105 36.8(12) 3_765 2_645 ? C105 C101 C102 108.01(9) . . ? C105 C101 C103 104.4(8) . 2_645 ? C102 C101 C103 110.1(9) . 2_645 ? C110 C101 C106 49.8(11) 3_765 3_765 ? C104 C101 C106 146(3) 2_645 3_765 ? C105 C101 C106 128.9(13) . 3_765 ? C103 C101 C106 89.4(15) 2_645 3_765 ? C105 C101 Co1 70.9 . . ? C102 C101 Co1 67.6 . . ? C103 C101 Co1 67.6(4) 2_645 . ? C106 C101 Co1 69.7(9) 3_765 . ? C105 C101 C109 115.7(19) . 3_765 ? C102 C101 C109 96.7(3) . 3_765 ? C103 C101 C109 14.8(2) 2_645 3_765 ? C106 C101 C109 74.9(18) 3_765 3_765 ? Co1 C101 C109 65.7(17) . 3_765 ? C109 C102 C103 24.4(9) 2_645 . ? C109 C102 C101 130.8(18) 2_645 . ? C103 C102 C101 108.1 . . ? C109 C102 C110 154.3(4) 2_645 3_765 ? C103 C102 C110 140.7(19) . 3_765 ? C101 C102 C110 36.9(5) . 3_765 ? C106 C102 C108 60.5(15) 3_765 2_645 ? C101 C102 C108 134.6(15) . 2_645 ? C103 C102 Co1 70.4 . . ? C101 C102 Co1 68.7 . . ? C108 C102 Co1 69.7(19) 2_645 . ? C106 C102 C107 35.3(16) 3_765 3_765 ? C103 C102 C107 104.1(17) . 3_765 ? C101 C102 C107 109(2) . 3_765 ? C108 C102 C107 34.8(16) 2_645 3_765 ? Co1 C102 C107 65.3(15) . 3_765 ? C110 C103 C104 74.2(13) 2_645 . ? C102 C103 C104 107.91(6) . . ? C102 C103 C101 128.5(13) . 3_765 ? C104 C103 C101 39.0(10) . 3_765 ? C109 C103 C108 30.5(19) 2_645 2_645 ? C104 C103 C108 135.3(14) . 2_645 ? C102 C103 Co1 66.4 . . ? C104 C103 Co1 70.7 . . ? C101 C103 Co1 65.0(12) 3_765 . ? C108 C103 Co1 65.3(12) 2_645 . ? C101 C104 C105 86(3) 3_765 3_765 ? C101 C104 C105 131.3(19) 3_765 . ? C105 C104 C103 140.0(17) 3_765 . ? C105 C104 C103 107.97(8) . . ? C101 C104 C110 30.1(12) 3_765 2_645 ? C105 C104 C110 138.8(12) . 2_645 ? C103 C104 C110 48.8(18) . 2_645 ? C101 C104 Co1 70.5(16) 3_765 . ? C105 C104 Co1 73.1(19) 3_765 . ? C105 C104 Co1 68.2 . . ? C103 C104 Co1 67.1 . . ? C110 C104 Co1 71.0(15) 2_645 . ? C101 C104 C109 72.6(8) 3_765 2_645 ? C105 C104 C109 136(2) 3_765 2_645 ? C105 C104 C109 108.9(11) . 2_645 ? C103 C104 C109 5.6(19) . 2_645 ? C110 C104 C109 44.7(6) 2_645 2_645 ? Co1 C104 C109 63.2(7) . 2_645 ? C104 C105 C104 143.5(11) 2_645 . ? C101 C105 C104 108.0 . . ? C104 C105 Co1 75.6(15) 2_645 . ? C101 C105 Co1 66.3 . . ? C104 C105 Co1 70.0 . . ? C110 C106 C107 107.99(7) . . ? C110 C106 C108 135.8(19) . 3_765 ? C107 C106 C108 46.0(17) . 3_765 ? C110 C106 C109 117.2(5) . 3_765 ? C107 C106 C109 92.0(6) . 3_765 ? C108 C106 C109 48.7(18) 3_765 3_765 ? C102 C106 C101 48.0(13) 2_645 2_645 ? C107 C106 C101 118.5(9) . 2_645 ? C109 C106 C101 88.4(18) 3_765 2_645 ? C110 C106 Co1 70.2 . . ? C107 C106 Co1 69.2 . . ? C108 C106 Co1 66.9(18) 3_765 . ? C109 C106 Co1 62.7(4) 3_765 . ? C101 C106 Co1 57.0(10) 2_645 . ? C108 C107 C106 108.1 . . ? C108 C107 C102 59.6(15) 3_765 2_645 ? C108 C107 C102 106.1(6) . 2_645 ? C106 C107 C102 19.3(17) . 2_645 ? C107 C107 C102 97.7(17) 3_765 2_645 ? C107 C107 C102 119.4(6) 2_645 2_645 ? C108 C107 Co1 72.8(16) 3_765 . ? C108 C107 Co1 69.2 . . ? C106 C107 Co1 71.7 . . ? C102 C107 Co1 54.9(10) 2_645 . ? C107 C108 C109 134.9(9) 2_645 . ? C107 C108 C109 107.9 . . ? C107 C108 C106 136.8(12) . 2_645 ? C109 C108 C106 78.4(16) . 2_645 ? C107 C108 C102 129.7(11) . 3_765 ? C109 C108 C102 51.7(17) . 3_765 ? C106 C108 C102 27.9(4) 2_645 3_765 ? C107 C108 C103 124(2) 2_645 3_765 ? C107 C108 C103 103.6(11) . 3_765 ? C109 C108 C103 12.3(12) . 3_765 ? C106 C108 C103 73.4(8) 2_645 3_765 ? C102 C108 C103 45.6(8) 3_765 3_765 ? C107 C108 Co1 71.2 . . ? C109 C108 Co1 70.6 . . ? C106 C108 Co1 71.2(9) 2_645 . ? C102 C108 Co1 58.9(13) 3_765 . ? C103 C108 Co1 58.4(9) 3_765 . ? C102 C109 C110 129.1(14) 3_765 . ? C103 C109 C108 137(4) 3_765 . ? C110 C109 C108 108.03(5) . . ? C102 C109 C106 24.1(10) 3_765 2_645 ? C110 C109 C106 136.9(9) . 2_645 ? C108 C109 C106 52.8(7) . 2_645 ? C103 C109 C101 41(3) 3_765 2_645 ? C102 C109 C101 104.7(7) 3_765 2_645 ? C110 C109 C101 26.1(6) . 2_645 ? C108 C109 C101 114.7(17) . 2_645 ? C106 C109 C101 118.9(11) 2_645 2_645 ? C103 C109 C104 13.4(7) 3_765 3_765 ? C108 C109 C104 127.9(11) . 3_765 ? C106 C109 C104 104(3) 2_645 3_765 ? C101 C109 C104 29.3(17) 2_645 3_765 ? C102 C109 Co1 62.1(19) 3_765 . ? C110 C109 Co1 71.8 . . ? C108 C109 Co1 69.6 . . ? C106 C109 Co1 65.3(9) 2_645 . ? C101 C109 Co1 56.3(16) 2_645 . ? C104 C109 Co1 58.4(11) 3_765 . ? C101 C110 C109 111(2) 2_645 . ? C103 C110 C109 24.88(18) 3_765 . ? C103 C110 C106 124.0(15) 3_765 . ? C109 C110 C106 108.0 . . ? C103 C110 C102 124.5(3) 3_765 2_645 ? C109 C110 C102 122.9(14) . 2_645 ? C106 C110 C102 32.5(6) . 2_645 ? C106 C110 C104 125.1(12) . 3_765 ? C109 C110 Co1 68.9 . . ? C106 C110 Co1 70.9 . . ? C102 C110 Co1 60.3(18) 2_645 . ? C104 C110 Co1 62.5(18) 3_765 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O01 C01 C02 O02 5(3) . . . . ? C06 C01 C02 O02 -174(2) . . . . ? O01 C01 C02 C03 -179(2) . . . . ? C06 C01 C02 C03 2(4) . . . . ? O02 C02 C03 C04 172(2) . . . . ? C01 C02 C03 C04 -4(4) . . . . ? C02 C03 C04 C05 3(4) . . . . ? C03 C04 C05 C06 -1(4) . . . . ? O01 C01 C06 C05 -179(2) . . . . ? C02 C01 C06 C05 1(4) . . . . ? O01 C01 C06 C07 2(4) . . . . ? C02 C01 C06 C07 -179(2) . . . . ? C04 C05 C06 C01 -1(4) . . . . ? C04 C05 C06 C07 178(2) . . . . ? C13 C08 C09 C10 -4(4) . . . . ? N01 C08 C09 C10 176(2) . . . . ? C08 C09 C10 C11 -2(4) . . . . ? C09 C10 C11 C12 3(4) . . . . ? C10 C11 C12 C17 -179(2) . . . . ? C10 C11 C12 C13 3(3) . . . . ? N01 C08 C13 C12 -171(2) . . . . ? C09 C08 C13 C12 10(4) . . . . ? N01 C08 C13 C14 7(4) . . . . ? C09 C08 C13 C14 -172(2) . . . . ? C17 C12 C13 C08 172(2) . . . . ? C11 C12 C13 C08 -9(4) . . . . ? C17 C12 C13 C14 -6(4) . . . . ? C11 C12 C13 C14 173(2) . . . . ? C08 C13 C14 C15 -174(2) . . . . ? C12 C13 C14 C15 4(4) . . . . ? C13 C14 C15 C16 -2(4) . . . . ? C14 C15 C16 C17 3(4) . . . . ? C13 C12 C17 C16 6(4) . . . . ? C11 C12 C17 C16 -173(2) . . . . ? C13 C12 C17 N02 -169(2) . . . . ? C11 C12 C17 N02 12(4) . . . . ? C15 C16 C17 C12 -4(4) . . . . ? C15 C16 C17 N02 170(2) . . . . ? C18 C19 C20 C21 -177(2) . . . . ? C24 C19 C20 C21 0(3) . . . . ? C19 C20 C21 C22 -2(4) . . . . ? C20 C21 C22 C23 3(4) . . . . ? C21 C22 C23 O05 179(2) . . . . ? C21 C22 C23 C24 -4(3) . . . . ? O05 C23 C24 O06 2(3) . . . . ? C22 C23 C24 O06 -175.6(18) . . . . ? C18 C19 C24 C23 176(3) . . . . ? C20 C19 C24 O06 177.1(19) . . . . ? C39 C34 C35 O11 -177.8(18) . . . . ? O11 C35 C36 C37 -176(2) . . . . ? C30 C25 C26 O08 -179.6(19) . . . . ? O07 C25 C26 C27 -178.5(19) . . . . ? C30 C25 C26 C27 -1(3) . . . . ? O08 C26 C27 C28 -177(2) . . . . ? N04 C41 C42 C43 177.8(18) . . . . ? C41 C42 C43 C44 1(3) . . . . ? C42 C43 C44 C45 5(3) . . . . ? C43 C44 C45 C32 179(2) . . . 2_645 ? C43 C44 C45 C46 -5(3) . . . . ? C42 C41 C46 C45 7(3) . . . . ? N04 C41 C46 C45 -177.9(17) . . . . ? C42 C41 C46 C47 -177.9(19) . . . . ? N04 C41 C46 C47 -3(3) . . . . ? C32 C45 C46 C41 175.8(18) 2_645 . . . ? C44 C45 C46 C41 -1(3) . . . . ? C32 C45 C46 C47 0(3) 2_645 . . . ? C44 C45 C46 C47 -176.2(17) . . . . ? C41 C46 C47 C48 -178(2) . . . . ? C45 C46 C47 C48 -3(3) . . . . ? C45 C32 C33 C48 -4(3) 3_765 . . 3_765 ? N03 C32 C33 C48 176.6(19) . . . 3_765 ? C205 Co2 C205 C201 -157.1(15) 10_545 . . . ? C204 Co2 C205 C201 -113.3(11) 10_545 . . . ? C204 Co2 C205 C201 119.7 . . . . ? C203 Co2 C205 C201 -71.5(6) 10_545 . . . ? C203 Co2 C205 C201 81.79(7) . . . . ? C201 Co2 C205 C201 167.5(17) 10_545 . . . ? C202 Co2 C205 C201 -37.2(19) 10_545 . . . ? C202 Co2 C205 C201 37.48(7) . . . . ? C205 Co2 C205 C204 83.2(15) 10_545 . . . ? C204 Co2 C205 C204 127.0(11) 10_545 . . . ? C203 Co2 C205 C204 168.8(6) 10_545 . . . ? C203 Co2 C205 C204 -37.89(9) . . . . ? C201 Co2 C205 C204 -119.7 . . . . ? C201 Co2 C205 C204 47.9(17) 10_545 . . . ? C202 Co2 C205 C204 -156.9(19) 10_545 . . . ? C202 Co2 C205 C204 -82.20(9) . . . . ? C204 C205 C201 C202 0.2 . . . . ? Co2 C205 C201 C202 -58.43(11) . . . . ? C204 C205 C201 Co2 58.59(12) . . . . ? C205 Co2 C201 C202 170(2) 10_545 . . . ? C205 Co2 C201 C202 120.1 . . . . ? C204 Co2 C201 C202 -155.9(5) 10_545 . . . ? C204 Co2 C201 C202 82.11(9) . . . . ? C203 Co2 C201 C202 -112.7(3) 10_545 . . . ? C203 Co2 C201 C202 37.62(10) . . . . ? C201 Co2 C201 C202 -40(3) 10_545 . . . ? C202 Co2 C201 C202 -71.5(10) 10_545 . . . ? C205 Co2 C201 C205 50(2) 10_545 . . . ? C204 Co2 C201 C205 83.9(4) 10_545 . . . ? C204 Co2 C201 C205 -38.03(12) . . . . ? C203 Co2 C201 C205 127.2(3) 10_545 . . . ? C203 Co2 C201 C205 -82.53(13) . . . . ? C201 Co2 C201 C205 -160(3) 10_545 . . . ? C202 Co2 C201 C205 168.4(10) 10_545 . . . ? C202 Co2 C201 C205 -120.1 . . . . ? C205 C201 C202 C203 -0.1 . . . . ? Co2 C201 C202 C203 -58.01(11) . . . . ? C205 C201 C202 Co2 57.86(12) . . . . ? C205 Co2 C202 C201 -164(3) 10_545 . . . ? C205 Co2 C202 C201 -37.72(7) . . . . ? C204 Co2 C202 C201 50.5(12) 10_545 . . . ? C204 Co2 C202 C201 -82.39(17) . . . . ? C203 Co2 C202 C201 83.5(8) 10_545 . . . ? C203 Co2 C202 C201 -120.15(19) . . . . ? C201 Co2 C202 C201 167.0(9) 10_545 . . . ? C202 Co2 C202 C201 126.4(11) 10_545 . . . ? C205 Co2 C202 C203 -43(2) 10_545 . . . ? C205 Co2 C202 C203 82.4(2) . . . . ? C204 Co2 C202 C203 170.7(13) 10_545 . . . ? C204 Co2 C202 C203 37.76(7) . . . . ? C203 Co2 C202 C203 -156.3(9) 10_545 . . . ? C201 Co2 C202 C203 120.2(2) . . . . ? C201 Co2 C202 C203 -72.9(10) 10_545 . . . ? C202 Co2 C202 C203 -113.4(12) 10_545 . . . ? C201 C202 C203 C204 0.1 . . . . ? Co2 C202 C203 C204 -58.0(2) . . . . ? C201 C202 C203 Co2 58.1(2) . . . . ? C205 Co2 C203 C204 -73.4(4) 10_545 . . . ? C205 Co2 C203 C204 38.03(5) . . . . ? C204 Co2 C203 C204 -42(4) 10_545 . . . ? C203 Co2 C203 C204 168.7(19) 10_545 . . . ? C201 Co2 C203 C204 82.51(11) . . . . ? C201 Co2 C203 C204 -114.4(3) 10_545 . . . ? C202 Co2 C203 C204 -157.5(10) 10_545 . . . ? C202 Co2 C203 C204 120.03(11) . . . . ? C205 Co2 C203 C202 166.6(5) 10_545 . . . ? C205 Co2 C203 C202 -82.00(12) . . . . ? C204 Co2 C203 C202 -120.03(12) . . . . ? C203 Co2 C203 C202 48.6(19) 10_545 . . . ? C201 Co2 C203 C202 -37.51(5) . . . . ? C201 Co2 C203 C202 125.6(4) 10_545 . . . ? C202 Co2 C203 C202 82.5(10) 10_545 . . . ? C202 C203 C204 C205 0.0 . . . . ? Co2 C203 C204 C205 -58.47(15) . . . . ? C202 C203 C204 Co2 58.50(14) . . . . ? C201 C205 C204 C203 -0.1 . . . . ? Co2 C205 C204 C203 58.8 . . . . ? C201 C205 C204 Co2 -58.9 . . . . ? C205 Co2 C204 C203 126.0(10) 10_545 . . . ? C205 Co2 C204 C203 -119.68(11) . . . . ? C204 Co2 C204 C203 167.7(15) 10_545 . . . ? C203 Co2 C204 C203 -158(3) 10_545 . . . ? C201 Co2 C204 C203 -81.80(14) . . . . ? C201 Co2 C204 C203 82.3(5) 10_545 . . . ? C202 Co2 C204 C203 47.1(11) 10_545 . . . ? C202 Co2 C204 C203 -37.63(7) . . . . ? C205 Co2 C204 C205 -114.3(10) 10_545 . . . ? C204 Co2 C204 C205 -72.6(15) 10_545 . . . ? C203 Co2 C204 C205 -39(3) 10_545 . . . ? C203 Co2 C204 C205 119.68(11) . . . . ? C201 Co2 C204 C205 37.88(7) . . . . ? C201 Co2 C204 C205 -158.0(5) 10_545 . . . ? C202 Co2 C204 C205 166.8(11) 10_545 . . . ? C202 Co2 C204 C205 82.05(11) . . . . ? C46 C47 C48 C33 2(3) . . . 2_645 ? C23 C24 O06 Ti1 -7(2) . . . . ? C19 C24 O06 Ti1 174.0(17) . . . . ? O08 Ti1 O06 C24 56(4) . . . . ? O11 Ti1 O06 C24 -81.4(13) . . . . ? O07 Ti1 O06 C24 105.9(13) . . . . ? O10 Ti1 O06 C24 -161.2(13) . . . . ? O05 Ti1 O06 C24 7.4(12) . . . . ? C30 C25 O07 Ti1 177.4(17) . . . . ? C26 C25 O07 Ti1 -6(2) . . . . ? O08 Ti1 O07 C25 4.8(13) . . . . ? O11 Ti1 O07 C25 49(3) . . . . ? O06 Ti1 O07 C25 -166.3(13) . . . . ? O10 Ti1 O07 C25 104.1(13) . . . . ? O05 Ti1 O07 C25 -86.9(13) . . . . ? C39 C34 O10 Ti1 173.4(16) . . . . ? C35 C34 O10 Ti1 -1(2) . . . . ? O08 Ti1 O10 C34 -85.7(13) . . . . ? O11 Ti1 O10 C34 3.1(13) . . . . ? O06 Ti1 O10 C34 101.3(13) . . . . ? O07 Ti1 O10 C34 -166.7(13) . . . . ? O05 Ti1 O10 C34 57(3) . . . . ? C24 C23 O05 Ti1 4(3) . . . . ? C22 C23 O05 Ti1 -178.6(17) . . . . ? O08 Ti1 O05 C23 -177.4(14) . . . . ? O11 Ti1 O05 C23 92.1(14) . . . . ? O06 Ti1 O05 C23 -5.9(13) . . . . ? O07 Ti1 O05 C23 -96.4(14) . . . . ? O10 Ti1 O05 C23 40(3) . . . . ? C27 C26 O08 Ti1 -177(2) . . . . ? C25 C26 O08 Ti1 1(3) . . . . ? O11 Ti1 O08 C26 -174.4(16) . . . . ? O06 Ti1 O08 C26 48(4) . . . . ? O07 Ti1 O08 C26 -3.0(16) . . . . ? O10 Ti1 O08 C26 -94.5(16) . . . . ? O05 Ti1 O08 C26 95.3(16) . . . . ? C03 C02 O02 Ti2 -168.7(17) . . . . ? C01 C02 O02 Ti2 8(3) . . . . ? O02 Ti2 O02 C02 175.2(16) 2_645 . . . ? O02 Ti2 O02 C02 85.5(18) 3_765 . . . ? O01 Ti2 O02 C02 51(4) 3_765 . . . ? O01 Ti2 O02 C02 -105.0(16) 2_645 . . . ? O01 Ti2 O02 C02 -12.2(15) . . . . ? C34 C35 O11 Ti1 5(2) . . . . ? C36 C35 O11 Ti1 -176.9(16) . . . . ? O08 Ti1 O11 C35 95.5(14) . . . . ? O06 Ti1 O11 C35 -92.3(14) . . . . ? O07 Ti1 O11 C35 52(3) . . . . ? O10 Ti1 O11 C35 -4.2(13) . . . . ? O05 Ti1 O11 C35 -171.4(14) . . . . ? C06 C01 O01 Ti2 165(2) . . . . ? C02 C01 O01 Ti2 -15(2) . . . . ? O02 Ti2 O01 C01 14.1(13) . . . . ? O02 Ti2 O01 C01 50(3) 2_645 . . . ? O02 Ti2 O01 C01 -74.3(14) 3_765 . . . ? O01 Ti2 O01 C01 -154.6(14) 3_765 . . . ? O01 Ti2 O01 C01 111.0(15) 2_645 . . . ? C42 C41 N04 C40 -33(3) . . . . ? C46 C41 N04 C40 151.3(19) . . . . ? C45 C32 N03 C31 155(2) 3_765 . . . ? C33 C32 N03 C31 -26(3) . . . . ? C12 C17 N02 C18 131(3) . . . . ? C16 C17 N02 C18 -44(4) . . . . ? C32 N03 C31 C30 -170.7(18) . . . . ? C29 C30 C31 N03 176.2(18) . . . . ? C41 N04 C40 C39 -174.3(17) . . . . ? C34 C39 C40 O12 -176.2(19) . . . . ? C38 C39 C40 O12 7(3) . . . . ? C34 C39 C40 N04 2(3) . . . . ? C38 C39 C40 N04 -175.3(18) . . . . ? C102 Co1 C101 C110 149.5(16) 3_765 . . 3_765 ? C103 Co1 C101 C110 -133.5(11) 3_765 . . 3_765 ? C102 Co1 C101 C105 103.4(8) 2_645 . . . ? C102 Co1 C101 C105 -119.8 . . . . ? C101 Co1 C101 C105 -42.5(10) 3_765 . . . ? C101 Co1 C101 C105 60.9(10) 2_645 . . . ? C103 Co1 C101 C105 -81.2 . . . . ? C103 Co1 C101 C105 115.3(11) 2_645 . . . ? C105 Co1 C101 C105 31.5(16) 2_645 . . . ? C102 Co1 C101 C102 -136.9(8) 2_645 . . . ? C101 Co1 C101 C102 77.3(10) 3_765 . . . ? C103 Co1 C101 C102 38.5 . . . . ? C103 Co1 C101 C102 -124.9(11) 2_645 . . . ? C105 Co1 C101 C102 119.8 . . . . ? C105 Co1 C101 C102 151.3(16) 2_645 . . . ? C102 Co1 C101 C103 -158.7(11) 3_765 . . 2_645 ? C102 Co1 C101 C103 -12.0(3) 2_645 . . 2_645 ? C102 Co1 C101 C103 124.9(11) . . . 2_645 ? C101 Co1 C101 C103 -157.8(7) 3_765 . . 2_645 ? C101 Co1 C101 C103 -54.4(7) 2_645 . . 2_645 ? C103 Co1 C101 C103 -81.7(18) 3_765 . . 2_645 ? C103 Co1 C101 C103 163.4(11) . . . 2_645 ? C105 Co1 C101 C103 -115.3(11) . . . 2_645 ? C105 Co1 C101 C103 -120.7(19) 3_765 . . 2_645 ? C105 Co1 C101 C103 -83.8(18) 2_645 . . 2_645 ? C102 Co1 C101 C106 103.3(11) 3_765 . . 3_765 ? C102 Co1 C101 C106 -110.0(18) 2_645 . . 3_765 ? C101 Co1 C101 C106 104.2(16) 3_765 . . 3_765 ? C101 Co1 C101 C106 -152.4(16) 2_645 . . 3_765 ? C103 Co1 C101 C106 -98.0(15) 2_645 . . 3_765 ? C105 Co1 C101 C106 141.3(18) 3_765 . . 3_765 ? C102 Co1 C101 C109 -174.6(10) 3_765 . . 3_765 ? C102 Co1 C101 C109 -27.9(5) 2_645 . . 3_765 ? C102 Co1 C101 C109 109.0(12) . . . 3_765 ? C101 Co1 C101 C109 -173.8(6) 3_765 . . 3_765 ? C101 Co1 C101 C109 -70.3(6) 2_645 . . 3_765 ? C103 Co1 C101 C109 -97.7(17) 3_765 . . 3_765 ? C103 Co1 C101 C109 147.5(12) . . . 3_765 ? C103 Co1 C101 C109 -15.9(3) 2_645 . . 3_765 ? C105 Co1 C101 C109 -131.3(12) . . . 3_765 ? C105 Co1 C101 C109 -136.6(18) 3_765 . . 3_765 ? C105 Co1 C101 C109 -99.7(17) 2_645 . . 3_765 ? C109 C101 C102 C106 29.7(13) 3_765 . . 3_765 ? C110 C101 C102 C109 -146.4(16) 3_765 . . 2_645 ? C106 C101 C102 C109 -139.0(18) 3_765 . . 2_645 ? C109 C101 C102 C109 -109.3(8) 3_765 . . 2_645 ? C103 C101 C102 C103 -113.4(6) 2_645 . . . ? Co1 C101 C102 C103 -59.6 . . . . ? C105 C101 C102 Co1 59.6 . . . . ? C103 C101 C102 Co1 -53.9(6) 2_645 . . . ? C105 C101 C102 C107 112.4(14) . . . 3_765 ? Co1 C101 C102 C107 52.8(14) . . . 3_765 ? C102 Co1 C102 C109 4.41(17) 3_765 . . 2_645 ? C102 Co1 C102 C109 -164.05(17) 2_645 . . 2_645 ? C101 Co1 C102 C109 144.07(9) . . . 2_645 ? C101 Co1 C102 C109 37.4(6) 3_765 . . 2_645 ? C101 Co1 C102 C109 145.3(17) 2_645 . . 2_645 ? C103 Co1 C102 C109 23.3(8) 3_765 . . 2_645 ? C103 Co1 C102 C109 24.52(9) . . . 2_645 ? C103 Co1 C102 C109 -177.9(3) 2_645 . . 2_645 ? C105 Co1 C102 C109 105.93(8) . . . 2_645 ? C105 Co1 C102 C109 79.3(18) 3_765 . . 2_645 ? C105 Co1 C102 C109 115.8(19) 2_645 . . 2_645 ? C102 Co1 C102 C103 -20.11(14) 3_765 . . . ? C102 Co1 C102 C103 171.44(14) 2_645 . . . ? C101 Co1 C102 C103 119.5 . . . . ? C101 Co1 C102 C103 12.9(6) 3_765 . . . ? C101 Co1 C102 C103 120.7(17) 2_645 . . . ? C103 Co1 C102 C103 157.5(3) 2_645 . . . ? C105 Co1 C102 C103 81.4 . . . . ? C105 Co1 C102 C103 54.8(18) 3_765 . . . ? C102 Co1 C102 C101 -139.66(14) 3_765 . . . ? C102 Co1 C102 C101 51.89(14) 2_645 . . . ? C101 Co1 C102 C101 -106.7(6) 3_765 . . . ? C101 Co1 C102 C101 1.2(17) 2_645 . . . ? C103 Co1 C102 C101 -120.8(8) 3_765 . . . ? C103 Co1 C102 C101 -119.5 . . . . ? C103 Co1 C102 C101 38.0(3) 2_645 . . . ? C105 Co1 C102 C101 -38.1 . . . . ? C105 Co1 C102 C101 -64.7(18) 3_765 . . . ? C102 Co1 C102 C110 -177.32(16) 3_765 . . 3_765 ? C102 Co1 C102 C110 14.22(16) 2_645 . . 3_765 ? C101 Co1 C102 C110 -37.7(3) . . . 3_765 ? C101 Co1 C102 C110 -144.3(4) 3_765 . . 3_765 ? C101 Co1 C102 C110 -36.5(19) 2_645 . . 3_765 ? C103 Co1 C102 C110 -158.4(11) 3_765 . . 3_765 ? C103 Co1 C102 C110 -157.2(3) . . . 3_765 ? C103 Co1 C102 C110 0.3 2_645 . . 3_765 ? C105 Co1 C102 C110 -75.8(3) . . . 3_765 ? C105 Co1 C102 C110 -102.4(18) 3_765 . . 3_765 ? C101 Co1 C102 C108 -160.1(6) 2_645 . . 2_645 ? C103 Co1 C102 C108 77.9(16) 3_765 . . 2_645 ? C105 Co1 C102 C108 134.0(15) 3_765 . . 2_645 ? C105 Co1 C102 C108 170.5(5) 2_645 . . 2_645 ? C101 Co1 C102 C107 -122.6(14) 2_645 . . 3_765 ? C103 Co1 C102 C107 115.5(19) 3_765 . . 3_765 ? C105 Co1 C102 C107 171.5(10) 3_765 . . 3_765 ? C105 Co1 C102 C107 -152.0(15) 2_645 . . 3_765 ? C108 C102 C103 C104 -132.4(17) 2_645 . . . ? Co1 C102 C103 C104 -58.6 . . . . ? C101 C102 C103 C101 38.0(12) . . . 3_765 ? Co1 C102 C103 C101 -20.5(11) . . . 3_765 ? C107 C102 C103 C101 -77.4(14) 3_765 . . 3_765 ? C101 C102 C103 C108 132.3(17) . . . 2_645 ? C110 C102 C103 C108 110.4(19) 3_765 . . 2_645 ? Co1 C102 C103 C108 73.8(17) . . . 2_645 ? C101 C102 C103 Co1 58.5 . . . . ? C108 C102 C103 Co1 -73.8(17) 2_645 . . . ? C102 Co1 C103 C110 -162.6(5) . . . 2_645 ? C101 Co1 C103 C110 158.4(5) . . . 2_645 ? C101 Co1 C103 C110 35.0(16) 3_765 . . 2_645 ? C101 Co1 C103 C110 73(3) 2_645 . . 2_645 ? C103 Co1 C103 C110 16.9(2) 3_765 . . 2_645 ? C103 Co1 C103 C110 172.2(2) 2_645 . . 2_645 ? C105 Co1 C103 C110 113.4(5) . . . 2_645 ? C105 Co1 C103 C110 74.8(16) 3_765 . . 2_645 ? C102 Co1 C103 C102 162.3(3) 3_765 . . . ? C102 Co1 C103 C102 -24.2(14) 2_645 . . . ? C101 Co1 C103 C102 -39.0 . . . . ? C101 Co1 C103 C102 -162.4(11) 3_765 . . . ? C103 Co1 C103 C102 -25.2(3) 2_645 . . . ? C105 Co1 C103 C102 -84.0 . . . . ? C105 Co1 C103 C102 -122.6(14) 3_765 . . . ? C105 Co1 C103 C102 -102(2) 2_645 . . . ? C102 Co1 C103 C104 -77.2(3) 3_765 . . . ? C102 Co1 C103 C104 96.3(14) 2_645 . . . ? C102 Co1 C103 C104 120.59(6) . . . . ? C101 Co1 C103 C104 81.6 . . . . ? C101 Co1 C103 C104 -41.8(11) 3_765 . . . ? C101 Co1 C103 C104 -4(3) 2_645 . . . ? C103 Co1 C103 C104 -59.8(3) 3_765 . . . ? C103 Co1 C103 C104 95.4(3) 2_645 . . . ? C105 Co1 C103 C104 36.6 . . . . ? C105 Co1 C103 C104 -2.0(15) 3_765 . . . ? C105 Co1 C103 C104 19(2) 2_645 . . . ? C102 Co1 C103 C101 -35.4(14) 3_765 . . 3_765 ? C102 Co1 C103 C101 138(2) 2_645 . . 3_765 ? C102 Co1 C103 C101 162.4(11) . . . 3_765 ? C101 Co1 C103 C101 123.4(11) . . . 3_765 ? C101 Co1 C103 C101 38(4) 2_645 . . 3_765 ? C103 Co1 C103 C101 -18.1(14) 3_765 . . 3_765 ? C103 Co1 C103 C101 137.2(14) 2_645 . . 3_765 ? C105 Co1 C103 C101 78.4(11) . . . 3_765 ? C105 Co1 C103 C101 39.8(12) 3_765 . . 3_765 ? C101 Co1 C103 C108 168.0(11) 2_645 . . 2_645 ? C105 Co1 C103 C108 -151(3) . . . 2_645 ? C105 Co1 C103 C108 -169.2(9) 2_645 . . 2_645 ? C102 C103 C104 C101 129.8(18) . . . 3_765 ? C108 C103 C104 C101 64(5) 2_645 . . 3_765 ? Co1 C103 C104 C101 73.9(18) . . . 3_765 ? C101 C103 C104 C105 -129.7(18) 3_765 . . . ? C108 C103 C104 C105 -66(4) 2_645 . . . ? Co1 C103 C104 C105 -55.8 . . . . ? C102 C103 C104 Co1 56.0 . . . . ? C101 C103 C104 Co1 -73.9(18) 3_765 . . . ? C102 Co1 C104 C101 7.4(16) 3_765 . . 3_765 ? C102 Co1 C104 C101 122.8(15) 2_645 . . 3_765 ? C101 Co1 C104 C101 93.3(8) 2_645 . . 3_765 ? C103 Co1 C104 C101 46.1(15) 3_765 . . 3_765 ? C103 Co1 C104 C101 169.3(15) 2_645 . . 3_765 ? C105 Co1 C104 C101 116.1(17) 2_645 . . 3_765 ? C102 Co1 C104 C105 -146.3(14) 3_765 . . . ? C102 Co1 C104 C105 83.8 . . . . ? C101 Co1 C104 C105 37.7 . . . . ? C101 Co1 C104 C105 -154(3) 3_765 . . . ? C101 Co1 C104 C105 -60(2) 2_645 . . . ? C103 Co1 C104 C105 -107.6(13) 3_765 . . . ? C103 Co1 C104 C105 122.0 . . . . ? C103 Co1 C104 C105 15.6(16) 2_645 . . . ? C105 Co1 C104 C105 -62(3) 3_765 . . . ? C105 Co1 C104 C105 -38(3) 2_645 . . . ? C102 Co1 C104 C103 91.7(15) 3_765 . . . ? C102 Co1 C104 C103 -153(3) 2_645 . . . ? C102 Co1 C104 C103 -38.25(6) . . . . ? C101 Co1 C104 C103 -84.37(6) . . . . ? C103 Co1 C104 C103 130.4(13) 3_765 . . . ? C103 Co1 C104 C103 -106.5(17) 2_645 . . . ? C105 Co1 C104 C103 -122.02(7) . . . . ? C102 Co1 C104 C110 39.3(9) 3_765 . . 2_645 ? C102 Co1 C104 C110 154.7(2) 2_645 . . 2_645 ? C102 Co1 C104 C110 -91(2) . . . 2_645 ? C101 Co1 C104 C110 -137(2) . . . 2_645 ? C101 Co1 C104 C110 31.9(14) 3_765 . . 2_645 ? C101 Co1 C104 C110 125.1(11) 2_645 . . 2_645 ? C103 Co1 C104 C110 78.0(11) 3_765 . . 2_645 ? C103 Co1 C104 C110 -158.9(8) 2_645 . . 2_645 ? C105 Co1 C104 C110 -174(2) . . . 2_645 ? C105 Co1 C104 C110 124(4) 3_765 . . 2_645 ? C105 Co1 C104 C110 148(2) 2_645 . . 2_645 ? C102 Co1 C104 C109 87.3(8) 3_765 . . 2_645 ? C102 Co1 C104 C109 -157.3(6) 2_645 . . 2_645 ? C102 Co1 C104 C109 -43(2) . . . 2_645 ? C101 Co1 C104 C109 -89(2) . . . 2_645 ? C101 Co1 C104 C109 79.9(11) 3_765 . . 2_645 ? C101 Co1 C104 C109 173.2(6) 2_645 . . 2_645 ? C103 Co1 C104 C109 126.0(9) 3_765 . . 2_645 ? C103 Co1 C104 C109 -4(2) . . . 2_645 ? C103 Co1 C104 C109 -110.8(6) 2_645 . . 2_645 ? C105 Co1 C104 C109 -126(2) . . . 2_645 ? C105 Co1 C104 C109 172(3) 3_765 . . 2_645 ? C105 Co1 C104 C109 -164.0(19) 2_645 . . 2_645 ? C102 C101 C105 C104 0.1 . . . . ? C103 C101 C105 C104 117.3(7) 2_645 . . . ? C106 C101 C105 C104 16(3) 3_765 . . . ? Co1 C101 C105 C104 57.6 . . . . ? C109 C101 C105 C104 107.0(7) 3_765 . . . ? C110 C101 C105 Co1 36(4) 3_765 . . . ? C104 C101 C105 Co1 93(3) 2_645 . . . ? C102 C101 C105 Co1 -57.5 . . . . ? C103 C101 C105 Co1 59.7(7) 2_645 . . . ? C106 C101 C105 Co1 -41(3) 3_765 . . . ? C109 C101 C105 Co1 49.4(7) 3_765 . . . ? C105 C104 C105 C101 -138.5(17) 3_765 . . . ? C103 C104 C105 C101 -0.1 . . . . ? C110 C104 C105 C101 -47(4) 2_645 . . . ? Co1 C104 C105 C101 -55.3 . . . . ? C109 C104 C105 C101 -6.0(18) 2_645 . . . ? C101 C104 C105 Co1 -34(3) 3_765 . . . ? C105 C104 C105 Co1 -83.2(17) 3_765 . . . ? C103 C104 C105 Co1 55.2 . . . . ? C110 C104 C105 Co1 8(4) 2_645 . . . ? C109 C104 C105 Co1 49.4(18) 2_645 . . . ? C102 Co1 C105 C104 -158(2) 3_765 . . 2_645 ? C102 Co1 C105 C104 -33(2) 2_645 . . 2_645 ? C102 Co1 C105 C104 85(3) . . . 2_645 ? C101 Co1 C105 C104 46(3) . . . 2_645 ? C101 Co1 C105 C104 -179(2) 3_765 . . 2_645 ? C101 Co1 C105 C104 -72.7(18) 2_645 . . 2_645 ? C103 Co1 C105 C104 -113.4(19) 3_765 . . 2_645 ? C103 Co1 C105 C104 131(3) . . . 2_645 ? C103 Co1 C105 C104 2.5(19) 2_645 . . 2_645 ? C105 Co1 C105 C104 -142(3) 3_765 . . 2_645 ? C105 Co1 C105 C104 -79(3) 2_645 . . 2_645 ? C102 Co1 C105 C101 155.3(17) 3_765 . . . ? C102 Co1 C105 C101 -79.6(16) 2_645 . . . ? C102 Co1 C105 C101 38.9 . . . . ? C101 Co1 C105 C101 134.8(17) 3_765 . . . ? C101 Co1 C105 C101 -119(2) 2_645 . . . ? C103 Co1 C105 C101 -159.8(19) 3_765 . . . ? C103 Co1 C105 C101 84.4 . . . . ? C103 Co1 C105 C101 -43.9(17) 2_645 . . . ? C105 Co1 C105 C101 171(4) 3_765 . . . ? C105 Co1 C105 C101 -125(4) 2_645 . . . ? C102 Co1 C105 C104 34.0(17) 3_765 . . . ? C102 Co1 C105 C104 159.1(16) 2_645 . . . ? C102 Co1 C105 C104 -82.4 . . . . ? C101 Co1 C105 C104 -121.3 . . . . ? C101 Co1 C105 C104 13.5(17) 3_765 . . . ? C101 Co1 C105 C104 120(2) 2_645 . . . ? C103 Co1 C105 C104 78.8(19) 3_765 . . . ? C103 Co1 C105 C104 -36.9 . . . . ? C103 Co1 C105 C104 -165.2(17) 2_645 . . . ? C105 Co1 C105 C104 50(4) 3_765 . . . ? C105 Co1 C105 C104 113(4) 2_645 . . . ? C102 Co1 C106 C102 133(3) 3_765 . . 2_645 ? C102 Co1 C106 C102 -79(4) . . . 2_645 ? C101 Co1 C106 C102 -34(4) . . . 2_645 ? C101 Co1 C106 C102 107(4) 3_765 . . 2_645 ? C101 Co1 C106 C102 56(2) 2_645 . . 2_645 ? C103 Co1 C106 C102 106(3) 3_765 . . 2_645 ? C103 Co1 C106 C102 -124(4) . . . 2_645 ? C103 Co1 C106 C102 -34(3) 2_645 . . 2_645 ? C105 Co1 C106 C102 11(4) . . . 2_645 ? C105 Co1 C106 C102 54(5) 3_765 . . 2_645 ? C105 Co1 C106 C102 34(4) 2_645 . . 2_645 ? C102 Co1 C106 C110 47.4(8) 3_765 . . . ? C102 Co1 C106 C110 -86(4) 2_645 . . . ? C102 Co1 C106 C110 -165.2 . . . . ? C101 Co1 C106 C110 -120.14(5) . . . . ? C101 Co1 C106 C110 21.3(8) 3_765 . . . ? C101 Co1 C106 C110 -30(3) 2_645 . . . ? C103 Co1 C106 C110 20.6(8) 3_765 . . . ? C103 Co1 C106 C110 149.72(18) . . . . ? C103 Co1 C106 C110 -119.9(10) 2_645 . . . ? C105 Co1 C106 C110 -74.96(5) . . . . ? C105 Co1 C106 C110 -31.7(16) 3_765 . . . ? C105 Co1 C106 C110 -52(2) 2_645 . . . ? C102 Co1 C106 C107 -71.7(8) 3_765 . . . ? C102 Co1 C106 C107 155(4) 2_645 . . . ? C102 Co1 C106 C107 75.59(5) . . . . ? C101 Co1 C106 C107 120.7 . . . . ? C101 Co1 C106 C107 -97.9(9) 3_765 . . . ? C101 Co1 C106 C107 -149(3) 2_645 . . . ? C103 Co1 C106 C107 -98.5(7) 3_765 . . . ? C103 Co1 C106 C107 30.53(8) . . . . ? C103 Co1 C106 C107 120.9(9) 2_645 . . . ? C105 Co1 C106 C107 165.9 . . . . ? C105 Co1 C106 C107 -150.9(17) 3_765 . . . ? C105 Co1 C106 C107 -171(2) 2_645 . . . ? C102 Co1 C106 C108 -122(2) 3_765 . . 3_765 ? C102 Co1 C106 C108 105(5) 2_645 . . 3_765 ? C102 Co1 C106 C108 25.8(18) . . . 3_765 ? C101 Co1 C106 C108 70.9(18) . . . 3_765 ? C101 Co1 C106 C108 -147.7(11) 3_765 . . 3_765 ? C101 Co1 C106 C108 161(3) 2_645 . . 3_765 ? C103 Co1 C106 C108 -148(2) 3_765 . . 3_765 ? C103 Co1 C106 C108 -19.3(19) . . . 3_765 ? C103 Co1 C106 C108 71(2) 2_645 . . 3_765 ? C105 Co1 C106 C108 116.1(18) . . . 3_765 ? C105 Co1 C106 C108 159.4(8) 3_765 . . 3_765 ? C105 Co1 C106 C108 139(3) 2_645 . . 3_765 ? C102 Co1 C106 C109 -175.6(2) 3_765 . . 3_765 ? C102 Co1 C106 C109 51(3) 2_645 . . 3_765 ? C102 Co1 C106 C109 -28.2(7) . . . 3_765 ? C101 Co1 C106 C109 16.9(7) . . . 3_765 ? C101 Co1 C106 C109 158.3(12) 3_765 . . 3_765 ? C101 Co1 C106 C109 107(2) 2_645 . . 3_765 ? C103 Co1 C106 C109 157.65(13) 3_765 . . 3_765 ? C103 Co1 C106 C109 -73.3(6) . . . 3_765 ? C103 Co1 C106 C109 17.1(3) 2_645 . . 3_765 ? C105 Co1 C106 C109 62.0(7) . . . 3_765 ? C105 Co1 C106 C109 105.3(18) 3_765 . . 3_765 ? C105 Co1 C106 C109 85.4(19) 2_645 . . 3_765 ? C102 Co1 C106 C101 77(2) 3_765 . . 2_645 ? C102 Co1 C106 C101 -56(2) 2_645 . . 2_645 ? C102 Co1 C106 C101 -136(3) . . . 2_645 ? C101 Co1 C106 C101 -90(3) . . . 2_645 ? C101 Co1 C106 C101 51(3) 3_765 . . 2_645 ? C103 Co1 C106 C101 50.3(19) 3_765 . . 2_645 ? C103 Co1 C106 C101 -90.2(18) 2_645 . . 2_645 ? C105 Co1 C106 C101 -45(3) . . . 2_645 ? C105 Co1 C106 C101 -2(3) 3_765 . . 2_645 ? C105 Co1 C106 C101 -21.9(14) 2_645 . . 2_645 ? C102 C106 C107 C108 -50(4) 2_645 . . 3_765 ? C110 C106 C107 C108 -137(2) . . . 3_765 ? C101 C106 C107 C108 -107(4) 2_645 . . 3_765 ? Co1 C106 C107 C108 -78(2) . . . 3_765 ? C102 C106 C107 C108 87(3) 2_645 . . . ? C110 C106 C107 C108 0.1 . . . . ? C108 C106 C107 C108 137(2) 3_765 . . . ? C109 C106 C107 C108 119.6(4) 3_765 . . . ? C101 C106 C107 C108 30(2) 2_645 . . . ? Co1 C106 C107 C108 59.9 . . . . ? C110 C106 C107 C102 -87(2) . . . 2_645 ? C108 C106 C107 C102 50(4) 3_765 . . 2_645 ? C109 C106 C107 C102 33(2) 3_765 . . 2_645 ? C101 C106 C107 C102 -56.8(13) 2_645 . . 2_645 ? Co1 C106 C107 C102 -27(2) . . . 2_645 ? C102 C106 C107 Co1 27(3) 2_645 . . . ? C110 C106 C107 Co1 -59.7 . . . . ? C108 C106 C107 Co1 78(2) 3_765 . . . ? C109 C106 C107 Co1 59.7(4) 3_765 . . . ? C101 C106 C107 Co1 -30(2) 2_645 . . . ? C102 Co1 C107 C108 -171(3) 3_765 . . 3_765 ? C102 Co1 C107 C108 65(3) 2_645 . . 3_765 ? C102 Co1 C107 C108 -49(3) . . . 3_765 ? C101 Co1 C107 C108 -2(3) . . . 3_765 ? C101 Co1 C107 C108 -157.1(17) 3_765 . . 3_765 ? C101 Co1 C107 C108 99.7(16) 2_645 . . 3_765 ? C103 Co1 C107 C108 147(2) 3_765 . . 3_765 ? C103 Co1 C107 C108 -95(3) . . . 3_765 ? C103 Co1 C107 C108 27(2) 2_645 . . 3_765 ? C105 Co1 C107 C108 43(3) . . . 3_765 ? C105 Co1 C107 C108 136(2) 3_765 . . 3_765 ? C105 Co1 C107 C108 87.1(10) 2_645 . . 3_765 ? C102 Co1 C107 C108 -4.7(15) 3_765 . . . ? C102 Co1 C107 C108 -129.0(19) 2_645 . . . ? C102 Co1 C107 C108 117.4 . . . . ? C101 Co1 C107 C108 164.3 . . . . ? C101 Co1 C107 C108 9(2) 3_765 . . . ? C101 Co1 C107 C108 -94(2) 2_645 . . . ? C103 Co1 C107 C108 -46.9(16) 3_765 . . . ? C103 Co1 C107 C108 71.7 . . . . ? C103 Co1 C107 C108 -167.0(15) 2_645 . . . ? C105 Co1 C107 C108 -150.83(5) . . . . ? C105 Co1 C107 C108 -58(4) 3_765 . . . ? C105 Co1 C107 C108 -106(3) 2_645 . . . ? C102 Co1 C107 C106 113.7(16) 3_765 . . . ? C102 Co1 C107 C106 -11(2) 2_645 . . . ? C102 Co1 C107 C106 -124.25(6) . . . . ? C101 Co1 C107 C106 -77.32(6) . . . . ? C101 Co1 C107 C106 128(2) 3_765 . . . ? C101 Co1 C107 C106 25(2) 2_645 . . . ? C103 Co1 C107 C106 71.5(17) 3_765 . . . ? C103 Co1 C107 C106 -169.90(6) . . . . ? C103 Co1 C107 C106 -48.6(16) 2_645 . . . ? C105 Co1 C107 C106 -32.45(5) . . . . ? C105 Co1 C107 C106 61(4) 3_765 . . . ? C105 Co1 C107 C106 12(3) 2_645 . . . ? C102 Co1 C107 C102 124.3(5) 3_765 . . 2_645 ? C102 Co1 C107 C102 -113.6(19) . . . 2_645 ? C101 Co1 C107 C102 -66.7(19) . . . 2_645 ? C101 Co1 C107 C102 138.3(11) 3_765 . . 2_645 ? C101 Co1 C107 C102 35.1(11) 2_645 . . 2_645 ? C103 Co1 C107 C102 82.1(5) 3_765 . . 2_645 ? C103 Co1 C107 C102 -159.3(19) . . . 2_645 ? C103 Co1 C107 C102 -38.0(5) 2_645 . . 2_645 ? C105 Co1 C107 C102 -21.8(19) . . . 2_645 ? C106 C107 C108 C107 -136.9(12) . . . 2_645 ? C107 C107 C108 C107 -16.3(7) 3_765 . . 2_645 ? C102 C107 C108 C107 -116.9(16) 2_645 . . 2_645 ? Co1 C107 C108 C107 -75.4(12) . . . 2_645 ? C106 C107 C108 C109 -0.1 . . . . ? C107 C107 C108 C109 120.5(5) 3_765 . . . ? C107 C107 C108 C109 136.8(12) 2_645 . . . ? C102 C107 C108 C109 19.9(18) 2_645 . . . ? Co1 C107 C108 C109 61.4 . . . . ? C106 C107 C108 C103 -12.1(18) . . . 3_765 ? C106 C107 C108 Co1 -61.5 . . . . ? C107 C107 C108 Co1 59.1(5) 3_765 . . . ? C107 C107 C108 Co1 75.4(11) 2_645 . . . ? C102 C107 C108 Co1 -41.4(18) 2_645 . . . ? C105 Co1 C108 C107 -115.5(13) 3_765 . . 2_645 ? C105 Co1 C108 C107 -159.9(12) 2_645 . . 2_645 ? C102 Co1 C108 C107 174(2) 3_765 . . . ? C102 Co1 C108 C107 42.2(13) 2_645 . . . ? C102 Co1 C108 C107 -81.8 . . . . ? C101 Co1 C108 C107 -39.4 . . . . ? C101 Co1 C108 C107 -173.2(13) 3_765 . . . ? C101 Co1 C108 C107 85.9(15) 2_645 . . . ? C103 Co1 C108 C107 120(2) 3_765 . . . ? C103 Co1 C108 C107 -126.9 . . . . ? C103 Co1 C108 C107 15.5(16) 2_645 . . . ? C105 Co1 C108 C107 149.2 . . . . ? C105 Co1 C108 C107 152(2) 3_765 . . . ? C105 Co1 C108 C107 108(2) 2_645 . . . ? C102 Co1 C108 C109 56(2) 3_765 . . . ? C102 Co1 C108 C109 -75.5(13) 2_645 . . . ? C102 Co1 C108 C109 160.5 . . . . ? C101 Co1 C108 C109 -157.2 . . . . ? C101 Co1 C108 C109 69.1(14) 3_765 . . . ? C101 Co1 C108 C109 -31.8(15) 2_645 . . . ? C103 Co1 C108 C109 2(2) 3_765 . . . ? C103 Co1 C108 C109 115.4 . . . . ? C103 Co1 C108 C109 -102.2(16) 2_645 . . . ? C105 Co1 C108 C109 31.5 . . . . ? C105 Co1 C108 C109 34(2) 3_765 . . . ? C105 Co1 C108 C109 -10(2) 2_645 . . . ? C102 Co1 C108 C106 -27.7(9) 3_765 . . 2_645 ? C102 Co1 C108 C106 -159.5(9) 2_645 . . 2_645 ? C102 Co1 C108 C106 76.4(18) . . . 2_645 ? C101 Co1 C108 C106 118.8(18) . . . 2_645 ? C101 Co1 C108 C106 -14.9(10) 3_765 . . 2_645 ? C101 Co1 C108 C106 -115.9(9) 2_645 . . 2_645 ? C103 Co1 C108 C106 -81.7(7) 3_765 . . 2_645 ? C103 Co1 C108 C106 31.4(18) . . . 2_645 ? C103 Co1 C108 C106 173.8(6) 2_645 . . 2_645 ? C105 Co1 C108 C106 -52.5(18) . . . 2_645 ? C105 Co1 C108 C106 -50(2) 3_765 . . 2_645 ? C105 Co1 C108 C106 -94(2) 2_645 . . 2_645 ? C102 Co1 C108 C102 -131.8(7) 2_645 . . 3_765 ? C102 Co1 C108 C102 104(2) . . . 3_765 ? C101 Co1 C108 C102 147(2) . . . 3_765 ? C101 Co1 C108 C102 12.8(12) 3_765 . . 3_765 ? C101 Co1 C108 C102 -88.1(12) 2_645 . . 3_765 ? C103 Co1 C108 C102 -54.0(5) 3_765 . . 3_765 ? C103 Co1 C108 C102 59(2) . . . 3_765 ? C103 Co1 C108 C102 -158.5(5) 2_645 . . 3_765 ? C105 Co1 C108 C102 -25(2) . . . 3_765 ? C105 Co1 C108 C102 -22(3) 3_765 . . 3_765 ? C105 Co1 C108 C102 -66(3) 2_645 . . 3_765 ? C102 Co1 C108 C103 54.0(5) 3_765 . . 3_765 ? C102 Co1 C108 C103 -77.8(10) 2_645 . . 3_765 ? C102 Co1 C108 C103 158(2) . . . 3_765 ? C101 Co1 C108 C103 -159(2) . . . 3_765 ? C101 Co1 C108 C103 66.8(11) 3_765 . . 3_765 ? C101 Co1 C108 C103 -34.2(10) 2_645 . . 3_765 ? C103 Co1 C108 C103 113(2) . . . 3_765 ? C103 Co1 C108 C103 -104.6(6) 2_645 . . 3_765 ? C107 C108 C109 C102 -126.9(17) . . . 3_765 ? C106 C108 C109 C102 8.8(17) 2_645 . . 3_765 ? Co1 C108 C109 C102 -65.1(18) . . . 3_765 ? C107 C108 C109 C110 105(5) 2_645 . . . ? C107 C108 C109 C110 0.1 . . . . ? C106 C108 C109 C110 135.8(11) 2_645 . . . ? C102 C108 C109 C110 127.0(17) 3_765 . . . ? C103 C108 C109 C110 71(8) 3_765 . . . ? Co1 C108 C109 C110 61.8 . . . . ? C107 C108 C109 C106 -31(4) 2_645 . . 2_645 ? C107 C108 C109 C106 -135.7(11) . . . 2_645 ? C102 C108 C109 C106 -8.8(17) 3_765 . . 2_645 ? C103 C108 C109 C106 -65(9) 3_765 . . 2_645 ? Co1 C108 C109 C106 -73.9(11) . . . 2_645 ? C107 C108 C109 C101 -27.1(8) . . . 2_645 ? C106 C108 C109 C101 108.6(13) 2_645 . . 2_645 ? C102 C108 C109 C101 99.9(13) 3_765 . . 2_645 ? C103 C108 C109 C101 44(9) 3_765 . . 2_645 ? Co1 C108 C109 C101 34.7(8) . . . 2_645 ? C107 C108 C109 C104 47(7) 2_645 . . 3_765 ? C107 C108 C109 C104 -58(3) . . . 3_765 ? C106 C108 C109 C104 78(4) 2_645 . . 3_765 ? C102 C108 C109 C104 69(4) 3_765 . . 3_765 ? C103 C108 C109 C104 13(6) 3_765 . . 3_765 ? Co1 C108 C109 C104 4(3) . . . 3_765 ? C107 C108 C109 Co1 43(5) 2_645 . . . ? C107 C108 C109 Co1 -61.8 . . . . ? C106 C108 C109 Co1 73.9(11) 2_645 . . . ? C102 C108 C109 Co1 65.1(17) 3_765 . . . ? C103 C108 C109 Co1 9(8) 3_765 . . . ? C102 Co1 C109 C103 89(6) 3_765 . . 3_765 ? C102 Co1 C109 C103 -87(6) 2_645 . . 3_765 ? C102 Co1 C109 C103 127(7) . . . 3_765 ? C101 Co1 C109 C103 -29(7) . . . 3_765 ? C101 Co1 C109 C103 65(6) 3_765 . . 3_765 ? C101 Co1 C109 C103 -45(6) 2_645 . . 3_765 ? C103 Co1 C109 C103 91(6) . . . 3_765 ? C103 Co1 C109 C103 -83(6) 2_645 . . 3_765 ? C105 Co1 C109 C103 6(6) . . . 3_765 ? C105 Co1 C109 C103 22(6) 3_765 . . 3_765 ? C105 Co1 C109 C103 -15(6) 2_645 . . 3_765 ? C102 Co1 C109 C102 -176.1(2) 2_645 . . 3_765 ? C102 Co1 C109 C102 37.7(5) . . . 3_765 ? C101 Co1 C109 C102 -117.7(6) . . . 3_765 ? C101 Co1 C109 C102 -24.4(6) 3_765 . . 3_765 ? C101 Co1 C109 C102 -134.3(7) 2_645 . . 3_765 ? C103 Co1 C109 C102 -89(6) 3_765 . . 3_765 ? C103 Co1 C109 C102 2.3(5) . . . 3_765 ? C103 Co1 C109 C102 -171.6(5) 2_645 . . 3_765 ? C105 Co1 C109 C102 -82.7(6) . . . 3_765 ? C105 Co1 C109 C102 -66.9(19) 3_765 . . 3_765 ? C105 Co1 C109 C102 -103.6(16) 2_645 . . 3_765 ? C102 Co1 C109 C110 157.8(6) 3_765 . . . ? C102 Co1 C109 C110 -18.3(3) 2_645 . . . ? C102 Co1 C109 C110 -164.5 . . . . ? C101 Co1 C109 C110 40.1 . . . . ? C101 Co1 C109 C110 133.4(6) 3_765 . . . ? C101 Co1 C109 C110 23.5(10) 2_645 . . . ? C103 Co1 C109 C110 69(6) 3_765 . . . ? C103 Co1 C109 C110 160.1 . . . . ? C103 Co1 C109 C110 -13.77(13) 2_645 . . . ? C105 Co1 C109 C110 75.1 . . . . ? C105 Co1 C109 C110 91(2) 3_765 . . . ? C105 Co1 C109 C110 54.2(16) 2_645 . . . ? C102 Co1 C109 C108 -84.2(5) 3_765 . . . ? C102 Co1 C109 C108 99.7(3) 2_645 . . . ? C102 Co1 C109 C108 -46.4 . . . . ? C101 Co1 C109 C108 158.12(7) . . . . ? C101 Co1 C109 C108 -108.5(5) 3_765 . . . ? C101 Co1 C109 C108 141.6(10) 2_645 . . . ? C103 Co1 C109 C108 -173(6) 3_765 . . . ? C103 Co1 C109 C108 -81.8 . . . . ? C103 Co1 C109 C108 104.29(11) 2_645 . . . ? C105 Co1 C109 C108 -166.9 . . . . ? C105 Co1 C109 C108 -151(2) 3_765 . . . ? C105 Co1 C109 C108 172.3(16) 2_645 . . . ? C102 Co1 C109 C106 -26.7(12) 3_765 . . 2_645 ? C102 Co1 C109 C106 157.2(10) 2_645 . . 2_645 ? C102 Co1 C109 C106 11.0(7) . . . 2_645 ? C101 Co1 C109 C106 -144.4(6) . . . 2_645 ? C101 Co1 C109 C106 -51.1(8) 3_765 . . 2_645 ? C101 Co1 C109 C106 -161.0(13) 2_645 . . 2_645 ? C103 Co1 C109 C106 -116(7) 3_765 . . 2_645 ? C103 Co1 C109 C106 -24.4(7) . . . 2_645 ? C103 Co1 C109 C106 161.7(7) 2_645 . . 2_645 ? C105 Co1 C109 C106 -109.4(7) . . . 2_645 ? C105 Co1 C109 C106 -94(2) 3_765 . . 2_645 ? C105 Co1 C109 C106 -130.3(15) 2_645 . . 2_645 ? C102 Co1 C109 C101 134.3(7) 3_765 . . 2_645 ? C102 Co1 C109 C101 -41.8(8) 2_645 . . 2_645 ? C102 Co1 C109 C101 172.0(10) . . . 2_645 ? C101 Co1 C109 C101 16.6(10) . . . 2_645 ? C101 Co1 C109 C101 109.9(6) 3_765 . . 2_645 ? C103 Co1 C109 C101 45(6) 3_765 . . 2_645 ? C103 Co1 C109 C101 136.6(10) . . . 2_645 ? C103 Co1 C109 C101 -37.3(9) 2_645 . . 2_645 ? C105 Co1 C109 C101 51.6(9) . . . 2_645 ? C105 Co1 C109 C101 67.4(14) 3_765 . . 2_645 ? C105 Co1 C109 C101 30.7(10) 2_645 . . 2_645 ? C102 Co1 C109 C104 99(2) 3_765 . . 3_765 ? C102 Co1 C109 C104 -77(3) 2_645 . . 3_765 ? C102 Co1 C109 C104 137(3) . . . 3_765 ? C101 Co1 C109 C104 75(2) 3_765 . . 3_765 ? C101 Co1 C109 C104 -34.9(19) 2_645 . . 3_765 ? C103 Co1 C109 C104 10(4) 3_765 . . 3_765 ? C103 Co1 C109 C104 102(3) . . . 3_765 ? C103 Co1 C109 C104 -72(3) 2_645 . . 3_765 ? C105 Co1 C109 C104 32.5(14) 3_765 . . 3_765 ? C102 C109 C110 C106 85.9(17) 3_765 . . . ? C106 C109 C110 C106 54.4(9) 2_645 . . . ? C101 C109 C110 C106 109(4) 2_645 . . . ? C104 C109 C110 C106 124.2(14) 3_765 . . . ? Co1 C109 C110 C106 60.4 . . . . ? C103 C109 C110 C102 102(3) 3_765 . . 2_645 ? C102 C109 C110 C102 53.7(4) 3_765 . . 2_645 ? C108 C109 C110 C102 -32.2(13) . . . 2_645 ? C106 C109 C110 C102 22(2) 2_645 . . 2_645 ? C101 C109 C110 C102 77(5) 2_645 . . 2_645 ? C104 C109 C110 C102 92.0(14) 3_765 . . 2_645 ? Co1 C109 C110 C102 28.2(13) . . . 2_645 ? C103 C109 C110 C104 10(4) 3_765 . . 3_765 ? C102 C109 C110 C104 -38.3(17) 3_765 . . 3_765 ? C108 C109 C110 C104 -124.2(14) . . . 3_765 ? C106 C109 C110 C104 -69.7(17) 2_645 . . 3_765 ? C101 C109 C110 C104 -15(5) 2_645 . . 3_765 ? Co1 C109 C110 C104 -63.8(14) . . . 3_765 ? C103 C109 C110 Co1 74(5) 3_765 . . . ? C102 C109 C110 Co1 25.5(17) 3_765 . . . ? C108 C109 C110 Co1 -60.4 . . . . ? C106 C109 C110 Co1 -6.0(8) 2_645 . . . ? C101 C109 C110 Co1 49(4) 2_645 . . . ? C104 C109 C110 Co1 63.8(14) 3_765 . . . ? C102 C106 C110 C101 -7(3) 2_645 . . 2_645 ? C107 C106 C110 C101 116.4(14) . . . 2_645 ? C108 C106 C110 C101 72(2) 3_765 . . 2_645 ? C109 C106 C110 C101 14.4(17) 3_765 . . 2_645 ? Co1 C106 C110 C101 57.3(14) . . . 2_645 ? C102 C106 C110 C103 -102.3(16) 2_645 . . 3_765 ? C107 C106 C110 C103 21.2(16) . . . 3_765 ? C108 C106 C110 C103 -23(3) 3_765 . . 3_765 ? C109 C106 C110 C103 -80.8(12) 3_765 . . 3_765 ? C101 C106 C110 C103 -95(2) 2_645 . . 3_765 ? Co1 C106 C110 C103 -37.9(16) . . . 3_765 ? C102 C106 C110 C109 -124(3) 2_645 . . . ? C107 C106 C110 C109 -0.1 . . . . ? C109 C106 C110 C109 -102.1(6) 3_765 . . . ? C101 C106 C110 C109 -116.5(15) 2_645 . . . ? Co1 C106 C110 C109 -59.2 . . . . ? C107 C106 C110 C102 123(3) . . . 2_645 ? C108 C106 C110 C102 79(5) 3_765 . . 2_645 ? C109 C106 C110 C102 21(3) 3_765 . . 2_645 ? C101 C106 C110 C102 7(3) 2_645 . . 2_645 ? Co1 C106 C110 C102 64(3) . . . 2_645 ? C102 C106 C110 C104 -32(6) 2_645 . . 3_765 ? C107 C106 C110 C104 92(3) . . . 3_765 ? C108 C106 C110 C104 47(3) 3_765 . . 3_765 ? C109 C106 C110 C104 -10(4) 3_765 . . 3_765 ? C101 C106 C110 C104 -24(3) 2_645 . . 3_765 ? Co1 C106 C110 C104 33(3) . . . 3_765 ? C102 C106 C110 Co1 -64(3) 2_645 . . . ? C107 C106 C110 Co1 59.1 . . . . ? C108 C106 C110 Co1 15(2) 3_765 . . . ? C109 C106 C110 Co1 -42.9(5) 3_765 . . . ? C101 C106 C110 Co1 -57.3(14) 2_645 . . . ? C102 Co1 C110 C101 114(4) 3_765 . . 2_645 ? C102 Co1 C110 C101 -79(4) 2_645 . . 2_645 ? C102 Co1 C110 C101 -71(4) . . . 2_645 ? C101 Co1 C110 C101 -35(4) . . . 2_645 ? C101 Co1 C110 C101 80(5) 3_765 . . 2_645 ? C103 Co1 C110 C101 102(4) 3_765 . . 2_645 ? C103 Co1 C110 C101 86(4) . . . 2_645 ? C103 Co1 C110 C101 -63(4) 2_645 . . 2_645 ? C105 Co1 C110 C101 8(4) . . . 2_645 ? C105 Co1 C110 C101 41(4) 3_765 . . 2_645 ? C105 Co1 C110 C101 9(3) 2_645 . . 2_645 ? C102 Co1 C110 C103 12.06(10) 3_765 . . 3_765 ? C101 Co1 C110 C103 -136.81(7) . . . 3_765 ? C101 Co1 C110 C103 -21.6(8) 3_765 . . 3_765 ? C101 Co1 C110 C103 -102(4) 2_645 . . 3_765 ? C103 Co1 C110 C103 -15.82(8) . . . 3_765 ? C103 Co1 C110 C103 -165.1(2) 2_645 . . 3_765 ? C105 Co1 C110 C103 -93.96(6) . . . 3_765 ? C105 Co1 C110 C103 -60.7(15) 3_765 . . 3_765 ? C105 Co1 C110 C103 -92(2) 2_645 . . 3_765 ? C102 Co1 C110 C109 -14.62(7) 3_765 . . . ? C102 Co1 C110 C109 152.8(3) 2_645 . . . ? C102 Co1 C110 C109 160.3 . . . . ? C101 Co1 C110 C109 -163.5 . . . . ? C101 Co1 C110 C109 -48.3(8) 3_765 . . . ? C101 Co1 C110 C109 -128(4) 2_645 . . . ? C103 Co1 C110 C109 -26.67(7) 3_765 . . . ? C103 Co1 C110 C109 -42.5 . . . . ? C103 Co1 C110 C109 168.3(2) 2_645 . . . ? C105 Co1 C110 C109 -120.6 . . . . ? C105 Co1 C110 C109 -87.4(16) 3_765 . . . ? C105 Co1 C110 C109 -119(2) 2_645 . . . ? C102 Co1 C110 C106 -133.52(10) 3_765 . . . ? C102 Co1 C110 C106 33.9(3) 2_645 . . . ? C102 Co1 C110 C106 41.41(5) . . . . ? C101 Co1 C110 C106 77.6 . . . . ? C101 Co1 C110 C106 -167.2(8) 3_765 . . . ? C101 Co1 C110 C106 113(4) 2_645 . . . ? C103 Co1 C110 C106 -145.57(7) 3_765 . . . ? C103 Co1 C110 C106 -161.4 . . . . ? C103 Co1 C110 C106 49.4(2) 2_645 . . . ? C105 Co1 C110 C106 120.5 . . . . ? C105 Co1 C110 C106 153.7(16) 3_765 . . . ? C105 Co1 C110 C106 122(2) 2_645 . . . ? C102 Co1 C110 C102 -167.4(2) 3_765 . . 2_645 ? C102 Co1 C110 C102 7.5(3) . . . 2_645 ? C101 Co1 C110 C102 43.7(3) . . . 2_645 ? C101 Co1 C110 C102 158.9(5) 3_765 . . 2_645 ? C101 Co1 C110 C102 79(4) 2_645 . . 2_645 ? C103 Co1 C110 C102 164.7(2) . . . 2_645 ? C103 Co1 C110 C102 15.48(10) 2_645 . . 2_645 ? C105 Co1 C110 C102 86.6(3) . . . 2_645 ? C105 Co1 C110 C102 119.8(16) 3_765 . . 2_645 ? C105 Co1 C110 C102 88(2) 2_645 . . 2_645 ? C102 Co1 C110 C104 76(2) 3_765 . . 3_765 ? C102 Co1 C110 C104 -116(3) 2_645 . . 3_765 ? C102 Co1 C110 C104 -109(2) . . . 3_765 ? C101 Co1 C110 C104 -72(2) . . . 3_765 ? C101 Co1 C110 C104 43(3) 3_765 . . 3_765 ? C101 Co1 C110 C104 -37(3) 2_645 . . 3_765 ? C103 Co1 C110 C104 64(2) 3_765 . . 3_765 ? C103 Co1 C110 C104 49(2) . . . 3_765 ? C103 Co1 C110 C104 -101(3) 2_645 . . 3_765 ? C105 Co1 C110 C104 -30(2) . . . 3_765 ? C105 Co1 C110 C104 3.7(16) 3_765 . . 3_765 ? C105 Co1 C110 C104 -27.8(16) 2_645 . . 3_765 ? N3S C11S N3S C10S 32.5(5) 2_645 . . . ? N3S C11S N3S C10S -32.5(5) 3_765 . . . ? N3S C10S N3S C11S -32.5(5) 2_645 . . . ? N3S C10S N3S C11S 32.5(5) 3_765 . . . ? O10S O1S O9S O2S -109(4) . . . . ? O2S O9S O10S O1S 87(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 17.25 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.938 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.163 #===END data_Structure6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Cp*2Co) Ga4L6 complex' _chemical_melting_point 'not measured' _chemical_formula_moiety 'C204 H174 Co3 Ga4 K9 N12 O36' _chemical_formula_sum 'C204 H174 Co3 Ga4 K9 N12 O36' _chemical_formula_weight 4177.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' -0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' -0.0031 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' -0.0041 0.0074 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.1756 1.1428 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ga' 'Ga' 0.0992 1.8807 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.1807 0.2973 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'F d -3 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+3/4, z+1/2' '-x+3/4, y+1/2, -z+1/4' 'x+1/2, -y+1/4, -z+3/4' 'z, x, y' 'z+1/2, -x+1/4, -y+3/4' '-z+1/4, -x+3/4, y+1/2' '-z+3/4, x+1/2, -y+1/4' 'y, z, x' '-y+3/4, z+1/2, -x+1/4' 'y+1/2, -z+1/4, -x+3/4' '-y+1/4, -z+3/4, x+1/2' 'y+3/4, x+1/4, -z' '-y+1/2, -x+1/2, -z+1/2' 'y+1/4, -x, z+3/4' '-y, x+3/4, z+1/4' 'x+3/4, z+1/4, -y' '-x, z+3/4, y+1/4' '-x+1/2, -z+1/2, -y+1/2' 'x+1/4, -z, y+3/4' 'z+3/4, y+1/4, -x' 'z+1/4, -y, x+3/4' '-z, y+3/4, x+1/4' '-z+1/2, -y+1/2, -x+1/2' 'x, y+1/2, z+1/2' '-x+1/4, -y+5/4, z+1' '-x+3/4, y+1, -z+3/4' 'x+1/2, -y+3/4, -z+5/4' 'z, x+1/2, y+1/2' 'z+1/2, -x+3/4, -y+5/4' '-z+1/4, -x+5/4, y+1' '-z+3/4, x+1, -y+3/4' 'y, z+1/2, x+1/2' '-y+3/4, z+1, -x+3/4' 'y+1/2, -z+3/4, -x+5/4' '-y+1/4, -z+5/4, x+1' 'y+3/4, x+3/4, -z+1/2' '-y+1/2, -x+1, -z+1' 'y+1/4, -x+1/2, z+5/4' '-y, x+5/4, z+3/4' 'x+3/4, z+3/4, -y+1/2' '-x, z+5/4, y+3/4' '-x+1/2, -z+1, -y+1' 'x+1/4, -z+1/2, y+5/4' 'z+3/4, y+3/4, -x+1/2' 'z+1/4, -y+1/2, x+5/4' '-z, y+5/4, x+3/4' '-z+1/2, -y+1, -x+1' 'x+1/2, y, z+1/2' '-x+3/4, -y+3/4, z+1' '-x+5/4, y+1/2, -z+3/4' 'x+1, -y+1/4, -z+5/4' 'z+1/2, x, y+1/2' 'z+1, -x+1/4, -y+5/4' '-z+3/4, -x+3/4, y+1' '-z+5/4, x+1/2, -y+3/4' 'y+1/2, z, x+1/2' '-y+5/4, z+1/2, -x+3/4' 'y+1, -z+1/4, -x+5/4' '-y+3/4, -z+3/4, x+1' 'y+5/4, x+1/4, -z+1/2' '-y+1, -x+1/2, -z+1' 'y+3/4, -x, z+5/4' '-y+1/2, x+3/4, z+3/4' 'x+5/4, z+1/4, -y+1/2' '-x+1/2, z+3/4, y+3/4' '-x+1, -z+1/2, -y+1' 'x+3/4, -z, y+5/4' 'z+5/4, y+1/4, -x+1/2' 'z+3/4, -y, x+5/4' '-z+1/2, y+3/4, x+3/4' '-z+1, -y+1/2, -x+1' 'x+1/2, y+1/2, z' '-x+3/4, -y+5/4, z+1/2' '-x+5/4, y+1, -z+1/4' 'x+1, -y+3/4, -z+3/4' 'z+1/2, x+1/2, y' 'z+1, -x+3/4, -y+3/4' '-z+3/4, -x+5/4, y+1/2' '-z+5/4, x+1, -y+1/4' 'y+1/2, z+1/2, x' '-y+5/4, z+1, -x+1/4' 'y+1, -z+3/4, -x+3/4' '-y+3/4, -z+5/4, x+1/2' 'y+5/4, x+3/4, -z' '-y+1, -x+1, -z+1/2' 'y+3/4, -x+1/2, z+3/4' '-y+1/2, x+5/4, z+1/4' 'x+5/4, z+3/4, -y' '-x+1/2, z+5/4, y+1/4' '-x+1, -z+1, -y+1/2' 'x+3/4, -z+1/2, y+3/4' 'z+5/4, y+3/4, -x' 'z+3/4, -y+1/2, x+3/4' '-z+1/2, y+5/4, x+1/4' '-z+1, -y+1, -x+1/2' '-x, -y, -z' 'x-1/4, y-3/4, -z-1/2' 'x-3/4, -y-1/2, z-1/4' '-x-1/2, y-1/4, z-3/4' '-z, -x, -y' '-z-1/2, x-1/4, y-3/4' 'z-1/4, x-3/4, -y-1/2' 'z-3/4, -x-1/2, y-1/4' '-y, -z, -x' 'y-3/4, -z-1/2, x-1/4' '-y-1/2, z-1/4, x-3/4' 'y-1/4, z-3/4, -x-1/2' '-y-3/4, -x-1/4, z' 'y-1/2, x-1/2, z-1/2' '-y-1/4, x, -z-3/4' 'y, -x-3/4, -z-1/4' '-x-3/4, -z-1/4, y' 'x, -z-3/4, -y-1/4' 'x-1/2, z-1/2, y-1/2' '-x-1/4, z, -y-3/4' '-z-3/4, -y-1/4, x' '-z-1/4, y, -x-3/4' 'z, -y-3/4, -x-1/4' 'z-1/2, y-1/2, x-1/2' '-x, -y+1/2, -z+1/2' 'x-1/4, y-1/4, -z' 'x-3/4, -y, z+1/4' '-x-1/2, y+1/4, z-1/4' '-z, -x+1/2, -y+1/2' '-z-1/2, x+1/4, y-1/4' 'z-1/4, x-1/4, -y' 'z-3/4, -x, y+1/4' '-y, -z+1/2, -x+1/2' 'y-3/4, -z, x+1/4' '-y-1/2, z+1/4, x-1/4' 'y-1/4, z-1/4, -x' '-y-3/4, -x+1/4, z+1/2' 'y-1/2, x, z' '-y-1/4, x+1/2, -z-1/4' 'y, -x-1/4, -z+1/4' '-x-3/4, -z+1/4, y+1/2' 'x, -z-1/4, -y+1/4' 'x-1/2, z, y' '-x-1/4, z+1/2, -y-1/4' '-z-3/4, -y+1/4, x+1/2' '-z-1/4, y+1/2, -x-1/4' 'z, -y-1/4, -x+1/4' 'z-1/2, y, x' '-x+1/2, -y, -z+1/2' 'x+1/4, y-3/4, -z' 'x-1/4, -y-1/2, z+1/4' '-x, y-1/4, z-1/4' '-z+1/2, -x, -y+1/2' '-z, x-1/4, y-1/4' 'z+1/4, x-3/4, -y' 'z-1/4, -x-1/2, y+1/4' '-y+1/2, -z, -x+1/2' 'y-1/4, -z-1/2, x+1/4' '-y, z-1/4, x-1/4' 'y+1/4, z-3/4, -x' '-y-1/4, -x-1/4, z+1/2' 'y, x-1/2, z' '-y+1/4, x, -z-1/4' 'y+1/2, -x-3/4, -z+1/4' '-x-1/4, -z-1/4, y+1/2' 'x+1/2, -z-3/4, -y+1/4' 'x, z-1/2, y' '-x+1/4, z, -y-1/4' '-z-1/4, -y-1/4, x+1/2' '-z+1/4, y, -x-1/4' 'z+1/2, -y-3/4, -x+1/4' 'z, y-1/2, x' '-x+1/2, -y+1/2, -z' 'x+1/4, y-1/4, -z-1/2' 'x-1/4, -y, z-1/4' '-x, y+1/4, z-3/4' '-z+1/2, -x+1/2, -y' '-z, x+1/4, y-3/4' 'z+1/4, x-1/4, -y-1/2' 'z-1/4, -x, y-1/4' '-y+1/2, -z+1/2, -x' 'y-1/4, -z, x-1/4' '-y, z+1/4, x-3/4' 'y+1/4, z-1/4, -x-1/2' '-y-1/4, -x+1/4, z' 'y, x, z-1/2' '-y+1/4, x+1/2, -z-3/4' 'y+1/2, -x-1/4, -z-1/4' '-x-1/4, -z+1/4, y' 'x+1/2, -z-1/4, -y-1/4' 'x, z, y-1/2' '-x+1/4, z+1/2, -y-3/4' '-z-1/4, -y+1/4, x' '-z+1/4, y+1/2, -x-3/4' 'z+1/2, -y-1/4, -x-1/4' 'z, y, x-1/2' _cell_length_a 50.004(2) _cell_length_b 50.004(2) _cell_length_c 50.004(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 125030(9) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9206 _cell_measurement_theta_min 2.176 _cell_measurement_theta_max 22.518 _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.888 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 34336 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.7877 _exptl_absorpt_correction_T_max 0.7877 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Advanced Light Source Station 11.3.1' _diffrn_radiation_monochromator 'channel cut Si-<111> crystal' _diffrn_measurement_device_type 'Bruker Platinum 200' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean 3.623 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 73270 _diffrn_reflns_av_R_equivalents 0.1053 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 22.79 _reflns_number_total 2738 _reflns_number_gt 1091 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v. 2.0.2' _computing_cell_refinement 'SAINT v. 7.23' _computing_data_reduction 'SAINT v. 7.23' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 v.1.08, POV-Ray v3.6.1c.icl8.win32' _computing_publication_material 'ORTEP-3 v.1.08, POV-Ray v3.6.1c.icl8.win32' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The two data sets used in the refinement were combined in SAINT using a high angle cutoff(2(theta) = 30.68 deg., 1.45A) for the data collected with one second frames and both low and high angle cutoffs (2(theta) = 15.74 deg, 2.8A; 2(theta) = 32.10 deg, 1.40A) for the data collected with three second frames. Higher angle data collected using both five and ten second frames had anomalously high Rint values even when using aggressive low angle cutoffs for the data so were not included in the refinement. Five reflections were omitted from refinement because they had very large Fcalc^2 values but negative Fobs^2 values, and were assumed to have been blocked by the backstop during data collection. The Ga and Co atoms as well as the N and O atoms in the assembly were refined anisotropically. Hydrogen atoms were included at calculated positions on the ligand and the ordered NEt4+ on the exterior of the assembly and their positions were refined using the riding model. Hydrogen atoms were not included on any of the disordered solvent molecules in the asymmetric unit. Several restraints were used in the modeling of the aromatic rings: Anisotropic displacement parameters for the catechol and naphthalene rings were separately constrainted to be equivalent and the aromatic rings were restrained to have typical aromatic distances and geometries. One methanol solvent molecule was located near the periphery of the solvent channel and was modeled using typical MeOH bond lenghts. Other potential solvent peaks in the Fourier map could not be modeled satisfactorily as any solvent used, so the electron density in these solvent channels was calculated in Platon using the method of Spek to be 21,816 electrons. This is sufficient to account for the solvated potassium cations and disordered water and methanol in the solvent channels (up to 70 water molecules per assembly). The Cp*2Co+ molecules were both disordered based on the site symmetry of the cobalt in the crystal lattice. The encapsulated Cp*2Co+ molecule has 23. crystallographic site symmetry and was modeled as a rigid body using a known structure of Cp*2Co+ (CSD-DIMJIS01) with an occupancy of 1/12 to account for the site symmetry. The exterior Cp*2Co+ molecule is disordered with 3-bar symmetry and was similarly modeled using the know structure of Cp*2Co+. Hydrogen atoms were not included on the Cp*2Co+ molecules because of the high level of disorder. Thermal displacement parameters on the carbon atoms in these molecules were also constrained to be identical. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 2738 _refine_ls_number_parameters 177 _refine_ls_number_restraints 145 _refine_ls_R_factor_all 0.2242 _refine_ls_R_factor_gt 0.1469 _refine_ls_wR_factor_ref 0.4067 _refine_ls_wR_factor_gt 0.3666 _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_restrained_S_all 1.181 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga01 Ga 0.46404(3) 0.46404(3) 0.28596(3) 0.1904(15) Uani 1 3 d SD . . Co1 Co 0.3750 0.3750 0.3750 0.187(2) Uani 1 12 d SG . . C1 C 0.3967(5) 0.3900(8) 0.3433(4) 0.161(9) Uiso 0.08 1 d PG A -1 C2 C 0.3703(6) 0.4012(5) 0.3436(5) 0.161(9) Uiso 0.08 1 d PG A -1 C3 C 0.3518(4) 0.3797(5) 0.3411(2) 0.161(9) Uiso 0.08 1 d PG A -1 C4 C 0.3664(5) 0.3553(6) 0.3395(4) 0.161(9) Uiso 0.08 1 d PG A -1 C5 C 0.3943(4) 0.3617(8) 0.3408(3) 0.161(9) Uiso 0.08 1 d PG A -1 C6 C 0.4222(7) 0.4057(12) 0.3431(8) 0.161(9) Uiso 0.08 1 d PG A -1 C7 C 0.3635(11) 0.4303(5) 0.3458(10) 0.161(9) Uiso 0.08 1 d PG A -1 C8 C 0.3219(4) 0.3824(9) 0.3390(6) 0.161(9) Uiso 0.08 1 d PG A -1 C9 C 0.3548(9) 0.3279(6) 0.3365(9) 0.161(9) Uiso 0.08 1 d PG A -1 C10 C 0.4169(6) 0.3425(12) 0.3382(7) 0.161(9) Uiso 0.08 1 d PG A -1 C11 C 0.3829(5) 0.3942(6) 0.4096(4) 0.161(9) Uiso 0.08 1 d PG B -1 C12 C 0.3551(4) 0.3877(8) 0.4083(3) 0.161(9) Uiso 0.08 1 d PG B -1 C13 C 0.3526(5) 0.3594(8) 0.4058(4) 0.161(9) Uiso 0.08 1 d PG B -1 C14 C 0.3790(6) 0.3482(5) 0.4055(5) 0.161(9) Uiso 0.08 1 d PG B -1 C15 C 0.3976(4) 0.3697(5) 0.4080(2) 0.161(9) Uiso 0.08 1 d PG B -1 C16 C 0.3946(9) 0.4216(6) 0.4125(9) 0.161(9) Uiso 0.08 1 d PG B -1 C17 C 0.3324(6) 0.4069(12) 0.4109(7) 0.161(9) Uiso 0.08 1 d PG B -1 C18 C 0.3271(7) 0.3441(12) 0.4052(8) 0.161(9) Uiso 0.08 1 d PG B -1 C19 C 0.3858(11) 0.3192(4) 0.4033(10) 0.161(9) Uiso 0.08 1 d PG B -1 C20 C 0.4269(4) 0.3674(8) 0.4102(5) 0.161(9) Uiso 0.08 1 d PG B -1 Co2 Co 0.2500 0.5000 0.2500 0.195(2) Uani 1 6 d SG . . C21 C 0.2366(3) 0.5210(3) 0.2828(2) 0.330(11) Uiso 0.17 1 d PG C -1 C22 C 0.2267(3) 0.4941(4) 0.2831(2) 0.330(11) Uiso 0.17 1 d PG C -1 C23 C 0.21143(10) 0.4902(3) 0.2593(3) 0.330(11) Uiso 0.17 1 d PG C -1 C24 C 0.21212(12) 0.5143(3) 0.2441(3) 0.330(11) Uiso 0.17 1 d PG C -1 C25 C 0.2276(3) 0.5334(2) 0.2587(4) 0.330(11) Uiso 0.17 1 d PG C -1 C26 C 0.2521(6) 0.5343(5) 0.3044(3) 0.330(11) Uiso 0.17 1 d PG C -1 C27 C 0.2311(5) 0.4740(6) 0.3048(3) 0.330(11) Uiso 0.17 1 d PG C -1 C28 C 0.1962(3) 0.4653(4) 0.2522(5) 0.330(11) Uiso 0.17 1 d PG C -1 C29 C 0.1986(3) 0.5189(5) 0.2177(5) 0.330(11) Uiso 0.17 1 d PG C -1 C30 C 0.2322(5) 0.56182(14) 0.2510(6) 0.330(11) Uiso 0.17 1 d PG C -1 C31 C 0.28791(12) 0.4857(3) 0.2560(3) 0.330(11) Uiso 0.17 1 d PG C -1 C32 C 0.2724(3) 0.4666(2) 0.2413(4) 0.330(11) Uiso 0.17 1 d PG C -1 C33 C 0.2634(3) 0.4790(3) 0.2172(2) 0.330(11) Uiso 0.17 1 d PG C -1 C34 C 0.2733(3) 0.5059(4) 0.2169(2) 0.330(11) Uiso 0.17 1 d PG C -1 C35 C 0.28858(10) 0.5098(3) 0.2407(3) 0.330(11) Uiso 0.17 1 d PG C -1 C36 C 0.3014(3) 0.4811(5) 0.2823(5) 0.330(11) Uiso 0.17 1 d PG C -1 C37 C 0.2678(5) 0.43818(14) 0.2490(6) 0.330(11) Uiso 0.17 1 d PG C -1 C38 C 0.2479(6) 0.4658(5) 0.1956(3) 0.330(11) Uiso 0.17 1 d PG C -1 C39 C 0.2689(5) 0.5260(6) 0.1952(3) 0.330(11) Uiso 0.17 1 d PG C -1 C40 C 0.3038(3) 0.5347(4) 0.2478(5) 0.330(11) Uiso 0.17 1 d PG C -1 O001 O 0.42601(15) 0.45900(15) 0.27921(15) 0.188(3) Uani 1 1 d D . . O002 O 0.4571(2) 0.50115(14) 0.27676(18) 0.213(3) Uani 1 1 d D . . O003 O 0.3483(3) 0.46266(16) 0.2458(2) 0.247(4) Uani 1 1 d . . . N001 N 0.3795(2) 0.4351(2) 0.26489(19) 0.198(4) Uani 1 1 d . . . H001 H 0.3951 0.4348 0.2731 0.237 Uiso 1 1 calc R . . C001 C 0.4143(3) 0.4820(3) 0.2687(2) 0.191(4) Uani 1 1 d DU . . C002 C 0.4307(3) 0.5042(3) 0.2681(2) 0.201(4) Uani 1 1 d DU . . C003 C 0.4199(3) 0.5282(3) 0.2594(2) 0.224(5) Uani 1 1 d DU . . H003 H 0.4308 0.5438 0.2591 0.269 Uiso 1 1 calc R . . C004 C 0.3934(3) 0.5300(3) 0.2510(3) 0.235(5) Uani 1 1 d DU . . H004 H 0.3859 0.5466 0.2456 0.282 Uiso 1 1 calc R . . C005 C 0.3784(3) 0.5071(3) 0.2510(3) 0.219(5) Uani 1 1 d DU . . H005 H 0.3606 0.5077 0.2444 0.263 Uiso 1 1 calc R . . C006 C 0.3883(3) 0.4832(3) 0.2602(3) 0.192(4) Uani 1 1 d DU . . C007 C 0.3726(4) 0.4590(4) 0.2561(3) 0.203(6) Uani 1 1 d . . . C008 C 0.3815(3) 0.3869(2) 0.2636(3) 0.197(5) Uani 1 1 d DU . . C009 C 0.3674(3) 0.4110(3) 0.2639(2) 0.218(5) Uani 1 1 d DU . . C010 C 0.3400(3) 0.4103(2) 0.2635(3) 0.227(5) Uani 1 1 d DU . . H010 H 0.3299 0.4264 0.2639 0.272 Uiso 1 1 calc R . . C011 C 0.3273(3) 0.3856(3) 0.2623(3) 0.227(5) Uani 1 1 d DU . . H011 H 0.3084 0.3849 0.2613 0.273 Uiso 1 1 calc R . . C012 C 0.3415(3) 0.3622(3) 0.2625(3) 0.223(5) Uani 1 1 d DU . . H012 H 0.3325 0.3455 0.2620 0.268 Uiso 1 1 calc R . . K1 K 0.5000 0.53279(8) 0.28279(8) 0.084(2) Uani 0.33 2 d SP . . O1S O 0.4521(8) 0.5719(8) 0.3145(8) 0.260(15) Uiso 0.25 1 d PD . . C1S C 0.4362(13) 0.5527(12) 0.3278(14) 0.30(3) Uiso 0.25 1 d PD . . O2S O 0.5000 0.5000 0.2500 0.347(17) Uiso 1 6 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga01 0.1904(15) 0.1904(15) 0.1904(15) 0.0335(8) 0.0335(8) -0.0335(8) Co1 0.187(2) 0.187(2) 0.187(2) 0.000 0.000 0.000 Co2 0.195(2) 0.195(2) 0.195(2) 0.0278(14) -0.0278(14) 0.0278(14) O001 0.208(7) 0.168(6) 0.188(7) 0.033(5) 0.055(5) -0.034(5) O002 0.239(9) 0.156(7) 0.244(8) 0.021(5) 0.053(6) -0.089(6) O003 0.344(13) 0.149(7) 0.248(10) 0.050(6) 0.010(9) -0.011(7) N001 0.215(10) 0.142(8) 0.237(10) 0.044(7) -0.037(7) 0.025(8) C001 0.212(10) 0.170(8) 0.190(9) 0.045(8) 0.013(8) -0.038(8) C002 0.225(10) 0.169(10) 0.210(9) 0.048(8) 0.021(9) -0.045(8) C003 0.233(10) 0.181(8) 0.259(11) 0.057(8) 0.026(9) -0.026(9) C004 0.234(11) 0.188(9) 0.283(11) 0.062(9) 0.026(10) -0.025(8) C005 0.216(10) 0.189(10) 0.252(10) 0.069(9) 0.028(8) -0.022(7) C006 0.194(10) 0.167(8) 0.213(10) 0.036(8) 0.033(8) -0.028(9) C007 0.237(17) 0.212(18) 0.160(11) 0.001(10) -0.050(10) 0.049(14) C008 0.155(10) 0.142(10) 0.294(13) 0.028(8) -0.016(9) -0.027(7) C009 0.189(9) 0.142(9) 0.322(12) 0.031(10) -0.003(10) -0.032(8) C010 0.180(9) 0.159(8) 0.343(13) 0.038(9) 0.021(10) 0.000(7) C011 0.179(9) 0.160(9) 0.343(12) 0.009(11) -0.004(9) -0.007(7) C012 0.178(11) 0.154(9) 0.337(14) 0.004(11) 0.003(11) -0.015(8) K1 0.095(4) 0.079(3) 0.079(3) 0.022(3) 0.030(2) -0.030(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga01 O002 1.943(8) 83_455 ? Ga01 O002 1.943(8) 32_545 ? Ga01 O002 1.943(8) . ? Ga01 O001 1.948(7) . ? Ga01 O001 1.948(7) 32_545 ? Ga01 O001 1.948(7) 83_455 ? Ga01 K1 3.883(4) 83_455 ? Ga01 K1 3.883(4) . ? Ga01 K1 3.883(4) 32_545 ? Co1 C11 2.017(17) 5 ? Co1 C11 2.02(2) 78_455 ? Co1 C11 2.02(3) 9 ? Co1 C11 2.02(2) 83_455 ? Co1 C11 2.017(9) 76_455 ? Co1 C11 2.0171 . ? Co1 C11 2.02(3) 60_554 ? Co1 C11 2.02(3) 34_545 ? Co1 C11 2.02(3) 27_545 ? Co1 C11 2.02(3) 50_554 ? Co1 C11 2.017(17) 32_545 ? Co1 C11 2.02(3) 55_554 ? C1 C5 1.4278 . ? C1 C2 1.4301 . ? C1 C6 1.4969 . ? C2 C3 1.4271 . ? C2 C7 1.4969 . ? C3 C4 1.4265 . ? C3 C8 1.5003 . ? C4 C5 1.4298 . ? C4 C9 1.4968 . ? C5 C10 1.4895 . ? C11 C15 1.4280 . ? C11 C12 1.4303 . ? C11 C16 1.4970 . ? C12 C13 1.4285 . ? C12 C17 1.4899 . ? C13 C14 1.4317 . ? C13 C18 1.4880 . ? C14 C15 1.4267 . ? C14 C19 1.4966 . ? C15 C20 1.4731 . ? Co2 C23 2.044(17) 78_455 ? Co2 C23 2.0439 145_565 ? Co2 C23 2.044(17) 126_655 ? Co2 C23 2.044(16) 108_566 ? Co2 C23 2.0439 . ? Co2 C23 2.044(16) 60_554 ? Co2 C35 2.045(17) 126_655 ? Co2 C35 2.045(16) 108_566 ? Co2 C35 2.045(17) 78_455 ? Co2 C35 2.045(16) 60_554 ? Co2 C35 2.0445 . ? Co2 C35 2.0445 145_565 ? C21 C25 1.4278 . ? C21 C22 1.4308 . ? C21 C26 1.4893 . ? C22 C23 1.4278 . ? C22 C27 1.4959 . ? C23 C24 1.4271 . ? C23 C28 1.4992 . ? C24 C25 1.4302 . ? C24 C29 1.4965 . ? C25 C30 1.4892 . ? C31 C35 1.4273 . ? C31 C32 1.4310 . ? C31 C36 1.4959 . ? C32 C33 1.4277 . ? C32 C37 1.4897 . ? C33 C34 1.4311 . ? C33 C38 1.4883 . ? C34 C35 1.4273 . ? C34 C39 1.4962 . ? C35 C40 1.4990 . ? O001 C001 1.395(14) . ? O002 C002 1.400(14) . ? O002 K1 2.682(9) . ? O002 K1 3.021(9) 32_545 ? O003 C007 1.333(13) . ? N001 C007 1.320(16) . ? N001 C009 1.349(13) . ? N001 H001 0.8800 . ? C001 C006 1.369(10) . ? C001 C002 1.377(10) . ? C002 C003 1.387(10) . ? C002 K1 3.140(12) 32_545 ? C003 C004 1.391(9) . ? C003 K1 3.470(12) 32_545 ? C003 H003 0.9500 . ? C004 C005 1.370(10) . ? C004 H004 0.9500 . ? C005 C006 1.371(10) . ? C005 H005 0.9500 . ? C006 C007 1.457(18) . ? C008 C012 1.351(14) 50_554 ? C008 C008 1.36(2) 50_554 ? C008 C009 1.393(10) . ? C009 C010 1.373(9) . ? C010 C011 1.390(9) . ? C010 H010 0.9500 . ? C011 C012 1.369(9) . ? C011 H011 0.9500 . ? C012 C008 1.351(14) 50_554 ? C012 H012 0.9500 . ? K1 O2S 2.319(6) . ? K1 O002 2.682(9) 42_644 ? K1 O002 3.021(9) 83_455 ? K1 O002 3.021(9) 86 ? K1 C002 3.140(12) 83_455 ? K1 C002 3.140(12) 86 ? K1 C003 3.470(12) 83_455 ? K1 C003 3.470(12) 86 ? K1 Ga01 3.883(4) 86 ? K1 K1 4.016(10) 83_455 ? O1S C1S 1.412(10) . ? O2S K1 2.319(6) 83_455 ? O2S K1 2.319(6) 32_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O002 Ga01 O002 89.2(4) 83_455 32_545 ? O002 Ga01 O002 89.2(4) 83_455 . ? O002 Ga01 O002 89.2(4) 32_545 . ? O002 Ga01 O001 173.7(3) 83_455 . ? O002 Ga01 O001 92.5(3) 32_545 . ? O002 Ga01 O001 84.8(4) . . ? O002 Ga01 O001 92.5(3) 83_455 32_545 ? O002 Ga01 O001 84.8(4) 32_545 32_545 ? O002 Ga01 O001 173.7(3) . 32_545 ? O001 Ga01 O001 93.7(3) . 32_545 ? O002 Ga01 O001 84.8(4) 83_455 83_455 ? O002 Ga01 O001 173.7(3) 32_545 83_455 ? O002 Ga01 O001 92.5(3) . 83_455 ? O001 Ga01 O001 93.7(3) . 83_455 ? O001 Ga01 O001 93.7(3) 32_545 83_455 ? O002 Ga01 K1 39.4(3) 83_455 83_455 ? O002 Ga01 K1 49.9(2) 32_545 83_455 ? O002 Ga01 K1 90.5(3) . 83_455 ? O001 Ga01 K1 142.1(2) . 83_455 ? O001 Ga01 K1 86.9(2) 32_545 83_455 ? O001 Ga01 K1 124.0(2) 83_455 83_455 ? O002 Ga01 K1 49.9(2) 83_455 . ? O002 Ga01 K1 90.5(3) 32_545 . ? O002 Ga01 K1 39.4(3) . . ? O001 Ga01 K1 124.0(2) . . ? O001 Ga01 K1 142.1(2) 32_545 . ? O001 Ga01 K1 86.9(2) 83_455 . ? K1 Ga01 K1 62.28(11) 83_455 . ? O002 Ga01 K1 90.5(3) 83_455 32_545 ? O002 Ga01 K1 39.4(3) 32_545 32_545 ? O002 Ga01 K1 49.9(2) . 32_545 ? O001 Ga01 K1 86.9(2) . 32_545 ? O001 Ga01 K1 124.0(2) 32_545 32_545 ? O001 Ga01 K1 142.1(2) 83_455 32_545 ? K1 Ga01 K1 62.28(11) 83_455 32_545 ? K1 Ga01 K1 62.28(11) . 32_545 ? C11 Co1 C11 61.9(16) 5 78_455 ? C11 Co1 C11 48.0(10) 5 9 ? C11 Co1 C11 81.6(6) 78_455 9 ? C11 Co1 C11 81.6(7) 5 83_455 ? C11 Co1 C11 48.0(12) 78_455 83_455 ? C11 Co1 C11 123.3(9) 9 83_455 ? C11 Co1 C11 109.4(11) 5 76_455 ? C11 Co1 C11 48.0(14) 78_455 76_455 ? C11 Co1 C11 118.9(10) 9 76_455 ? C11 Co1 C11 48.0(19) 83_455 76_455 ? C11 Co1 C11 48.0(11) 5 . ? C11 Co1 C11 109.4(16) 78_455 . ? C11 Co1 C11 48.0(18) 9 . ? C11 Co1 C11 118.9(9) 83_455 . ? C11 Co1 C11 157.39(6) 76_455 . ? C11 Co1 C11 118.9(14) 5 60_554 ? C11 Co1 C11 109.4(2) 78_455 60_554 ? C11 Co1 C11 157.4(2) 9 60_554 ? C11 Co1 C11 61.9(13) 83_455 60_554 ? C11 Co1 C11 81.6(7) 76_455 60_554 ? C11 Co1 C11 109.4(18) . 60_554 ? C11 Co1 C11 109.4(9) 5 34_545 ? C11 Co1 C11 118.9(4) 78_455 34_545 ? C11 Co1 C11 61.9(13) 9 34_545 ? C11 Co1 C11 157.4(2) 83_455 34_545 ? C11 Co1 C11 109(2) 76_455 34_545 ? C11 Co1 C11 81.6(12) . 34_545 ? C11 Co1 C11 123.3(9) 60_554 34_545 ? C11 Co1 C11 118.9(7) 5 27_545 ? C11 Co1 C11 81.6(16) 78_455 27_545 ? C11 Co1 C11 81.6(14) 9 27_545 ? C11 Co1 C11 109.4(12) 83_455 27_545 ? C11 Co1 C11 61.9(15) 76_455 27_545 ? C11 Co1 C11 123.3(4) . 27_545 ? C11 Co1 C11 118.9(16) 60_554 27_545 ? C11 Co1 C11 48.0(12) 34_545 27_545 ? C11 Co1 C11 81.6(5) 5 50_554 ? C11 Co1 C11 118.9(18) 78_455 50_554 ? C11 Co1 C11 109.4(9) 9 50_554 ? C11 Co1 C11 82(2) 83_455 50_554 ? C11 Co1 C11 123.3(4) 76_455 50_554 ? C11 Co1 C11 61.9(15) . 50_554 ? C11 Co1 C11 48.0(10) 60_554 50_554 ? C11 Co1 C11 118.9(14) 34_545 50_554 ? C11 Co1 C11 157.39(5) 27_545 50_554 ? C11 Co1 C11 157.4(4) 5 32_545 ? C11 Co1 C11 123.3(9) 78_455 32_545 ? C11 Co1 C11 109.4(9) 9 32_545 ? C11 Co1 C11 118.86(18) 83_455 32_545 ? C11 Co1 C11 81.6(12) 76_455 32_545 ? C11 Co1 C11 118.9(9) . 32_545 ? C11 Co1 C11 81.6(4) 60_554 32_545 ? C11 Co1 C11 48.0(12) 34_545 32_545 ? C11 Co1 C11 48.0(16) 27_545 32_545 ? C11 Co1 C11 109.4(16) 50_554 32_545 ? C11 Co1 C11 123.3(9) 5 55_554 ? C11 Co1 C11 157.4(4) 78_455 55_554 ? C11 Co1 C11 118.9(15) 9 55_554 ? C11 Co1 C11 109.4(9) 83_455 55_554 ? C11 Co1 C11 118.9(13) 76_455 55_554 ? C11 Co1 C11 81.6(10) . 55_554 ? C11 Co1 C11 48.0(7) 60_554 55_554 ? C11 Co1 C11 81.59(12) 34_545 55_554 ? C11 Co1 C11 109.4(4) 27_545 55_554 ? C11 Co1 C11 48.0(4) 50_554 55_554 ? C11 Co1 C11 61.9(16) 32_545 55_554 ? C5 C1 C2 108.0 . . ? C5 C1 C6 126.1 . . ? C2 C1 C6 125.6 . . ? C5 C1 Co1 70.2 . . ? C2 C1 Co1 69.5 . . ? C6 C1 Co1 130.1 . . ? C3 C2 C1 107.8 . . ? C3 C2 C7 126.2 . . ? C1 C2 C7 126.1 . . ? C3 C2 Co1 70.3 . . ? C1 C2 Co1 69.9 . . ? C7 C2 Co1 126.1 . . ? C4 C3 C2 108.4 . . ? C4 C3 C8 125.8 . . ? C2 C3 C8 125.8 . . ? C4 C3 Co1 70.1 . . ? C2 C3 Co1 69.3 . . ? C8 C3 Co1 128.6 . . ? C3 C4 C5 107.8 . . ? C3 C4 C9 126.1 . . ? C5 C4 C9 126.1 . . ? C3 C4 Co1 69.7 . . ? C5 C4 Co1 69.7 . . ? C9 C4 Co1 126.9 . . ? C1 C5 C4 108.0 . . ? C1 C5 C10 125.7 . . ? C4 C5 C10 126.2 . . ? C1 C5 Co1 69.4 . . ? C4 C5 Co1 70.0 . . ? C10 C5 Co1 129.1 . . ? C15 C11 C12 107.8 . . ? C15 C11 C16 126.1 . . ? C12 C11 C16 126.1 . . ? C15 C11 Co1 69.3 . . ? C12 C11 Co1 70.4 . . ? C16 C11 Co1 126.6 . . ? C13 C12 C11 108.1 . . ? C13 C12 C17 125.7 . . ? C11 C12 C17 126.2 . . ? C13 C12 Co1 70.1 . . ? C11 C12 Co1 68.4 . . ? C17 C12 Co1 129.9 . . ? C12 C13 C14 108.0 . . ? C12 C13 C18 125.7 . . ? C14 C13 C18 126.2 . . ? C12 C13 Co1 69.1 . . ? C14 C13 Co1 68.9 . . ? C18 C13 Co1 130.4 . . ? C15 C14 C13 107.8 . . ? C15 C14 C19 126.1 . . ? C13 C14 C19 126.1 . . ? C15 C14 Co1 68.7 . . ? C13 C14 Co1 70.2 . . ? C19 C14 Co1 127.3 . . ? C14 C15 C11 108.4 . . ? C14 C15 C20 126.5 . . ? C11 C15 C20 125.0 . . ? C14 C15 Co1 70.1 . . ? C11 C15 Co1 69.2 . . ? C20 C15 Co1 128.8 . . ? C23 Co2 C23 67.2(5) 78_455 145_565 ? C23 Co2 C23 180.0(10) 78_455 126_655 ? C23 Co2 C23 112.8(8) 145_565 126_655 ? C23 Co2 C23 67.2(4) 78_455 108_566 ? C23 Co2 C23 112.8(8) 145_565 108_566 ? C23 Co2 C23 112.76(14) 126_655 108_566 ? C23 Co2 C23 112.8(8) 78_455 . ? C23 Co2 C23 180.0 145_565 . ? C23 Co2 C23 67.2(5) 126_655 . ? C23 Co2 C23 67.2(5) 108_566 . ? C23 Co2 C23 112.76(14) 78_455 60_554 ? C23 Co2 C23 67.2(5) 145_565 60_554 ? C23 Co2 C23 67.2(4) 126_655 60_554 ? C23 Co2 C23 180.0(11) 108_566 60_554 ? C23 Co2 C23 112.8(8) . 60_554 ? C23 Co2 C35 0.0(10) 78_455 126_655 ? C23 Co2 C35 67.2(8) 145_565 126_655 ? C23 Co2 C35 180.0 126_655 126_655 ? C23 Co2 C35 67.23(14) 108_566 126_655 ? C23 Co2 C35 112.8(5) . 126_655 ? C23 Co2 C35 112.8(4) 60_554 126_655 ? C23 Co2 C35 112.8(4) 78_455 108_566 ? C23 Co2 C35 67.2(8) 145_565 108_566 ? C23 Co2 C35 67.25(14) 126_655 108_566 ? C23 Co2 C35 180.0 108_566 108_566 ? C23 Co2 C35 112.8(5) . 108_566 ? C23 Co2 C35 0.0(8) 60_554 108_566 ? C35 Co2 C35 112.77(14) 126_655 108_566 ? C23 Co2 C35 180.0 78_455 78_455 ? C23 Co2 C35 112.8(5) 145_565 78_455 ? C23 Co2 C35 0.0(10) 126_655 78_455 ? C23 Co2 C35 112.8(4) 108_566 78_455 ? C23 Co2 C35 67.2(8) . 78_455 ? C23 Co2 C35 67.23(14) 60_554 78_455 ? C35 Co2 C35 180.0(10) 126_655 78_455 ? C35 Co2 C35 67.2(4) 108_566 78_455 ? C23 Co2 C35 67.25(14) 78_455 60_554 ? C23 Co2 C35 112.8(5) 145_565 60_554 ? C23 Co2 C35 112.8(4) 126_655 60_554 ? C23 Co2 C35 0.0(8) 108_566 60_554 ? C23 Co2 C35 67.2(8) . 60_554 ? C23 Co2 C35 180.0 60_554 60_554 ? C35 Co2 C35 67.2(4) 126_655 60_554 ? C35 Co2 C35 180.0(9) 108_566 60_554 ? C35 Co2 C35 112.77(14) 78_455 60_554 ? C23 Co2 C35 67.2(8) 78_455 . ? C23 Co2 C35 0.0(14) 145_565 . ? C23 Co2 C35 112.8(5) 126_655 . ? C23 Co2 C35 112.8(5) 108_566 . ? C23 Co2 C35 180.0 . . ? C23 Co2 C35 67.2(8) 60_554 . ? C35 Co2 C35 67.2(5) 126_655 . ? C35 Co2 C35 67.2(5) 108_566 . ? C35 Co2 C35 112.8(8) 78_455 . ? C35 Co2 C35 112.8(8) 60_554 . ? C23 Co2 C35 112.8(5) 78_455 145_565 ? C23 Co2 C35 180.0 145_565 145_565 ? C23 Co2 C35 67.2(8) 126_655 145_565 ? C23 Co2 C35 67.2(8) 108_566 145_565 ? C23 Co2 C35 0.0(14) . 145_565 ? C23 Co2 C35 112.8(5) 60_554 145_565 ? C35 Co2 C35 112.8(8) 126_655 145_565 ? C35 Co2 C35 112.8(8) 108_566 145_565 ? C35 Co2 C35 67.2(5) 78_455 145_565 ? C35 Co2 C35 67.2(5) 60_554 145_565 ? C35 Co2 C35 180.0 . 145_565 ? C25 C21 C22 108.1 . . ? C25 C21 C26 125.7 . . ? C22 C21 C26 126.1 . . ? C25 C21 Co2 69.7 . . ? C22 C21 Co2 69.2 . . ? C26 C21 Co2 129.5 . . ? C23 C22 C21 107.7 . . ? C23 C22 C27 126.1 . . ? C21 C22 C27 126.1 . . ? C23 C22 Co2 69.4 . . ? C21 C22 Co2 70.0 . . ? C27 C22 Co2 126.7 . . ? C24 C23 C22 108.4 . . ? C24 C23 C28 125.8 . . ? C22 C23 C28 125.7 . . ? C24 C23 Co2 69.7 . . ? C22 C23 Co2 69.7 . . ? C28 C23 Co2 128.6 . . ? C23 C24 C25 107.8 . . ? C23 C24 C29 126.1 . . ? C25 C24 C29 126.1 . . ? C23 C24 Co2 69.5 . . ? C25 C24 Co2 70.1 . . ? C29 C24 Co2 126.8 . . ? C21 C25 C24 108.1 . . ? C21 C25 C30 125.7 . . ? C24 C25 C30 126.2 . . ? C21 C25 Co2 69.7 . . ? C24 C25 Co2 69.1 . . ? C30 C25 Co2 129.5 . . ? C35 C31 C32 107.7 . . ? C35 C31 C36 126.2 . . ? C32 C31 C36 126.1 . . ? C35 C31 Co2 69.5 . . ? C32 C31 Co2 70.0 . . ? C36 C31 Co2 126.7 . . ? C33 C32 C31 108.1 . . ? C33 C32 C37 125.7 . . ? C31 C32 C37 126.1 . . ? C33 C32 Co2 69.7 . . ? C31 C32 Co2 69.2 . . ? C37 C32 Co2 129.5 . . ? C32 C33 C34 108.0 . . ? C32 C33 C38 125.8 . . ? C34 C33 C38 126.1 . . ? C32 C33 Co2 69.7 . . ? C34 C33 Co2 69.2 . . ? C38 C33 Co2 129.5 . . ? C35 C34 C33 107.8 . . ? C35 C34 C39 126.1 . . ? C33 C34 C39 126.1 . . ? C35 C34 Co2 69.5 . . ? C33 C34 Co2 70.0 . . ? C39 C34 Co2 126.7 . . ? C31 C35 C34 108.4 . . ? C31 C35 C40 125.8 . . ? C34 C35 C40 125.8 . . ? C31 C35 Co2 69.7 . . ? C34 C35 Co2 69.7 . . ? C40 C35 Co2 128.6 . . ? C001 O001 Ga01 111.6(7) . . ? C002 O002 Ga01 110.2(7) . . ? C002 O002 K1 136.5(7) . . ? Ga01 O002 K1 113.2(5) . . ? C002 O002 K1 81.7(6) . 32_545 ? Ga01 O002 K1 100.7(3) . 32_545 ? K1 O002 K1 89.3(3) . 32_545 ? C007 N001 C009 132.9(13) . . ? C007 N001 H001 113.5 . . ? C009 N001 H001 113.5 . . ? C006 C001 C002 121.5(15) . . ? C006 C001 O001 123.4(12) . . ? C002 C001 O001 115.1(13) . . ? C001 C002 C003 118.2(14) . . ? C001 C002 O002 117.8(13) . . ? C003 C002 O002 124.0(12) . . ? C001 C002 K1 108.0(7) . 32_545 ? C003 C002 K1 91.7(6) . 32_545 ? O002 C002 K1 72.2(6) . 32_545 ? C002 C003 C004 121.4(14) . . ? C002 C003 K1 64.8(6) . 32_545 ? C004 C003 K1 119.6(9) . 32_545 ? C002 C003 H003 119.3 . . ? C004 C003 H003 119.3 . . ? K1 C003 H003 86.0 32_545 . ? C005 C004 C003 117.8(14) . . ? C005 C004 H004 121.1 . . ? C003 C004 H004 121.1 . . ? C004 C005 C006 122.0(14) . . ? C004 C005 H005 119.0 . . ? C006 C005 H005 119.0 . . ? C001 C006 C005 119.1(15) . . ? C001 C006 C007 121.2(14) . . ? C005 C006 C007 118.7(15) . . ? N001 C007 O003 119.3(17) . . ? N001 C007 C006 124.5(14) . . ? O003 C007 C006 115.6(16) . . ? C012 C008 C008 120.4(17) 50_554 50_554 ? C012 C008 C009 118.6(13) 50_554 . ? C008 C008 C009 121.0(17) 50_554 . ? N001 C009 C010 117.9(13) . . ? N001 C009 C008 123.0(13) . . ? C010 C009 C008 119.0(14) . . ? C009 C010 C011 118.4(12) . . ? C009 C010 H010 120.8 . . ? C011 C010 H010 120.8 . . ? C012 C011 C010 121.6(12) . . ? C012 C011 H011 119.2 . . ? C010 C011 H011 119.2 . . ? C008 C012 C011 119.4(14) 50_554 . ? C008 C012 H012 120.3 50_554 . ? C011 C012 H012 120.3 . . ? O2S K1 O002 60.2(2) . . ? O2S K1 O002 60.2(2) . 42_644 ? O002 K1 O002 120.4(4) . 42_644 ? O2S K1 O002 54.6(2) . 83_455 ? O002 K1 O002 56.8(3) . 83_455 ? O002 K1 O002 88.4(2) 42_644 83_455 ? O2S K1 O002 54.6(2) . 86 ? O002 K1 O002 88.4(2) . 86 ? O002 K1 O002 56.8(3) 42_644 86 ? O002 K1 O002 109.2(4) 83_455 86 ? O2S K1 C002 80.7(3) . 83_455 ? O002 K1 C002 69.0(3) . 83_455 ? O002 K1 C002 101.5(3) 42_644 83_455 ? O002 K1 C002 26.2(2) 83_455 83_455 ? O002 K1 C002 135.3(5) 86 83_455 ? O2S K1 C002 80.7(3) . 86 ? O002 K1 C002 101.5(3) . 86 ? O002 K1 C002 69.0(3) 42_644 86 ? O002 K1 C002 135.3(5) 83_455 86 ? O002 K1 C002 26.2(2) 86 86 ? C002 K1 C002 161.4(6) 83_455 86 ? O2S K1 C003 93.0(2) . 83_455 ? O002 K1 C003 92.5(3) . 83_455 ? O002 K1 C003 90.5(3) 42_644 83_455 ? O002 K1 C003 43.9(3) 83_455 83_455 ? O002 K1 C003 141.4(3) 86 83_455 ? C002 K1 C003 23.56(19) 83_455 83_455 ? C002 K1 C003 159.0(3) 86 83_455 ? O2S K1 C003 93.0(2) . 86 ? O002 K1 C003 90.5(3) . 86 ? O002 K1 C003 92.5(3) 42_644 86 ? O002 K1 C003 141.4(3) 83_455 86 ? O002 K1 C003 43.9(3) 86 86 ? C002 K1 C003 159.0(3) 83_455 86 ? C002 K1 C003 23.56(19) 86 86 ? C003 K1 C003 173.9(5) 83_455 86 ? O2S K1 Ga01 53.33(7) . . ? O002 K1 Ga01 27.4(2) . . ? O002 K1 Ga01 107.1(2) 42_644 . ? O002 K1 Ga01 29.45(15) 83_455 . ? O002 K1 Ga01 100.3(2) 86 . ? C002 K1 Ga01 44.7(3) 83_455 . ? C002 K1 Ga01 121.2(3) 86 . ? C003 K1 Ga01 67.8(2) 83_455 . ? C003 K1 Ga01 116.1(2) 86 . ? O2S K1 Ga01 53.33(7) . 86 ? O002 K1 Ga01 107.1(2) . 86 ? O002 K1 Ga01 27.4(2) 42_644 86 ? O002 K1 Ga01 100.3(2) 83_455 86 ? O002 K1 Ga01 29.45(15) 86 86 ? C002 K1 Ga01 121.2(3) 83_455 86 ? C002 K1 Ga01 44.7(3) 86 86 ? C003 K1 Ga01 116.1(2) 83_455 86 ? C003 K1 Ga01 67.8(2) 86 86 ? Ga01 K1 Ga01 106.66(14) . 86 ? O2S K1 K1 30.0 . 83_455 ? O002 K1 K1 78.4(2) . 83_455 ? O002 K1 K1 48.8(2) 42_644 83_455 ? O002 K1 K1 41.89(17) 83_455 83_455 ? O002 K1 K1 75.0(2) 86 83_455 ? C002 K1 K1 63.2(3) 83_455 83_455 ? C002 K1 K1 99.9(3) 86 83_455 ? C003 K1 K1 67.4(2) 83_455 83_455 ? C003 K1 K1 118.4(2) 86 83_455 ? Ga01 K1 K1 58.86(6) . 83_455 ? Ga01 K1 K1 58.86(6) 86 83_455 ? K1 O2S K1 120.000(1) 83_455 . ? K1 O2S K1 120.0 83_455 32_545 ? K1 O2S K1 120.000(1) . 32_545 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Co1 C1 C5 106.0(9) 5 . . . ? C11 Co1 C1 C5 48(3) 78_455 . . . ? C11 Co1 C1 C5 153.8(12) 9 . . . ? C11 Co1 C1 C5 23.7(9) 83_455 . . . ? C11 Co1 C1 C5 -16.2(14) 76_455 . . . ? C11 Co1 C1 C5 142.9 . . . . ? C11 Co1 C1 C5 -16.4(2) 60_554 . . . ? C11 Co1 C1 C5 -141.7(15) 34_545 . . . ? C11 Co1 C1 C5 -101.8(6) 27_545 . . . ? C11 Co1 C1 C5 73(5) 50_554 . . . ? C11 Co1 C1 C5 -95.2(9) 32_545 . . . ? C11 Co1 C1 C5 -100.1(16) 55_554 . . . ? C11 Co1 C1 C2 -134.9(9) 5 . . . ? C11 Co1 C1 C2 168(3) 78_455 . . . ? C11 Co1 C1 C2 -87.1(12) 9 . . . ? C11 Co1 C1 C2 142.8(9) 83_455 . . . ? C11 Co1 C1 C2 102.9(14) 76_455 . . . ? C11 Co1 C1 C2 -98.0 . . . . ? C11 Co1 C1 C2 102.7(3) 60_554 . . . ? C11 Co1 C1 C2 -22.6(15) 34_545 . . . ? C11 Co1 C1 C2 17.2(6) 27_545 . . . ? C11 Co1 C1 C2 -168(5) 50_554 . . . ? C11 Co1 C1 C2 23.9(9) 32_545 . . . ? C11 Co1 C1 C2 19.0(16) 55_554 . . . ? C11 Co1 C1 C6 -15.1(9) 5 . . . ? C11 Co1 C1 C6 -73(3) 78_455 . . . ? C11 Co1 C1 C6 32.7(12) 9 . . . ? C11 Co1 C1 C6 -97.4(9) 83_455 . . . ? C11 Co1 C1 C6 -137.3(14) 76_455 . . . ? C11 Co1 C1 C6 21.9 . . . . ? C11 Co1 C1 C6 -137.5(2) 60_554 . . . ? C11 Co1 C1 C6 97.2(15) 34_545 . . . ? C11 Co1 C1 C6 137.1(6) 27_545 . . . ? C11 Co1 C1 C6 -48(5) 50_554 . . . ? C11 Co1 C1 C6 143.8(9) 32_545 . . . ? C11 Co1 C1 C6 138.9(16) 55_554 . . . ? C5 C1 C2 C3 -0.5 . . . . ? C6 C1 C2 C3 174.4 . . . . ? Co1 C1 C2 C3 -60.4 . . . . ? C5 C1 C2 C7 -179.5 . . . . ? C6 C1 C2 C7 -4.6 . . . . ? Co1 C1 C2 C7 120.7 . . . . ? C5 C1 C2 Co1 59.9 . . . . ? C6 C1 C2 Co1 -125.3 . . . . ? C11 Co1 C2 C3 166.4(10) 5 . . . ? C11 Co1 C2 C3 110.1(17) 78_455 . . . ? C11 Co1 C2 C3 -165.9(17) 9 . . . ? C11 Co1 C2 C3 76.0(8) 83_455 . . . ? C11 Co1 C2 C3 61.9(5) 76_455 . . . ? C11 Co1 C2 C3 -142.1 . . . . ? C11 Co1 C2 C3 1(2) 60_554 . . . ? C11 Co1 C2 C3 -96(2) 34_545 . . . ? C11 Co1 C2 C3 23(8) 27_545 . . . ? C11 Co1 C2 C3 -74(4) 50_554 . . . ? C11 Co1 C2 C3 -31.6(11) 32_545 . . . ? C11 Co1 C2 C3 -52.2(8) 55_554 . . . ? C11 Co1 C2 C1 47.9(10) 5 . . . ? C11 Co1 C2 C1 -8.3(17) 78_455 . . . ? C11 Co1 C2 C1 75.6(17) 9 . . . ? C11 Co1 C2 C1 -42.4(8) 83_455 . . . ? C11 Co1 C2 C1 -56.6(5) 76_455 . . . ? C11 Co1 C2 C1 99.4 . . . . ? C11 Co1 C2 C1 -117(2) 60_554 . . . ? C11 Co1 C2 C1 145(2) 34_545 . . . ? C11 Co1 C2 C1 -96(8) 27_545 . . . ? C11 Co1 C2 C1 168(4) 50_554 . . . ? C11 Co1 C2 C1 -150.0(11) 32_545 . . . ? C11 Co1 C2 C1 -170.6(8) 55_554 . . . ? C11 Co1 C2 C7 -72.7(10) 5 . . . ? C11 Co1 C2 C7 -128.9(17) 78_455 . . . ? C11 Co1 C2 C7 -45.0(17) 9 . . . ? C11 Co1 C2 C7 -163.0(8) 83_455 . . . ? C11 Co1 C2 C7 -177.2(5) 76_455 . . . ? C11 Co1 C2 C7 -21.2 . . . . ? C11 Co1 C2 C7 122(2) 60_554 . . . ? C11 Co1 C2 C7 25(2) 34_545 . . . ? C11 Co1 C2 C7 144(8) 27_545 . . . ? C11 Co1 C2 C7 47(4) 50_554 . . . ? C11 Co1 C2 C7 89.4(11) 32_545 . . . ? C11 Co1 C2 C7 68.8(8) 55_554 . . . ? C1 C2 C3 C4 0.7 . . . . ? C7 C2 C3 C4 179.7 . . . . ? Co1 C2 C3 C4 -59.4 . . . . ? C1 C2 C3 C8 -176.6 . . . . ? C7 C2 C3 C8 2.4 . . . . ? Co1 C2 C3 C8 123.3 . . . . ? C1 C2 C3 Co1 60.1 . . . . ? C7 C2 C3 Co1 -120.9 . . . . ? C11 Co1 C3 C4 94.8(17) 5 . . . ? C11 Co1 C3 C4 50.3(14) 78_455 . . . ? C11 Co1 C3 C4 133.7(18) 9 . . . ? C11 Co1 C3 C4 1.92(13) 83_455 . . . ? C11 Co1 C3 C4 21(2) 76_455 . . . ? C11 Co1 C3 C4 -179.2 . . . . ? C11 Co1 C3 C4 -59.2(16) 60_554 . . . ? C11 Co1 C3 C4 170.3(14) 34_545 . . . ? C11 Co1 C3 C4 111(2) 27_545 . . . ? C11 Co1 C3 C4 -87(3) 50_554 . . . ? C11 Co1 C3 C4 -131.3(13) 32_545 . . . ? C11 Co1 C3 C4 -107.1(8) 55_554 . . . ? C11 Co1 C3 C2 -24.9(17) 5 . . . ? C11 Co1 C3 C2 -69.4(14) 78_455 . . . ? C11 Co1 C3 C2 14.0(18) 9 . . . ? C11 Co1 C3 C2 -117.78(14) 83_455 . . . ? C11 Co1 C3 C2 -99(2) 76_455 . . . ? C11 Co1 C3 C2 61.1 . . . . ? C11 Co1 C3 C2 -178.9(16) 60_554 . . . ? C11 Co1 C3 C2 50.6(14) 34_545 . . . ? C11 Co1 C3 C2 -9(2) 27_545 . . . ? C11 Co1 C3 C2 153(3) 50_554 . . . ? C11 Co1 C3 C2 109.0(13) 32_545 . . . ? C11 Co1 C3 C2 133.2(8) 55_554 . . . ? C11 Co1 C3 C8 -144.7(17) 5 . . . ? C11 Co1 C3 C8 170.8(14) 78_455 . . . ? C11 Co1 C3 C8 -105.8(18) 9 . . . ? C11 Co1 C3 C8 122.41(14) 83_455 . . . ? C11 Co1 C3 C8 142(2) 76_455 . . . ? C11 Co1 C3 C8 -58.7 . . . . ? C11 Co1 C3 C8 61.3(16) 60_554 . . . ? C11 Co1 C3 C8 -69.2(14) 34_545 . . . ? C11 Co1 C3 C8 -129(2) 27_545 . . . ? C11 Co1 C3 C8 34(3) 50_554 . . . ? C11 Co1 C3 C8 -10.8(13) 32_545 . . . ? C11 Co1 C3 C8 13.4(8) 55_554 . . . ? C2 C3 C4 C5 -0.7 . . . . ? C8 C3 C4 C5 176.6 . . . . ? Co1 C3 C4 C5 -59.5 . . . . ? C2 C3 C4 C9 -179.7 . . . . ? C8 C3 C4 C9 -2.4 . . . . ? Co1 C3 C4 C9 121.4 . . . . ? C2 C3 C4 Co1 58.9 . . . . ? C8 C3 C4 Co1 -123.9 . . . . ? C11 Co1 C4 C3 -134.4(17) 5 . . . ? C11 Co1 C4 C3 -126.1(7) 78_455 . . . ? C11 Co1 C4 C3 -67.4(17) 9 . . . ? C11 Co1 C4 C3 -130(6) 76_455 . . . ? C11 Co1 C4 C3 114.2(8) 60_554 . . . ? C11 Co1 C4 C3 -8.3(13) 34_545 . . . ? C11 Co1 C4 C3 -33.9(19) 27_545 . . . ? C11 Co1 C4 C3 121(2) 50_554 . . . ? C11 Co1 C4 C3 22.79(13) 32_545 . . . ? C11 Co1 C4 C3 74.2(13) 55_554 . . . ? C11 Co1 C4 C5 -15.4(17) 5 . . . ? C11 Co1 C4 C5 -7.1(7) 78_455 . . . ? C11 Co1 C4 C5 51.6(17) 9 . . . ? C11 Co1 C4 C5 -58.89(13) 83_455 . . . ? C11 Co1 C4 C5 -11(6) 76_455 . . . ? C11 Co1 C4 C5 -126.9(8) 60_554 . . . ? C11 Co1 C4 C5 110.6(13) 34_545 . . . ? C11 Co1 C4 C5 85.1(19) 27_545 . . . ? C11 Co1 C4 C5 -121(2) 50_554 . . . ? C11 Co1 C4 C5 141.77(13) 32_545 . . . ? C11 Co1 C4 C5 -166.8(13) 55_554 . . . ? C11 Co1 C4 C9 105.2(17) 5 . . . ? C11 Co1 C4 C9 113.4(8) 78_455 . . . ? C11 Co1 C4 C9 172.1(17) 9 . . . ? C11 Co1 C4 C9 61.70(13) 83_455 . . . ? C11 Co1 C4 C9 110(6) 76_455 . . . ? C11 Co1 C4 C9 -6.3(8) 60_554 . . . ? C11 Co1 C4 C9 -128.8(13) 34_545 . . . ? C11 Co1 C4 C9 -154.3(19) 27_545 . . . ? C11 Co1 C4 C9 -97.64(13) 32_545 . . . ? C11 Co1 C4 C9 -46.2(13) 55_554 . . . ? C2 C1 C5 C4 0.1 . . . . ? C6 C1 C5 C4 -174.8 . . . . ? Co1 C1 C5 C4 59.5 . . . . ? C2 C1 C5 C10 176.6 . . . . ? C6 C1 C5 C10 1.7 . . . . ? Co1 C1 C5 C10 -124.0 . . . . ? C2 C1 C5 Co1 -59.4 . . . . ? C6 C1 C5 Co1 125.8 . . . . ? C3 C4 C5 C1 0.4 . . . . ? C9 C4 C5 C1 179.4 . . . . ? Co1 C4 C5 C1 -59.1 . . . . ? C3 C4 C5 C10 -176.1 . . . . ? C9 C4 C5 C10 2.9 . . . . ? Co1 C4 C5 C10 124.4 . . . . ? C3 C4 C5 Co1 59.5 . . . . ? C9 C4 C5 Co1 -121.5 . . . . ? C11 Co1 C5 C1 -72.0(11) 5 . . . ? C11 Co1 C5 C1 -73.8(18) 78_455 . . . ? C11 Co1 C5 C1 -24.3(12) 9 . . . ? C11 Co1 C5 C1 -147.9(10) 83_455 . . . ? C11 Co1 C5 C1 133(7) 76_455 . . . ? C11 Co1 C5 C1 -60.6 . . . . ? C11 Co1 C5 C1 168.5(4) 60_554 . . . ? C11 Co1 C5 C1 40.0(17) 34_545 . . . ? C11 Co1 C5 C1 49.1(13) 27_545 . . . ? C11 Co1 C5 C1 -153.7(17) 50_554 . . . ? C11 Co1 C5 C1 86.6(5) 32_545 . . . ? C11 Co1 C5 C1 139(2) 55_554 . . . ? C11 Co1 C5 C4 168.7(11) 5 . . . ? C11 Co1 C5 C4 166.9(18) 78_455 . . . ? C11 Co1 C5 C4 -143.6(12) 9 . . . ? C11 Co1 C5 C4 92.8(10) 83_455 . . . ? C11 Co1 C5 C4 14(7) 76_455 . . . ? C11 Co1 C5 C4 -179.9 . . . . ? C11 Co1 C5 C4 49.2(4) 60_554 . . . ? C11 Co1 C5 C4 -79.3(17) 34_545 . . . ? C11 Co1 C5 C4 -70.2(13) 27_545 . . . ? C11 Co1 C5 C4 87.0(17) 50_554 . . . ? C11 Co1 C5 C4 -32.7(5) 32_545 . . . ? C11 Co1 C5 C4 19(2) 55_554 . . . ? C11 Co1 C5 C10 47.8(11) 5 . . . ? C11 Co1 C5 C10 46.1(18) 78_455 . . . ? C11 Co1 C5 C10 95.5(12) 9 . . . ? C11 Co1 C5 C10 -28.0(10) 83_455 . . . ? C11 Co1 C5 C10 -107(7) 76_455 . . . ? C11 Co1 C5 C10 59.2 . . . . ? C11 Co1 C5 C10 -71.7(4) 60_554 . . . ? C11 Co1 C5 C10 159.8(17) 34_545 . . . ? C11 Co1 C5 C10 168.9(13) 27_545 . . . ? C11 Co1 C5 C10 -33.9(17) 50_554 . . . ? C11 Co1 C5 C10 -153.6(5) 32_545 . . . ? C11 Co1 C5 C10 -102(2) 55_554 . . . ? C11 Co1 C11 C15 -46.0(16) 5 . . . ? C11 Co1 C11 C15 -54.1(7) 78_455 . . . ? C11 Co1 C11 C15 -112.3(16) 9 . . . ? C11 Co1 C11 C15 -2.08(14) 83_455 . . . ? C11 Co1 C11 C15 -51(6) 76_455 . . . ? C11 Co1 C11 C15 65.8(7) 60_554 . . . ? C11 Co1 C11 C15 -171.8(13) 34_545 . . . ? C11 Co1 C11 C15 -146.7(19) 27_545 . . . ? C11 Co1 C11 C15 59(2) 50_554 . . . ? C11 Co1 C11 C15 156.80(14) 32_545 . . . ? C11 Co1 C11 C15 105.5(13) 55_554 . . . ? C11 Co1 C11 C12 -164.7(16) 5 . . . ? C11 Co1 C11 C12 -172.9(7) 78_455 . . . ? C11 Co1 C11 C12 128.9(16) 9 . . . ? C11 Co1 C11 C12 -120.85(14) 83_455 . . . ? C11 Co1 C11 C12 -169(6) 76_455 . . . ? C11 Co1 C11 C12 -53.0(7) 60_554 . . . ? C11 Co1 C11 C12 69.4(13) 34_545 . . . ? C11 Co1 C11 C12 94.5(19) 27_545 . . . ? C11 Co1 C11 C12 -60(2) 50_554 . . . ? C11 Co1 C11 C12 38.03(14) 32_545 . . . ? C11 Co1 C11 C12 -13.2(13) 55_554 . . . ? C11 Co1 C11 C16 74.3(16) 5 . . . ? C11 Co1 C11 C16 66.2(7) 78_455 . . . ? C11 Co1 C11 C16 7.9(16) 9 . . . ? C11 Co1 C11 C16 118.20(14) 83_455 . . . ? C11 Co1 C11 C16 70(6) 76_455 . . . ? C11 Co1 C11 C16 -173.9(7) 60_554 . . . ? C11 Co1 C11 C16 -51.5(13) 34_545 . . . ? C11 Co1 C11 C16 -26.4(19) 27_545 . . . ? C11 Co1 C11 C16 179(2) 50_554 . . . ? C11 Co1 C11 C16 -82.93(14) 32_545 . . . ? C11 Co1 C11 C16 -134.2(13) 55_554 . . . ? C15 C11 C12 C13 -0.4 . . . . ? C16 C11 C12 C13 -179.4 . . . . ? Co1 C11 C12 C13 59.0 . . . . ? C15 C11 C12 C17 176.1 . . . . ? C16 C11 C12 C17 -2.9 . . . . ? Co1 C11 C12 C17 -124.5 . . . . ? C15 C11 C12 Co1 -59.5 . . . . ? C16 C11 C12 Co1 121.5 . . . . ? C11 Co1 C12 C13 -108.6(11) 5 . . . ? C11 Co1 C12 C13 -106.2(19) 78_455 . . . ? C11 Co1 C12 C13 -156.0(12) 9 . . . ? C11 Co1 C12 C13 -31.3(10) 83_455 . . . ? C11 Co1 C12 C13 48(6) 76_455 . . . ? C11 Co1 C12 C13 -119.9 . . . . ? C11 Co1 C12 C13 10.8(4) 60_554 . . . ? C11 Co1 C12 C13 140.0(17) 34_545 . . . ? C11 Co1 C12 C13 129.6(12) 27_545 . . . ? C11 Co1 C12 C13 -28.2(17) 50_554 . . . ? C11 Co1 C12 C13 92.9(5) 32_545 . . . ? C11 Co1 C12 C13 40(2) 55_554 . . . ? C11 Co1 C12 C11 11.3(11) 5 . . . ? C11 Co1 C12 C11 13.6(19) 78_455 . . . ? C11 Co1 C12 C11 -36.2(12) 9 . . . ? C11 Co1 C12 C11 88.5(10) 83_455 . . . ? C11 Co1 C12 C11 168(6) 76_455 . . . ? C11 Co1 C12 C11 130.7(4) 60_554 . . . ? C11 Co1 C12 C11 -100.1(17) 34_545 . . . ? C11 Co1 C12 C11 -110.5(12) 27_545 . . . ? C11 Co1 C12 C11 91.7(17) 50_554 . . . ? C11 Co1 C12 C11 -147.2(5) 32_545 . . . ? C11 Co1 C12 C11 160(2) 55_554 . . . ? C11 Co1 C12 C17 131.0(11) 5 . . . ? C11 Co1 C12 C17 133.4(19) 78_455 . . . ? C11 Co1 C12 C17 83.6(12) 9 . . . ? C11 Co1 C12 C17 -151.7(10) 83_455 . . . ? C11 Co1 C12 C17 -73(6) 76_455 . . . ? C11 Co1 C12 C17 119.8 . . . . ? C11 Co1 C12 C17 -109.6(4) 60_554 . . . ? C11 Co1 C12 C17 19.7(17) 34_545 . . . ? C11 Co1 C12 C17 9.2(12) 27_545 . . . ? C11 Co1 C12 C17 -148.5(17) 50_554 . . . ? C11 Co1 C12 C17 -27.4(5) 32_545 . . . ? C11 Co1 C12 C17 -80(2) 55_554 . . . ? C11 C12 C13 C14 0.0 . . . . ? C17 C12 C13 C14 -176.5 . . . . ? Co1 C12 C13 C14 58.0 . . . . ? C11 C12 C13 C18 176.6 . . . . ? C17 C12 C13 C18 0.1 . . . . ? Co1 C12 C13 C18 -125.4 . . . . ? C11 C12 C13 Co1 -58.0 . . . . ? C17 C12 C13 Co1 125.5 . . . . ? C11 Co1 C13 C12 74.6(9) 5 . . . ? C11 Co1 C13 C12 134(3) 78_455 . . . ? C11 Co1 C13 C12 26.3(13) 9 . . . ? C11 Co1 C13 C12 156.9(9) 83_455 . . . ? C11 Co1 C13 C12 -162.6(14) 76_455 . . . ? C11 Co1 C13 C12 37.7 . . . . ? C11 Co1 C13 C12 -164.2(3) 60_554 . . . ? C11 Co1 C13 C12 -38.2(15) 34_545 . . . ? C11 Co1 C13 C12 -79.1(6) 27_545 . . . ? C11 Co1 C13 C12 103(5) 50_554 . . . ? C11 Co1 C13 C12 -84.3(9) 32_545 . . . ? C11 Co1 C13 C12 -76.8(16) 55_554 . . . ? C11 Co1 C13 C14 -45.5(9) 5 . . . ? C11 Co1 C13 C14 14(3) 78_455 . . . ? C11 Co1 C13 C14 -93.8(13) 9 . . . ? C11 Co1 C13 C14 36.7(9) 83_455 . . . ? C11 Co1 C13 C14 77.2(14) 76_455 . . . ? C11 Co1 C13 C14 -82.5 . . . . ? C11 Co1 C13 C14 75.6(3) 60_554 . . . ? C11 Co1 C13 C14 -158.4(15) 34_545 . . . ? C11 Co1 C13 C14 160.7(6) 27_545 . . . ? C11 Co1 C13 C14 -17(5) 50_554 . . . ? C11 Co1 C13 C14 155.5(9) 32_545 . . . ? C11 Co1 C13 C14 163.0(16) 55_554 . . . ? C11 Co1 C13 C18 -165.7(9) 5 . . . ? C11 Co1 C13 C18 -106(3) 78_455 . . . ? C11 Co1 C13 C18 146.0(13) 9 . . . ? C11 Co1 C13 C18 -83.4(9) 83_455 . . . ? C11 Co1 C13 C18 -42.9(14) 76_455 . . . ? C11 Co1 C13 C18 157.4 . . . . ? C11 Co1 C13 C18 -44.5(3) 60_554 . . . ? C11 Co1 C13 C18 81.5(15) 34_545 . . . ? C11 Co1 C13 C18 40.6(6) 27_545 . . . ? C11 Co1 C13 C18 -137(5) 50_554 . . . ? C11 Co1 C13 C18 35.4(9) 32_545 . . . ? C11 Co1 C13 C18 42.9(16) 55_554 . . . ? C12 C13 C14 C15 0.4 . . . . ? C18 C13 C14 C15 -176.1 . . . . ? Co1 C13 C14 C15 58.6 . . . . ? C12 C13 C14 C19 179.5 . . . . ? C18 C13 C14 C19 3.0 . . . . ? Co1 C13 C14 C19 -122.3 . . . . ? C12 C13 C14 Co1 -58.2 . . . . ? C18 C13 C14 Co1 125.3 . . . . ? C11 Co1 C14 C15 13.2(10) 5 . . . ? C11 Co1 C14 C15 69.9(17) 78_455 . . . ? C11 Co1 C14 C15 -14.2(17) 9 . . . ? C11 Co1 C14 C15 103.0(8) 83_455 . . . ? C11 Co1 C14 C15 118.3(4) 76_455 . . . ? C11 Co1 C14 C15 -37.8 . . . . ? C11 Co1 C14 C15 179(2) 60_554 . . . ? C11 Co1 C14 C15 -86(2) 34_545 . . . ? C11 Co1 C14 C15 158(7) 27_545 . . . ? C11 Co1 C14 C15 -102(4) 50_554 . . . ? C11 Co1 C14 C15 -149.5(11) 32_545 . . . ? C11 Co1 C14 C15 -127.4(9) 55_554 . . . ? C11 Co1 C14 C13 132.4(10) 5 . . . ? C11 Co1 C14 C13 -170.8(17) 78_455 . . . ? C11 Co1 C14 C13 105.0(17) 9 . . . ? C11 Co1 C14 C13 -137.7(8) 83_455 . . . ? C11 Co1 C14 C13 -122.4(4) 76_455 . . . ? C11 Co1 C14 C13 81.4 . . . . ? C11 Co1 C14 C13 -62(2) 60_554 . . . ? C11 Co1 C14 C13 33(2) 34_545 . . . ? C11 Co1 C14 C13 -83(7) 27_545 . . . ? C11 Co1 C14 C13 17(4) 50_554 . . . ? C11 Co1 C14 C13 -30.2(11) 32_545 . . . ? C11 Co1 C14 C13 -8.1(9) 55_554 . . . ? C11 Co1 C14 C19 -106.8(10) 5 . . . ? C11 Co1 C14 C19 -50.0(17) 78_455 . . . ? C11 Co1 C14 C19 -134.1(17) 9 . . . ? C11 Co1 C14 C19 -16.9(8) 83_455 . . . ? C11 Co1 C14 C19 -1.6(4) 76_455 . . . ? C11 Co1 C14 C19 -157.8 . . . . ? C11 Co1 C14 C19 59(2) 60_554 . . . ? C11 Co1 C14 C19 154(2) 34_545 . . . ? C11 Co1 C14 C19 38(7) 27_545 . . . ? C11 Co1 C14 C19 138(4) 50_554 . . . ? C11 Co1 C14 C19 90.6(11) 32_545 . . . ? C11 Co1 C14 C19 112.7(8) 55_554 . . . ? C13 C14 C15 C11 -0.7 . . . . ? C19 C14 C15 C11 -179.8 . . . . ? Co1 C14 C15 C11 58.8 . . . . ? C13 C14 C15 C20 176.3 . . . . ? C19 C14 C15 C20 -2.8 . . . . ? Co1 C14 C15 C20 -124.2 . . . . ? C13 C14 C15 Co1 -59.5 . . . . ? C19 C14 C15 Co1 121.4 . . . . ? C12 C11 C15 C14 0.7 . . . . ? C16 C11 C15 C14 179.7 . . . . ? Co1 C11 C15 C14 -59.4 . . . . ? C12 C11 C15 C20 -176.3 . . . . ? C16 C11 C15 C20 2.7 . . . . ? Co1 C11 C15 C20 123.6 . . . . ? C12 C11 C15 Co1 60.1 . . . . ? C16 C11 C15 Co1 -120.9 . . . . ? C11 Co1 C15 C14 -156.2(17) 5 . . . ? C11 Co1 C15 C14 -110.6(14) 78_455 . . . ? C11 Co1 C15 C14 166.1(18) 9 . . . ? C11 Co1 C15 C14 -62.18(15) 83_455 . . . ? C11 Co1 C15 C14 -81(2) 76_455 . . . ? C11 Co1 C15 C14 119.7 . . . . ? C11 Co1 C15 C14 -1.0(16) 60_554 . . . ? C11 Co1 C15 C14 129.3(14) 34_545 . . . ? C11 Co1 C15 C14 -170(2) 27_545 . . . ? C11 Co1 C15 C14 28(3) 50_554 . . . ? C11 Co1 C15 C14 69.1(14) 32_545 . . . ? C11 Co1 C15 C14 46.9(8) 55_554 . . . ? C11 Co1 C15 C11 84.1(17) 5 . . . ? C11 Co1 C15 C11 129.7(14) 78_455 . . . ? C11 Co1 C15 C11 46.4(18) 9 . . . ? C11 Co1 C15 C11 178.14(15) 83_455 . . . ? C11 Co1 C15 C11 160(2) 76_455 . . . ? C11 Co1 C15 C11 -120.7(16) 60_554 . . . ? C11 Co1 C15 C11 9.6(14) 34_545 . . . ? C11 Co1 C15 C11 71(2) 27_545 . . . ? C11 Co1 C15 C11 -92(3) 50_554 . . . ? C11 Co1 C15 C11 -50.5(14) 32_545 . . . ? C11 Co1 C15 C11 -72.8(8) 55_554 . . . ? C11 Co1 C15 C20 -34.8(17) 5 . . . ? C11 Co1 C15 C20 10.9(14) 78_455 . . . ? C11 Co1 C15 C20 -72.4(18) 9 . . . ? C11 Co1 C15 C20 59.29(15) 83_455 . . . ? C11 Co1 C15 C20 41(2) 76_455 . . . ? C11 Co1 C15 C20 -118.8 . . . . ? C11 Co1 C15 C20 120.5(16) 60_554 . . . ? C11 Co1 C15 C20 -109.2(14) 34_545 . . . ? C11 Co1 C15 C20 -48(2) 27_545 . . . ? C11 Co1 C15 C20 149(3) 50_554 . . . ? C11 Co1 C15 C20 -169.4(14) 32_545 . . . ? C11 Co1 C15 C20 168.4(8) 55_554 . . . ? C23 Co2 C21 C25 62.8(3) 78_455 . . . ? C23 Co2 C21 C25 98.4(9) 145_565 . . . ? C23 Co2 C21 C25 -117.2(11) 126_655 . . . ? C23 Co2 C21 C25 -163.9(17) 108_566 . . . ? C23 Co2 C21 C25 -81.6 . . . . ? C23 Co2 C21 C25 16(2) 60_554 . . . ? C35 Co2 C21 C25 62.8(11) 126_655 . . . ? C35 Co2 C21 C25 16.1(17) 108_566 . . . ? C35 Co2 C21 C25 -117.2(3) 78_455 . . . ? C35 Co2 C21 C25 -164(2) 60_554 . . . ? C35 Co2 C21 C25 98.4 . . . . ? C35 Co2 C21 C25 -81.6(9) 145_565 . . . ? C23 Co2 C21 C22 -177.6(3) 78_455 . . . ? C23 Co2 C21 C22 -142.0(9) 145_565 . . . ? C23 Co2 C21 C22 2.4(11) 126_655 . . . ? C23 Co2 C21 C22 -44.3(17) 108_566 . . . ? C23 Co2 C21 C22 38.0 . . . . ? C23 Co2 C21 C22 136(2) 60_554 . . . ? C35 Co2 C21 C22 -177.6(11) 126_655 . . . ? C35 Co2 C21 C22 135.7(17) 108_566 . . . ? C35 Co2 C21 C22 2.4(3) 78_455 . . . ? C35 Co2 C21 C22 -44(2) 60_554 . . . ? C35 Co2 C21 C22 -142.0 . . . . ? C35 Co2 C21 C22 38.0(9) 145_565 . . . ? C23 Co2 C21 C26 -57.3(3) 78_455 . . . ? C23 Co2 C21 C26 -21.7(9) 145_565 . . . ? C23 Co2 C21 C26 122.7(11) 126_655 . . . ? C23 Co2 C21 C26 76.0(17) 108_566 . . . ? C23 Co2 C21 C26 158.3 . . . . ? C23 Co2 C21 C26 -104(2) 60_554 . . . ? C35 Co2 C21 C26 -57.3(11) 126_655 . . . ? C35 Co2 C21 C26 -104.0(17) 108_566 . . . ? C35 Co2 C21 C26 122.7(3) 78_455 . . . ? C35 Co2 C21 C26 76(2) 60_554 . . . ? C35 Co2 C21 C26 -21.7 . . . . ? C35 Co2 C21 C26 158.3(9) 145_565 . . . ? C25 C21 C22 C23 -0.3 . . . . ? C26 C21 C22 C23 176.1 . . . . ? Co2 C21 C22 C23 -59.4 . . . . ? C25 C21 C22 C27 -179.4 . . . . ? C26 C21 C22 C27 -3.0 . . . . ? Co2 C21 C22 C27 121.4 . . . . ? C25 C21 C22 Co2 59.1 . . . . ? C26 C21 C22 Co2 -124.4 . . . . ? C23 Co2 C22 C23 120.8(3) 78_455 . . . ? C23 Co2 C22 C23 180.0(15) 145_565 . . . ? C23 Co2 C22 C23 -59.2(9) 126_655 . . . ? C23 Co2 C22 C23 146(2) 108_566 . . . ? C23 Co2 C22 C23 -33.9(2) 60_554 . . . ? C35 Co2 C22 C23 120.8(9) 126_655 . . . ? C35 Co2 C22 C23 -34(2) 108_566 . . . ? C35 Co2 C22 C23 -59.2(3) 78_455 . . . ? C35 Co2 C22 C23 146.1(2) 60_554 . . . ? C35 Co2 C22 C23 180.0 . . . . ? C35 Co2 C22 C23 0.0(15) 145_565 . . . ? C23 Co2 C22 C21 1.9(3) 78_455 . . . ? C23 Co2 C22 C21 61.1(15) 145_565 . . . ? C23 Co2 C22 C21 -178.1(9) 126_655 . . . ? C23 Co2 C22 C21 27(2) 108_566 . . . ? C23 Co2 C22 C21 -118.9 . . . . ? C23 Co2 C22 C21 -152.7(2) 60_554 . . . ? C35 Co2 C22 C21 1.9(9) 126_655 . . . ? C35 Co2 C22 C21 -153(2) 108_566 . . . ? C35 Co2 C22 C21 -178.1(3) 78_455 . . . ? C35 Co2 C22 C21 27.3(2) 60_554 . . . ? C35 Co2 C22 C21 61.1 . . . . ? C35 Co2 C22 C21 -118.9(15) 145_565 . . . ? C23 Co2 C22 C27 -118.8(3) 78_455 . . . ? C23 Co2 C22 C27 -59.6(15) 145_565 . . . ? C23 Co2 C22 C27 61.2(9) 126_655 . . . ? C23 Co2 C22 C27 -93(2) 108_566 . . . ? C23 Co2 C22 C27 120.4 . . . . ? C23 Co2 C22 C27 86.5(2) 60_554 . . . ? C35 Co2 C22 C27 -118.8(9) 126_655 . . . ? C35 Co2 C22 C27 87(2) 108_566 . . . ? C35 Co2 C22 C27 61.2(3) 78_455 . . . ? C35 Co2 C22 C27 -93.5(2) 60_554 . . . ? C35 Co2 C22 C27 -59.6 . . . . ? C35 Co2 C22 C27 120.4(15) 145_565 . . . ? C21 C22 C23 C24 0.6 . . . . ? C27 C22 C23 C24 179.8 . . . . ? Co2 C22 C23 C24 -59.1 . . . . ? C21 C22 C23 C28 -176.6 . . . . ? C27 C22 C23 C28 2.5 . . . . ? Co2 C22 C23 C28 123.6 . . . . ? C21 C22 C23 Co2 59.8 . . . . ? C27 C22 C23 Co2 -121.1 . . . . ? C23 Co2 C23 C24 51.4(3) 78_455 . . . ? C23 Co2 C23 C24 -128.6(9) 126_655 . . . ? C23 Co2 C23 C24 102.2(10) 108_566 . . . ? C23 Co2 C23 C24 -77.8(3) 60_554 . . . ? C35 Co2 C23 C24 51.4(9) 126_655 . . . ? C35 Co2 C23 C24 -77.8(10) 108_566 . . . ? C35 Co2 C23 C24 -128.6(3) 78_455 . . . ? C35 Co2 C23 C24 102.2(3) 60_554 . . . ? C23 Co2 C23 C22 -68.3(3) 78_455 . . . ? C23 Co2 C23 C22 111.7(9) 126_655 . . . ? C23 Co2 C23 C22 -17.5(10) 108_566 . . . ? C23 Co2 C23 C22 162.5(3) 60_554 . . . ? C35 Co2 C23 C22 -68.3(9) 126_655 . . . ? C35 Co2 C23 C22 162.5(10) 108_566 . . . ? C35 Co2 C23 C22 111.7(3) 78_455 . . . ? C35 Co2 C23 C22 -17.5(3) 60_554 . . . ? C23 Co2 C23 C28 171.5(3) 78_455 . . . ? C23 Co2 C23 C28 -8.5(9) 126_655 . . . ? C23 Co2 C23 C28 -137.6(10) 108_566 . . . ? C23 Co2 C23 C28 42.4(3) 60_554 . . . ? C35 Co2 C23 C28 42.4(10) 108_566 . . . ? C35 Co2 C23 C28 -8.4(3) 78_455 . . . ? C35 Co2 C23 C28 -137.6(3) 60_554 . . . ? C22 C23 C24 C25 -0.7 . . . . ? C28 C23 C24 C25 176.5 . . . . ? Co2 C23 C24 C25 -59.9 . . . . ? C22 C23 C24 C29 -179.6 . . . . ? C28 C23 C24 C29 -2.4 . . . . ? Co2 C23 C24 C29 121.2 . . . . ? C22 C23 C24 Co2 59.2 . . . . ? C28 C23 C24 Co2 -123.6 . . . . ? C23 Co2 C24 C23 -133.7(6) 78_455 . . . ? C23 Co2 C24 C23 180.0(16) 145_565 . . . ? C23 Co2 C24 C23 46.3(5) 126_655 . . . ? C23 Co2 C24 C23 -66.0(5) 108_566 . . . ? C23 Co2 C24 C23 114.0(7) 60_554 . . . ? C35 Co2 C24 C23 -133.7(5) 126_655 . . . ? C35 Co2 C24 C23 114.0(5) 108_566 . . . ? C35 Co2 C24 C23 46.3(6) 78_455 . . . ? C35 Co2 C24 C23 -66.0(7) 60_554 . . . ? C35 Co2 C24 C23 -180.0 . . . . ? C35 Co2 C24 C23 0.0(16) 145_565 . . . ? C23 Co2 C24 C25 -14.9(6) 78_455 . . . ? C23 Co2 C24 C25 -61.2(16) 145_565 . . . ? C23 Co2 C24 C25 165.1(5) 126_655 . . . ? C23 Co2 C24 C25 52.8(5) 108_566 . . . ? C23 Co2 C24 C25 118.8 . . . . ? C23 Co2 C24 C25 -127.2(7) 60_554 . . . ? C35 Co2 C24 C25 -14.9(5) 126_655 . . . ? C35 Co2 C24 C25 -127.2(5) 108_566 . . . ? C35 Co2 C24 C25 165.1(6) 78_455 . . . ? C35 Co2 C24 C25 52.8(7) 60_554 . . . ? C35 Co2 C24 C25 -61.2 . . . . ? C35 Co2 C24 C25 118.8(16) 145_565 . . . ? C23 Co2 C24 C29 105.9(6) 78_455 . . . ? C23 Co2 C24 C29 59.6(16) 145_565 . . . ? C23 Co2 C24 C29 -74.1(5) 126_655 . . . ? C23 Co2 C24 C29 173.6(4) 108_566 . . . ? C23 Co2 C24 C29 -120.4 . . . . ? C23 Co2 C24 C29 -6.4(7) 60_554 . . . ? C35 Co2 C24 C29 105.9(5) 126_655 . . . ? C35 Co2 C24 C29 -6.4(4) 108_566 . . . ? C35 Co2 C24 C29 -74.1(6) 78_455 . . . ? C35 Co2 C24 C29 173.6(7) 60_554 . . . ? C35 Co2 C24 C29 59.7 . . . . ? C35 Co2 C24 C29 -120.3(16) 145_565 . . . ? C22 C21 C25 C24 -0.1 . . . . ? C26 C21 C25 C24 -176.6 . . . . ? Co2 C21 C25 C24 58.6 . . . . ? C22 C21 C25 C30 176.6 . . . . ? C26 C21 C25 C30 0.1 . . . . ? Co2 C21 C25 C30 -124.7 . . . . ? C22 C21 C25 Co2 -58.8 . . . . ? C26 C21 C25 Co2 124.8 . . . . ? C23 C24 C25 C21 0.5 . . . . ? C29 C24 C25 C21 179.4 . . . . ? Co2 C24 C25 C21 -59.0 . . . . ? C23 C24 C25 C30 -176.1 . . . . ? C29 C24 C25 C30 2.8 . . . . ? Co2 C24 C25 C30 124.3 . . . . ? C23 C24 C25 Co2 59.5 . . . . ? C29 C24 C25 Co2 -121.6 . . . . ? C23 Co2 C25 C21 -81.1(7) 78_455 . . . ? C23 Co2 C25 C21 -98.3(10) 145_565 . . . ? C23 Co2 C25 C21 98.9(9) 126_655 . . . ? C23 Co2 C25 C21 6.0(5) 108_566 . . . ? C23 Co2 C25 C21 81.7 . . . . ? C23 Co2 C25 C21 -174.0(10) 60_554 . . . ? C35 Co2 C25 C21 -81.1(9) 126_655 . . . ? C35 Co2 C25 C21 -173.9(5) 108_566 . . . ? C35 Co2 C25 C21 98.9(7) 78_455 . . . ? C35 Co2 C25 C21 6.1(10) 60_554 . . . ? C35 Co2 C25 C21 -98.3 . . . . ? C35 Co2 C25 C21 81.7(10) 145_565 . . . ? C23 Co2 C25 C24 159.2(7) 78_455 . . . ? C23 Co2 C25 C24 142.0(10) 145_565 . . . ? C23 Co2 C25 C24 -20.8(9) 126_655 . . . ? C23 Co2 C25 C24 -113.6(5) 108_566 . . . ? C23 Co2 C25 C24 -38.0 . . . . ? C23 Co2 C25 C24 66.4(10) 60_554 . . . ? C35 Co2 C25 C24 159.2(9) 126_655 . . . ? C35 Co2 C25 C24 66.4(5) 108_566 . . . ? C35 Co2 C25 C24 -20.8(7) 78_455 . . . ? C35 Co2 C25 C24 -113.6(10) 60_554 . . . ? C35 Co2 C25 C24 142.0 . . . . ? C35 Co2 C25 C24 -38.0(10) 145_565 . . . ? C23 Co2 C25 C30 38.9(7) 78_455 . . . ? C23 Co2 C25 C30 21.7(10) 145_565 . . . ? C23 Co2 C25 C30 -141.1(9) 126_655 . . . ? C23 Co2 C25 C30 126.1(5) 108_566 . . . ? C23 Co2 C25 C30 -158.3 . . . . ? C23 Co2 C25 C30 -53.9(10) 60_554 . . . ? C35 Co2 C25 C30 39.0(9) 126_655 . . . ? C35 Co2 C25 C30 -53.9(5) 108_566 . . . ? C35 Co2 C25 C30 -141.0(7) 78_455 . . . ? C35 Co2 C25 C30 126.1(10) 60_554 . . . ? C35 Co2 C25 C30 21.7 . . . . ? C35 Co2 C25 C30 -158.3(10) 145_565 . . . ? C23 Co2 C31 C35 -46.3(6) 78_455 . . . ? C23 Co2 C31 C35 0.0(16) 145_565 . . . ? C23 Co2 C31 C35 133.7(5) 126_655 . . . ? C23 Co2 C31 C35 -114.0(5) 108_566 . . . ? C23 Co2 C31 C35 -180.0 . . . . ? C23 Co2 C31 C35 66.0(7) 60_554 . . . ? C35 Co2 C31 C35 -46.3(5) 126_655 . . . ? C35 Co2 C31 C35 66.0(5) 108_566 . . . ? C35 Co2 C31 C35 133.7(6) 78_455 . . . ? C35 Co2 C31 C35 -114.0(7) 60_554 . . . ? C35 Co2 C31 C35 180.0(16) 145_565 . . . ? C23 Co2 C31 C32 -165.1(6) 78_455 . . . ? C23 Co2 C31 C32 -118.8(16) 145_565 . . . ? C23 Co2 C31 C32 14.9(5) 126_655 . . . ? C23 Co2 C31 C32 127.2(5) 108_566 . . . ? C23 Co2 C31 C32 61.2 . . . . ? C23 Co2 C31 C32 -52.8(7) 60_554 . . . ? C35 Co2 C31 C32 -165.1(5) 126_655 . . . ? C35 Co2 C31 C32 -52.8(5) 108_566 . . . ? C35 Co2 C31 C32 14.9(6) 78_455 . . . ? C35 Co2 C31 C32 127.2(7) 60_554 . . . ? C35 Co2 C31 C32 -118.8 . . . . ? C35 Co2 C31 C32 61.2(16) 145_565 . . . ? C23 Co2 C31 C36 74.1(6) 78_455 . . . ? C23 Co2 C31 C36 120.5(16) 145_565 . . . ? C23 Co2 C31 C36 -105.9(5) 126_655 . . . ? C23 Co2 C31 C36 6.5(4) 108_566 . . . ? C23 Co2 C31 C36 -59.5 . . . . ? C23 Co2 C31 C36 -173.5(7) 60_554 . . . ? C35 Co2 C31 C36 74.1(5) 126_655 . . . ? C35 Co2 C31 C36 -173.5(4) 108_566 . . . ? C35 Co2 C31 C36 -105.9(6) 78_455 . . . ? C35 Co2 C31 C36 6.5(7) 60_554 . . . ? C35 Co2 C31 C36 120.4 . . . . ? C35 Co2 C31 C36 -59.6(16) 145_565 . . . ? C35 C31 C32 C33 -0.4 . . . . ? C36 C31 C32 C33 -179.5 . . . . ? Co2 C31 C32 C33 59.0 . . . . ? C35 C31 C32 C37 176.1 . . . . ? C36 C31 C32 C37 -2.9 . . . . ? Co2 C31 C32 C37 -124.4 . . . . ? C35 C31 C32 Co2 -59.5 . . . . ? C36 C31 C32 Co2 121.5 . . . . ? C23 Co2 C32 C33 -98.9(7) 78_455 . . . ? C23 Co2 C32 C33 -81.7(10) 145_565 . . . ? C23 Co2 C32 C33 81.1(9) 126_655 . . . ? C23 Co2 C32 C33 174.0(5) 108_566 . . . ? C23 Co2 C32 C33 98.3 . . . . ? C23 Co2 C32 C33 -6.0(10) 60_554 . . . ? C35 Co2 C32 C33 -98.9(9) 126_655 . . . ? C35 Co2 C32 C33 -6.1(5) 108_566 . . . ? C35 Co2 C32 C33 81.1(7) 78_455 . . . ? C35 Co2 C32 C33 173.9(10) 60_554 . . . ? C35 Co2 C32 C33 -81.7 . . . . ? C35 Co2 C32 C33 98.3(10) 145_565 . . . ? C23 Co2 C32 C31 20.8(7) 78_455 . . . ? C23 Co2 C32 C31 38.0(10) 145_565 . . . ? C23 Co2 C32 C31 -159.2(9) 126_655 . . . ? C23 Co2 C32 C31 -66.4(5) 108_566 . . . ? C23 Co2 C32 C31 -142.0 . . . . ? C23 Co2 C32 C31 113.6(10) 60_554 . . . ? C35 Co2 C32 C31 20.7(9) 126_655 . . . ? C35 Co2 C32 C31 113.6(5) 108_566 . . . ? C35 Co2 C32 C31 -159.3(7) 78_455 . . . ? C35 Co2 C32 C31 -66.4(10) 60_554 . . . ? C35 Co2 C32 C31 38.0 . . . . ? C35 Co2 C32 C31 -142.0(10) 145_565 . . . ? C23 Co2 C32 C37 141.1(7) 78_455 . . . ? C23 Co2 C32 C37 158.3(10) 145_565 . . . ? C23 Co2 C32 C37 -38.9(9) 126_655 . . . ? C23 Co2 C32 C37 53.9(5) 108_566 . . . ? C23 Co2 C32 C37 -21.7 . . . . ? C23 Co2 C32 C37 -126.1(10) 60_554 . . . ? C35 Co2 C32 C37 141.0(9) 126_655 . . . ? C35 Co2 C32 C37 -126.1(5) 108_566 . . . ? C35 Co2 C32 C37 -39.0(7) 78_455 . . . ? C35 Co2 C32 C37 53.9(10) 60_554 . . . ? C35 Co2 C32 C37 158.3 . . . . ? C35 Co2 C32 C37 -21.7(10) 145_565 . . . ? C31 C32 C33 C34 0.0 . . . . ? C37 C32 C33 C34 -176.6 . . . . ? Co2 C32 C33 C34 58.7 . . . . ? C31 C32 C33 C38 176.6 . . . . ? C37 C32 C33 C38 0.0 . . . . ? Co2 C32 C33 C38 -124.7 . . . . ? C31 C32 C33 Co2 -58.7 . . . . ? C37 C32 C33 Co2 124.7 . . . . ? C23 Co2 C33 C32 117.2(3) 78_455 . . . ? C23 Co2 C33 C32 81.6(9) 145_565 . . . ? C23 Co2 C33 C32 -62.8(11) 126_655 . . . ? C23 Co2 C33 C32 -16.1(17) 108_566 . . . ? C23 Co2 C33 C32 -98.4 . . . . ? C23 Co2 C33 C32 164(2) 60_554 . . . ? C35 Co2 C33 C32 117.2(11) 126_655 . . . ? C35 Co2 C33 C32 163.9(17) 108_566 . . . ? C35 Co2 C33 C32 -62.8(3) 78_455 . . . ? C35 Co2 C33 C32 -16(2) 60_554 . . . ? C35 Co2 C33 C32 81.6 . . . . ? C35 Co2 C33 C32 -98.4(9) 145_565 . . . ? C23 Co2 C33 C34 -2.4(3) 78_455 . . . ? C23 Co2 C33 C34 -38.0(9) 145_565 . . . ? C23 Co2 C33 C34 177.6(11) 126_655 . . . ? C23 Co2 C33 C34 -135.7(17) 108_566 . . . ? C23 Co2 C33 C34 142.0 . . . . ? C23 Co2 C33 C34 44(2) 60_554 . . . ? C35 Co2 C33 C34 -2.4(11) 126_655 . . . ? C35 Co2 C33 C34 44.3(17) 108_566 . . . ? C35 Co2 C33 C34 177.6(3) 78_455 . . . ? C35 Co2 C33 C34 -136(2) 60_554 . . . ? C35 Co2 C33 C34 -38.0 . . . . ? C35 Co2 C33 C34 142.0(9) 145_565 . . . ? C23 Co2 C33 C38 -122.6(3) 78_455 . . . ? C23 Co2 C33 C38 -158.2(9) 145_565 . . . ? C23 Co2 C33 C38 57.4(11) 126_655 . . . ? C23 Co2 C33 C38 104.1(17) 108_566 . . . ? C23 Co2 C33 C38 21.8 . . . . ? C23 Co2 C33 C38 -76(2) 60_554 . . . ? C35 Co2 C33 C38 -122.6(11) 126_655 . . . ? C35 Co2 C33 C38 -75.9(17) 108_566 . . . ? C35 Co2 C33 C38 57.4(3) 78_455 . . . ? C35 Co2 C33 C38 104(2) 60_554 . . . ? C35 Co2 C33 C38 -158.2 . . . . ? C35 Co2 C33 C38 21.8(9) 145_565 . . . ? C32 C33 C34 C35 0.4 . . . . ? C38 C33 C34 C35 -176.2 . . . . ? Co2 C33 C34 C35 59.5 . . . . ? C32 C33 C34 C39 179.4 . . . . ? C38 C33 C34 C39 2.9 . . . . ? Co2 C33 C34 C39 -121.5 . . . . ? C32 C33 C34 Co2 -59.1 . . . . ? C38 C33 C34 Co2 124.4 . . . . ? C23 Co2 C34 C35 59.2(3) 78_455 . . . ? C23 Co2 C34 C35 0.0(15) 145_565 . . . ? C23 Co2 C34 C35 -120.8(9) 126_655 . . . ? C23 Co2 C34 C35 34(2) 108_566 . . . ? C23 Co2 C34 C35 180.0 . . . . ? C23 Co2 C34 C35 -146.2(2) 60_554 . . . ? C35 Co2 C34 C35 59.2(9) 126_655 . . . ? C35 Co2 C34 C35 -146(2) 108_566 . . . ? C35 Co2 C34 C35 -120.8(3) 78_455 . . . ? C35 Co2 C34 C35 33.8(2) 60_554 . . . ? C35 Co2 C34 C35 180.0(15) 145_565 . . . ? C23 Co2 C34 C33 178.1(3) 78_455 . . . ? C23 Co2 C34 C33 118.9(15) 145_565 . . . ? C23 Co2 C34 C33 -1.9(9) 126_655 . . . ? C23 Co2 C34 C33 153(2) 108_566 . . . ? C23 Co2 C34 C33 -61.1 . . . . ? C23 Co2 C34 C33 -27.3(2) 60_554 . . . ? C35 Co2 C34 C33 178.1(9) 126_655 . . . ? C35 Co2 C34 C33 -27(2) 108_566 . . . ? C35 Co2 C34 C33 -1.9(3) 78_455 . . . ? C35 Co2 C34 C33 152.7(2) 60_554 . . . ? C35 Co2 C34 C33 118.9 . . . . ? C35 Co2 C34 C33 -61.1(15) 145_565 . . . ? C23 Co2 C34 C39 -61.2(3) 78_455 . . . ? C23 Co2 C34 C39 -120.4(15) 145_565 . . . ? C23 Co2 C34 C39 118.8(9) 126_655 . . . ? C23 Co2 C34 C39 -87(2) 108_566 . . . ? C23 Co2 C34 C39 59.6 . . . . ? C23 Co2 C34 C39 93.4(2) 60_554 . . . ? C35 Co2 C34 C39 -61.2(9) 126_655 . . . ? C35 Co2 C34 C39 93(2) 108_566 . . . ? C35 Co2 C34 C39 118.8(3) 78_455 . . . ? C35 Co2 C34 C39 -86.6(2) 60_554 . . . ? C35 Co2 C34 C39 -120.4 . . . . ? C35 Co2 C34 C39 59.6(15) 145_565 . . . ? C32 C31 C35 C34 0.7 . . . . ? C36 C31 C35 C34 179.7 . . . . ? Co2 C31 C35 C34 -59.1 . . . . ? C32 C31 C35 C40 -176.6 . . . . ? C36 C31 C35 C40 2.5 . . . . ? Co2 C31 C35 C40 123.6 . . . . ? C32 C31 C35 Co2 59.8 . . . . ? C36 C31 C35 Co2 -121.2 . . . . ? C33 C34 C35 C31 -0.7 . . . . ? C39 C34 C35 C31 -179.7 . . . . ? Co2 C34 C35 C31 59.1 . . . . ? C33 C34 C35 C40 176.6 . . . . ? C39 C34 C35 C40 -2.4 . . . . ? Co2 C34 C35 C40 -123.6 . . . . ? C33 C34 C35 Co2 -59.8 . . . . ? C39 C34 C35 Co2 121.2 . . . . ? C23 Co2 C35 C31 128.6(3) 78_455 . . . ? C23 Co2 C35 C31 -51.4(9) 126_655 . . . ? C23 Co2 C35 C31 77.8(10) 108_566 . . . ? C23 Co2 C35 C31 -102.2(3) 60_554 . . . ? C35 Co2 C35 C31 128.6(9) 126_655 . . . ? C35 Co2 C35 C31 -102.2(10) 108_566 . . . ? C35 Co2 C35 C31 -51.4(3) 78_455 . . . ? C35 Co2 C35 C31 77.8(3) 60_554 . . . ? C23 Co2 C35 C34 -111.7(3) 78_455 . . . ? C23 Co2 C35 C34 68.3(9) 126_655 . . . ? C23 Co2 C35 C34 -162.5(10) 108_566 . . . ? C23 Co2 C35 C34 17.5(3) 60_554 . . . ? C35 Co2 C35 C34 -111.7(9) 126_655 . . . ? C35 Co2 C35 C34 17.5(10) 108_566 . . . ? C35 Co2 C35 C34 68.3(3) 78_455 . . . ? C35 Co2 C35 C34 -162.5(3) 60_554 . . . ? C23 Co2 C35 C40 8.5(3) 78_455 . . . ? C23 Co2 C35 C40 -171.5(9) 126_655 . . . ? C23 Co2 C35 C40 -42.4(10) 108_566 . . . ? C23 Co2 C35 C40 137.6(3) 60_554 . . . ? C35 Co2 C35 C40 8.5(9) 126_655 . . . ? C35 Co2 C35 C40 137.6(10) 108_566 . . . ? C35 Co2 C35 C40 -171.5(3) 78_455 . . . ? C35 Co2 C35 C40 -42.4(3) 60_554 . . . ? O002 Ga01 O001 C001 23(3) 83_455 . . . ? O002 Ga01 O001 C001 -81.9(7) 32_545 . . . ? O002 Ga01 O001 C001 7.0(7) . . . . ? O001 Ga01 O001 C001 -166.8(7) 32_545 . . . ? O001 Ga01 O001 C001 99.2(8) 83_455 . . . ? K1 Ga01 O001 C001 -77.0(8) 83_455 . . . ? K1 Ga01 O001 C001 10.3(8) . . . . ? K1 Ga01 O001 C001 -42.9(7) 32_545 . . . ? O002 Ga01 O002 C002 176.3(8) 83_455 . . . ? O002 Ga01 O002 C002 87.1(9) 32_545 . . . ? O001 Ga01 O002 C002 -5.4(7) . . . . ? O001 Ga01 O002 C002 -99.0(7) 83_455 . . . ? K1 Ga01 O002 C002 136.9(7) 83_455 . . . ? K1 Ga01 O002 C002 178.9(10) . . . . ? K1 Ga01 O002 C002 85.0(8) 32_545 . . . ? O002 Ga01 O002 K1 -91.79(12) 32_545 . . . ? O001 Ga01 O002 K1 82.1(4) 83_455 . . . ? K1 Ga01 O002 K1 -41.9(3) 83_455 . . . ? K1 Ga01 O002 K1 -93.9(4) 32_545 . . . ? O002 Ga01 O002 K1 91.35(10) 83_455 . . 32_545 ? O002 Ga01 O002 K1 2.1(3) 32_545 . . 32_545 ? O001 Ga01 O002 K1 -90.4(3) . . . 32_545 ? O001 Ga01 O002 K1 176.1(3) 83_455 . . 32_545 ? K1 Ga01 O002 K1 52.0(3) 83_455 . . 32_545 ? K1 Ga01 O002 K1 93.9(4) . . . 32_545 ? Ga01 O001 C001 C006 174.7(10) . . . . ? Ga01 O001 C001 C002 -7.3(11) . . . . ? C006 C001 C002 C003 1.9(14) . . . . ? O001 C001 C002 C003 -176.2(10) . . . . ? C006 C001 C002 O002 -179.0(12) . . . . ? O001 C001 C002 O002 2.9(13) . . . . ? C006 C001 C002 K1 -100.2(12) . . . 32_545 ? O001 C001 C002 K1 81.8(9) . . . 32_545 ? Ga01 O002 C002 C001 2.9(12) . . . . ? K1 O002 C002 C001 -178.5(7) . . . . ? K1 O002 C002 C001 101.3(9) 32_545 . . . ? Ga01 O002 C002 C003 -178.0(8) . . . . ? K1 O002 C002 C003 0.5(17) . . . . ? K1 O002 C002 C003 -79.6(10) 32_545 . . . ? Ga01 O002 C002 K1 -98.4(5) . . . 32_545 ? K1 O002 C002 K1 80.1(8) . . . 32_545 ? C001 C002 C003 C004 -0.8(14) . . . . ? O002 C002 C003 C004 -179.9(13) . . . . ? K1 C002 C003 C004 110.6(11) 32_545 . . . ? C001 C002 C003 K1 -111.5(9) . . . 32_545 ? O002 C002 C003 K1 69.5(10) . . . 32_545 ? C002 C003 C004 C005 -1.8(19) . . . . ? K1 C003 C004 C005 75.0(14) 32_545 . . . ? C003 C004 C005 C006 4(2) . . . . ? C002 C001 C006 C005 -0.3(18) . . . . ? O001 C001 C006 C005 177.6(11) . . . . ? C002 C001 C006 C007 168.4(11) . . . . ? O001 C001 C006 C007 -14(2) . . . . ? C004 C005 C006 C001 -3(2) . . . . ? C004 C005 C006 C007 -171.5(12) . . . . ? C009 N001 C007 O003 7(2) . . . . ? C009 N001 C007 C006 177.5(13) . . . . ? C001 C006 C007 N001 14(2) . . . . ? C005 C006 C007 N001 -177.2(12) . . . . ? C001 C006 C007 O003 -175.0(12) . . . . ? C005 C006 C007 O003 -6(2) . . . . ? C007 N001 C009 C010 -29.6(19) . . . . ? C007 N001 C009 C008 151.3(14) . . . . ? C012 C008 C009 N001 -4.4(17) 50_554 . . . ? C008 C008 C009 N001 177.4(8) 50_554 . . . ? C012 C008 C009 C010 176.5(13) 50_554 . . . ? C008 C008 C009 C010 -1.7(11) 50_554 . . . ? N001 C009 C010 C011 179.8(12) . . . . ? C008 C009 C010 C011 -1.1(15) . . . . ? C009 C010 C011 C012 2(2) . . . . ? C010 C011 C012 C008 -1(2) . . . 50_554 ? C002 O002 K1 O2S -111.5(11) . . . . ? Ga01 O002 K1 O2S 67.0(3) . . . . ? K1 O002 K1 O2S -34.39(11) 32_545 . . . ? C002 O002 K1 O002 -111.5(11) . . . 42_644 ? Ga01 O002 K1 O002 67.0(3) . . . 42_644 ? K1 O002 K1 O002 -34.39(11) 32_545 . . 42_644 ? C002 O002 K1 O002 -176.5(11) . . . 83_455 ? Ga01 O002 K1 O002 2.0(3) . . . 83_455 ? K1 O002 K1 O002 -99.4(2) 32_545 . . 83_455 ? C002 O002 K1 O002 -62.2(11) . . . 86 ? Ga01 O002 K1 O002 116.3(4) . . . 86 ? K1 O002 K1 O002 15.0(4) 32_545 . . 86 ? C002 O002 K1 C002 157.3(11) . . . 83_455 ? Ga01 O002 K1 C002 -24.2(4) . . . 83_455 ? K1 O002 K1 C002 -125.6(3) 32_545 . . 83_455 ? C002 O002 K1 C002 -39.3(11) . . . 86 ? Ga01 O002 K1 C002 139.2(4) . . . 86 ? K1 O002 K1 C002 37.8(4) 32_545 . . 86 ? C002 O002 K1 C003 156.4(10) . . . 83_455 ? Ga01 O002 K1 C003 -25.1(4) . . . 83_455 ? K1 O002 K1 C003 -126.5(3) 32_545 . . 83_455 ? C002 O002 K1 C003 -18.3(11) . . . 86 ? Ga01 O002 K1 C003 160.2(4) . . . 86 ? K1 O002 K1 C003 58.8(3) 32_545 . . 86 ? C002 O002 K1 Ga01 -178.5(13) . . . . ? K1 O002 K1 Ga01 -101.4(4) 32_545 . . . ? C002 O002 K1 Ga01 -85.2(10) . . . 86 ? Ga01 O002 K1 Ga01 93.3(3) . . . 86 ? K1 O002 K1 Ga01 -8.1(3) 32_545 . . 86 ? C002 O002 K1 K1 -137.2(10) . . . 83_455 ? Ga01 O002 K1 K1 41.3(3) . . . 83_455 ? K1 O002 K1 K1 -60.09(17) 32_545 . . 83_455 ? O002 Ga01 K1 O2S 81.4(4) 83_455 . . . ? O002 Ga01 K1 O2S -7.1(3) 32_545 . . . ? O002 Ga01 K1 O2S -95.2(4) . . . . ? O001 Ga01 K1 O2S -100.4(3) . . . . ? O001 Ga01 K1 O2S 75.0(4) 32_545 . . . ? O001 Ga01 K1 O2S 167.1(2) 83_455 . . . ? K1 Ga01 K1 O2S 35.75(2) 83_455 . . . ? K1 Ga01 K1 O2S -35.75(2) 32_545 . . . ? O002 Ga01 K1 O002 176.6(5) 83_455 . . . ? O002 Ga01 K1 O002 88.1(3) 32_545 . . . ? O001 Ga01 K1 O002 -5.2(5) . . . . ? O001 Ga01 K1 O002 170.2(5) 32_545 . . . ? O001 Ga01 K1 O002 -97.6(4) 83_455 . . . ? K1 Ga01 K1 O002 131.0(4) 83_455 . . . ? K1 Ga01 K1 O002 59.5(4) 32_545 . . . ? O002 Ga01 K1 O002 52.8(3) 83_455 . . 42_644 ? O002 Ga01 K1 O002 -35.7(3) 32_545 . . 42_644 ? O002 Ga01 K1 O002 -123.9(5) . . . 42_644 ? O001 Ga01 K1 O002 -129.1(3) . . . 42_644 ? O001 Ga01 K1 O002 46.4(5) 32_545 . . 42_644 ? O001 Ga01 K1 O002 138.5(3) 83_455 . . 42_644 ? K1 Ga01 K1 O002 7.1(2) 83_455 . . 42_644 ? K1 Ga01 K1 O002 -64.4(2) 32_545 . . 42_644 ? O002 Ga01 K1 O002 -88.5(3) 32_545 . . 83_455 ? O002 Ga01 K1 O002 -176.6(5) . . . 83_455 ? O001 Ga01 K1 O002 178.2(5) . . . 83_455 ? O001 Ga01 K1 O002 -6.4(5) 32_545 . . 83_455 ? O001 Ga01 K1 O002 85.7(4) 83_455 . . 83_455 ? K1 Ga01 K1 O002 -45.7(4) 83_455 . . 83_455 ? K1 Ga01 K1 O002 -117.2(4) 32_545 . . 83_455 ? O002 Ga01 K1 O002 111.0(5) 83_455 . . 86 ? O002 Ga01 K1 O002 22.5(4) 32_545 . . 86 ? O002 Ga01 K1 O002 -65.6(4) . . . 86 ? O001 Ga01 K1 O002 -70.8(3) . . . 86 ? O001 Ga01 K1 O002 104.6(4) 32_545 . . 86 ? O001 Ga01 K1 O002 -163.2(3) 83_455 . . 86 ? K1 Ga01 K1 O002 65.36(17) 83_455 . . 86 ? K1 Ga01 K1 O002 -6.13(18) 32_545 . . 86 ? O002 Ga01 K1 C002 -36.3(4) 83_455 . . 83_455 ? O002 Ga01 K1 C002 -124.8(4) 32_545 . . 83_455 ? O002 Ga01 K1 C002 147.1(6) . . . 83_455 ? O001 Ga01 K1 C002 141.9(5) . . . 83_455 ? O001 Ga01 K1 C002 -42.7(5) 32_545 . . 83_455 ? O001 Ga01 K1 C002 49.4(4) 83_455 . . 83_455 ? K1 Ga01 K1 C002 -82.0(4) 83_455 . . 83_455 ? K1 Ga01 K1 C002 -153.5(4) 32_545 . . 83_455 ? O002 Ga01 K1 C002 128.1(6) 83_455 . . 86 ? O002 Ga01 K1 C002 39.6(5) 32_545 . . 86 ? O002 Ga01 K1 C002 -48.5(5) . . . 86 ? O001 Ga01 K1 C002 -53.7(4) . . . 86 ? O001 Ga01 K1 C002 121.7(5) 32_545 . . 86 ? O001 Ga01 K1 C002 -146.1(4) 83_455 . . 86 ? K1 Ga01 K1 C002 82.5(3) 83_455 . . 86 ? K1 Ga01 K1 C002 11.0(3) 32_545 . . 86 ? O002 Ga01 K1 C003 -30.6(4) 83_455 . . 83_455 ? O002 Ga01 K1 C003 -119.1(4) 32_545 . . 83_455 ? O002 Ga01 K1 C003 152.8(5) . . . 83_455 ? O001 Ga01 K1 C003 147.6(4) . . . 83_455 ? O001 Ga01 K1 C003 -37.0(5) 32_545 . . 83_455 ? O001 Ga01 K1 C003 55.1(3) 83_455 . . 83_455 ? K1 Ga01 K1 C003 -76.3(3) 83_455 . . 83_455 ? K1 Ga01 K1 C003 -147.7(2) 32_545 . . 83_455 ? O002 Ga01 K1 C003 154.4(5) 83_455 . . 86 ? O002 Ga01 K1 C003 65.9(4) 32_545 . . 86 ? O002 Ga01 K1 C003 -22.2(5) . . . 86 ? O001 Ga01 K1 C003 -27.4(4) . . . 86 ? O001 Ga01 K1 C003 148.0(4) 32_545 . . 86 ? O001 Ga01 K1 C003 -119.8(3) 83_455 . . 86 ? K1 Ga01 K1 C003 108.8(3) 83_455 . . 86 ? K1 Ga01 K1 C003 37.3(3) 32_545 . . 86 ? O002 Ga01 K1 Ga01 81.4(4) 83_455 . . 86 ? O002 Ga01 K1 Ga01 -7.1(3) 32_545 . . 86 ? O002 Ga01 K1 Ga01 -95.2(4) . . . 86 ? O001 Ga01 K1 Ga01 -100.4(3) . . . 86 ? O001 Ga01 K1 Ga01 75.0(4) 32_545 . . 86 ? O001 Ga01 K1 Ga01 167.1(2) 83_455 . . 86 ? K1 Ga01 K1 Ga01 35.75(2) 83_455 . . 86 ? K1 Ga01 K1 Ga01 -35.75(2) 32_545 . . 86 ? O002 Ga01 K1 K1 45.7(4) 83_455 . . 83_455 ? O002 Ga01 K1 K1 -42.9(3) 32_545 . . 83_455 ? O002 Ga01 K1 K1 -131.0(4) . . . 83_455 ? O001 Ga01 K1 K1 -136.2(3) . . . 83_455 ? O001 Ga01 K1 K1 39.2(4) 32_545 . . 83_455 ? O001 Ga01 K1 K1 131.4(2) 83_455 . . 83_455 ? K1 Ga01 K1 K1 -71.49(5) 32_545 . . 83_455 ? O002 K1 O2S K1 -121.8(2) . . . 83_455 ? O002 K1 O2S K1 58.2(2) 42_644 . . 83_455 ? O002 K1 O2S K1 -53.40(16) 83_455 . . 83_455 ? O002 K1 O2S K1 126.60(16) 86 . . 83_455 ? C002 K1 O2S K1 -50.8(2) 83_455 . . 83_455 ? C002 K1 O2S K1 129.2(2) 86 . . 83_455 ? C003 K1 O2S K1 -30.7(2) 83_455 . . 83_455 ? C003 K1 O2S K1 149.3(2) 86 . . 83_455 ? Ga01 K1 O2S K1 -90.0 . . . 83_455 ? Ga01 K1 O2S K1 90.0 86 . . 83_455 ? O002 K1 O2S K1 58.2(2) . . . 32_545 ? O002 K1 O2S K1 -121.8(2) 42_644 . . 32_545 ? O002 K1 O2S K1 126.60(16) 83_455 . . 32_545 ? O002 K1 O2S K1 -53.40(16) 86 . . 32_545 ? C002 K1 O2S K1 129.2(2) 83_455 . . 32_545 ? C002 K1 O2S K1 -50.8(2) 86 . . 32_545 ? C003 K1 O2S K1 149.3(2) 83_455 . . 32_545 ? C003 K1 O2S K1 -30.7(2) 86 . . 32_545 ? Ga01 K1 O2S K1 90.0 . . . 32_545 ? Ga01 K1 O2S K1 -90.0 86 . . 32_545 ? K1 K1 O2S K1 180.0 83_455 . . 32_545 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.79 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.610 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.101 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.390 -0.003 0.065 53022 21816 ' ' _platon_squeeze_details ; ;