# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Bhattacharya, Subrato' _publ_contact_author_email bhatt99@yahoo.com _publ_section_title ; Synthesis and structural studies of an electron deficient hexatitanium cluster dication stabilized by novel tritin anions ; _publ_author_name S.Bhattacharya # Attachment '- monoclinic.cif' data_22mardm _database_code_depnum_ccdc_archive 'CCDC 739034' #TrackingRef '- monoclinic.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'TITANIUM CLUSTER' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H180 Cl12 O16 S20 Sn12 Ti12' _chemical_formula_weight 4800.20 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 '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, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.687(5) _cell_length_b 20.079(5) _cell_length_c 22.800(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 114.560(5) _cell_angle_gamma 90.000(5) _cell_volume 9030(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.765 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4688 _exptl_absorpt_coefficient_mu 2.576 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56900 _diffrn_reflns_av_R_equivalents 0.1757 _diffrn_reflns_av_sigmaI/netI 0.2237 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 28.55 _reflns_number_total 21900 _reflns_number_gt 9048 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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. ; _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^)+(0.0621P)^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 riding-model _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21900 _refine_ls_number_parameters 653 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.2260 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1392 _refine_ls_wR_factor_gt 0.0936 _refine_ls_goodness_of_fit_ref 0.808 _refine_ls_restrained_S_all 0.809 _refine_ls_shift/su_max 1.649 _refine_ls_shift/su_mean 0.122 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 Sn1 Sn 0.49779(8) 0.11797(9) 0.36311(9) 0.0891(6) Uani 1 1 d D . . Sn1' Sn 0.00232(8) 0.11798(9) 0.63686(9) 0.0891(6) Uani 1 1 d . . . Sn3 Sn 0.62513(8) 0.00074(9) 0.17951(9) 0.0929(6) Uani 1 1 d . . . Sn3' Sn -0.12506(8) 0.00090(9) 0.82045(10) 0.0928(6) Uani 1 1 d . . . Sn2 Sn 0.49259(7) -0.00792(8) 0.24198(9) 0.0841(6) Uani 1 1 d D . . Sn2' Sn 0.00735(7) -0.00802(8) 0.75798(9) 0.0842(6) Uani 1 1 d . . . Ti4 Ti 0.75017(19) 0.85570(8) 1.0000(2) 0.0452(4) Uani 1 1 d . . . Ti3 Ti 0.76030(15) 0.74892(17) 1.09641(15) 0.0454(9) Uani 1 1 d . . . Ti1 Ti 0.7500(2) 0.64347(8) 1.0000(2) 0.0489(4) Uani 1 1 d D . . Ti2 Ti 0.85719(15) 0.74951(17) 1.03311(16) 0.0462(9) Uani 1 1 d . . . Ti6 Ti 0.73978(15) 0.74914(17) 0.90370(16) 0.0474(9) Uani 1 1 d . . . Ti5 Ti 0.64279(14) 0.74952(16) 0.96684(16) 0.0439(9) Uani 1 1 d . . . Cl1' Cl 0.0247(3) 0.2349(3) 0.6425(4) 0.117(3) Uani 1 1 d . . . Cl2' Cl -0.0161(3) -0.0278(3) 0.6407(3) 0.107(2) Uani 1 1 d . . . S2 S 0.4661(4) 0.1051(3) 0.2517(4) 0.113(3) Uani 1 1 d . . . Cl1 Cl 0.4754(3) 0.2352(3) 0.3577(4) 0.116(3) Uani 1 1 d . . . Cl2 Cl 0.5159(3) -0.0278(3) 0.3594(3) 0.106(2) Uani 1 1 d . . . S2' S 0.0337(4) 0.1047(3) 0.7484(3) 0.111(3) Uani 1 1 d . . . S4' S -0.1090(3) -0.0307(4) 0.7289(3) 0.134(3) Uani 1 1 d . . . S3 S 0.4809(3) 0.0231(3) 0.1292(3) 0.095(2) Uani 1 1 d . . . H3 H 0.4363 0.0394 0.0788 0.114 Uiso 1 1 calc R . . S5' S -0.0959(3) -0.0832(3) 0.8969(4) 0.109(2) Uani 1 1 d . . . H5' H -0.1124 -0.1360 0.8703 0.163 Uiso 1 1 calc R . . S3' S 0.0194(3) 0.0228(3) 0.8710(3) 0.094(2) Uani 1 1 d . . . H3' H 0.0641 0.0388 0.9214 0.113 Uiso 1 1 calc R . . S4 S 0.6087(3) -0.0312(4) 0.2713(3) 0.139(3) Uani 1 1 d . . . Cl3 Cl 0.7440(3) -0.0217(4) 0.2265(4) 0.138(3) Uani 1 1 d . . . S1' S 0.0862(3) 0.0875(4) 0.6044(4) 0.119(3) Uani 1 1 d . . . H1' H 0.1207 0.1350 0.6068 0.179 Uiso 1 1 calc R . . S5 S 0.5956(3) -0.0831(3) 0.1038(4) 0.109(2) Uani 1 1 d . . . H5 H 0.6304 -0.1310 0.1266 0.163 Uiso 1 1 calc R . . O8 O 0.8067(5) 0.8111(5) 0.9633(5) 0.044(3) Uani 1 1 d . . . O6 O 0.6937(5) 0.6874(5) 1.0365(5) 0.047(3) Uani 1 1 d . . . Cl3' Cl -0.2432(3) -0.0220(4) 0.7738(4) 0.138(3) Uani 1 1 d . . . O4 O 0.8068(5) 0.6874(5) 0.9638(5) 0.046(3) Uani 1 1 d . . . S1 S 0.4138(4) 0.0876(4) 0.3949(4) 0.120(3) Uani 1 1 d . . . H1 H 0.4114 0.1272 0.4333 0.180 Uiso 1 1 calc R . . O7 O 0.6824(5) 0.8112(5) 0.9252(5) 0.047(3) Uani 1 1 d . . . O2 O 0.6943(5) 0.8106(5) 1.0366(5) 0.046(3) Uani 1 1 d . . . O1 O 0.8192(4) 0.8106(5) 1.0755(5) 0.042(3) Uani 1 1 d . . . O5 O 0.8185(4) 0.6872(5) 1.0751(5) 0.045(3) Uani 1 1 d . . . O3 O 0.6820(5) 0.6868(5) 0.9250(5) 0.050(3) Uani 1 1 d . . . C17 C 0.7719(16) 0.5427(10) 0.9629(18) 0.150(15) Uani 1 1 d D . . H17 H 0.7895 0.5415 0.9321 0.180 Uiso 1 1 calc R . . C15 C 0.7004(13) 0.5432(11) 1.0088(12) 0.109(8) Uani 1 1 d D . . H15 H 0.6609 0.5439 1.0155 0.131 Uiso 1 1 calc R . . C18 C 0.9536(10) 0.7576(18) 1.0143(11) 0.093(9) Uani 1 1 d . . . H18 H 0.9491 0.7641 0.9723 0.112 Uiso 1 1 calc R . . C33 C 0.5459(9) 0.7504(10) 0.9898(11) 0.086(4) Uani 1 1 d D . . H33 H 0.5489 0.7508 1.0317 0.103 Uiso 1 1 calc R . . C42 C 0.7701(7) 0.7908(8) 0.8239(6) 0.071(2) Uani 1 1 d D . . H42 H 0.8017 0.8249 0.8324 0.085 Uiso 1 1 calc R . . C29 C 0.786(3) 0.9555(14) 0.978(3) 0.17(2) Uani 1 1 d . . . H29 H 0.8168 0.9561 0.9589 0.204 Uiso 1 1 calc R . . C21 C 0.9641(7) 0.7792(16) 1.1111(10) 0.096(9) Uani 1 1 d . . . H21 H 0.9689 0.8013 1.1487 0.115 Uiso 1 1 calc R . . C26 C 0.7586(7) 0.8049(8) 1.1844(6) 0.074(2) Uani 1 1 d D . . H26 H 0.7497 0.8504 1.1821 0.089 Uiso 1 1 calc R . . C22 C 0.9572(8) 0.8060(10) 1.0541(16) 0.096(8) Uani 1 1 d . . . H22 H 0.9553 0.8513 1.0448 0.116 Uiso 1 1 calc R . . C28 C 0.8022(12) 0.9550(11) 1.042(2) 0.140(15) Uani 1 1 d . . . H28 H 0.8452 0.9542 1.0759 0.169 Uiso 1 1 calc R . . C31 C 0.6962(12) 0.9570(10) 0.9906(15) 0.098(8) Uani 1 1 d . . . H31 H 0.6508 0.9589 0.9834 0.117 Uiso 1 1 calc R . . C25 C 0.7112(8) 0.7547(8) 1.1693(7) 0.074(2) Uani 1 1 d D . . H25 H 0.6647 0.7607 1.1551 0.089 Uiso 1 1 calc R . . C34 C 0.5433(8) 0.8057(11) 0.9523(10) 0.086(4) Uani 1 1 d D . . H34 H 0.5459 0.8498 0.9657 0.103 Uiso 1 1 calc R . . C36 C 0.5364(8) 0.7143(10) 0.8921(10) 0.086(4) Uani 1 1 d D . . H36 H 0.5328 0.6864 0.8583 0.103 Uiso 1 1 calc R . . C40 C 0.7237(7) 0.6891(8) 0.8114(6) 0.071(2) Uani 1 1 d D . . H40 H 0.7180 0.6431 0.8103 0.085 Uiso 1 1 calc R . . C32 C 0.7451(15) 0.9559(10) 1.0461(12) 0.098(8) Uani 1 1 d . . . H32 H 0.7400 0.9557 1.0846 0.118 Uiso 1 1 calc R . . C19 C 0.9570(11) 0.6999(17) 1.0402(19) 0.140(15) Uani 1 1 d . . . H19 H 0.9560 0.6588 1.0210 0.168 Uiso 1 1 calc R . . C30 C 0.717(3) 0.9552(12) 0.9458(12) 0.145(16) Uani 1 1 d . . . H30 H 0.6908 0.9540 0.9016 0.174 Uiso 1 1 calc R . . C20 C 0.9623(9) 0.7103(13) 1.1002(15) 0.094(8) Uani 1 1 d . . . H20 H 0.9644 0.6774 1.1297 0.113 Uiso 1 1 calc R . . C38 C 0.7008(7) 0.7984(8) 0.8032(6) 0.071(2) Uani 1 1 d D . . H38 H 0.6774 0.8385 0.7962 0.085 Uiso 1 1 calc R . . C16 C 0.7047(10) 0.5421(9) 0.9513(9) 0.079(6) Uani 1 1 d D . . H16 H 0.6684 0.5412 0.9109 0.095 Uiso 1 1 calc R . . C24 C 0.7441(7) 0.6939(8) 1.1787(6) 0.074(2) Uani 1 1 d D . . H24 H 0.7237 0.6521 1.1711 0.089 Uiso 1 1 calc R . . C35 C 0.5362(8) 0.7850(10) 0.8916(10) 0.086(4) Uani 1 1 d D . . H35 H 0.5322 0.8123 0.8572 0.103 Uiso 1 1 calc R . . C13 C 0.8085(12) 0.5452(10) 1.028(2) 0.22(3) Uani 1 1 d D . . H13 H 0.8553 0.5478 1.0515 0.264 Uiso 1 1 calc R . . C27 C 0.8213(7) 0.7759(8) 1.2035(7) 0.074(2) Uani 1 1 d D . . H27 H 0.8624 0.7980 1.2158 0.089 Uiso 1 1 calc R . . C39 C 0.6735(8) 0.7364(7) 0.7950(7) 0.071(2) Uani 1 1 d D . . H39 H 0.6274 0.7273 0.7804 0.085 Uiso 1 1 calc R . . C23 C 0.8119(7) 0.7067(8) 1.2011(6) 0.074(2) Uani 1 1 d D . . H23 H 0.8460 0.6749 1.2128 0.089 Uiso 1 1 calc R . . C37 C 0.5431(8) 0.6949(11) 0.9531(9) 0.086(4) Uani 1 1 d D . . H37 H 0.5453 0.6510 0.9670 0.103 Uiso 1 1 calc R . . C41 C 0.7840(8) 0.7230(7) 0.8297(7) 0.071(2) Uani 1 1 d D . . H41 H 0.8268 0.7038 0.8435 0.085 Uiso 1 1 calc R . . C14 C 0.761(2) 0.5431(11) 1.0515(11) 0.168(17) Uani 1 1 d D . . H14 H 0.7709 0.5416 1.0954 0.202 Uiso 1 1 calc R . . C1' C -0.0977(8) 0.1185(11) 0.5644(9) 0.115(8) Uani 1 1 d D . . H1'1 H -0.1197 0.0775 0.5673 0.138 Uiso 1 1 calc R . . H1'2 H -0.1221 0.1550 0.5729 0.138 Uiso 1 1 calc R . . C2' C -0.1036(12) 0.1254(19) 0.4965(10) 0.208(16) Uani 1 1 d D . . H2'1 H -0.0812 0.1665 0.4943 0.250 Uiso 1 1 calc R . . H2'2 H -0.0781 0.0893 0.4890 0.250 Uiso 1 1 calc R . . C3' C -0.1697(13) 0.1258(14) 0.4440(15) 0.30(3) Uani 1 1 d D . . H3'1 H -0.1967 0.1615 0.4499 0.361 Uiso 1 1 calc R . . H3'2 H -0.1925 0.0840 0.4428 0.361 Uiso 1 1 calc R . . C4' C -0.163(2) 0.136(3) 0.3805(18) 0.39(4) Uani 1 1 d D . . H4'1 H -0.2069 0.1395 0.3457 0.587 Uiso 0.50 1 calc PR . . H4'2 H -0.1391 0.0986 0.3730 0.587 Uiso 0.50 1 calc PR . . H4'3 H -0.1375 0.1760 0.3829 0.587 Uiso 0.50 1 calc PR . . H4'4 H -0.1155 0.1366 0.3887 0.587 Uiso 0.50 1 calc PR . . H4'5 H -0.1832 0.1774 0.3614 0.587 Uiso 0.50 1 calc PR . . H4'6 H -0.1848 0.1001 0.3515 0.587 Uiso 0.50 1 calc PR . . C5' C 0.0897(18) -0.0749(19) 0.800(2) 0.289(13) Uani 1 1 d D . . H5'1 H 0.1278 -0.0559 0.7935 0.346 Uiso 1 1 calc R . . H5'2 H 0.1021 -0.0756 0.8456 0.346 Uiso 1 1 calc R . . C9' C -0.128(2) 0.103(2) 0.855(2) 0.235(13) Uani 1 1 d . . . H9'1 H -0.0875 0.1278 0.8593 0.281 Uiso 1 1 calc R . . H9'2 H -0.1675 0.1270 0.8246 0.281 Uiso 1 1 calc R . . C11' C -0.137(2) 0.1524(18) 1.0074(18) 0.235(13) Uani 1 1 d D . . H11A H -0.1478 0.1933 1.0228 0.352 Uiso 1 1 calc R . . H11B H -0.0934 0.1370 1.0373 0.352 Uiso 1 1 calc R . . H11C H -0.1707 0.1195 1.0033 0.352 Uiso 1 1 calc R . . C12' C -0.136(2) 0.1640(19) 0.9429(18) 0.235(13) Uani 1 1 d D . . H12A H -0.1768 0.1867 0.9143 0.281 Uiso 1 1 calc R . . H12B H -0.0971 0.1912 0.9476 0.281 Uiso 1 1 calc R . . C1 C 0.5983(15) 0.118(2) 0.4351(13) 0.232(11) Uani 1 1 d D . . H1A H 0.6198 0.0762 0.4328 0.278 Uiso 1 1 calc R . . H1B H 0.6233 0.1536 0.4262 0.278 Uiso 1 1 calc R . . C2 C 0.6027(13) 0.126(2) 0.5013(9) 0.232(11) Uani 1 1 d D . . H2A H 0.5825 0.0871 0.5111 0.278 Uiso 1 1 calc R . . H2B H 0.5743 0.1639 0.5005 0.278 Uiso 1 1 calc R . . C3 C 0.6712(11) 0.1368(18) 0.5574(12) 0.232(11) Uani 1 1 d D . . H3A H 0.6859 0.1824 0.5571 0.278 Uiso 1 1 calc R . . H3B H 0.7045 0.1075 0.5528 0.278 Uiso 1 1 calc R . . C8 C 0.357(2) -0.2471(19) 0.230(2) 0.278(14) Uani 1 1 d . . . H8A H 0.3189 -0.2742 0.2042 0.417 Uiso 1 1 calc R . . H8B H 0.3536 -0.2361 0.2699 0.417 Uiso 1 1 calc R . . H8C H 0.3981 -0.2713 0.2398 0.417 Uiso 1 1 calc R . . C6' C 0.0829(17) -0.1435(18) 0.778(2) 0.289(13) Uani 1 1 d D . . H6'1 H 0.0694 -0.1439 0.7316 0.346 Uiso 1 1 calc R . . H6'2 H 0.0471 -0.1645 0.7862 0.346 Uiso 1 1 calc R . . C7' C 0.1481(17) -0.1849(19) 0.8104(19) 0.289(13) Uani 1 1 d D . . H7'1 H 0.1878 -0.1582 0.8169 0.346 Uiso 1 1 calc R . . H7'2 H 0.1524 -0.2017 0.8518 0.346 Uiso 1 1 calc R . . C8' C 0.1405(19) -0.242(2) 0.7638(19) 0.289(13) Uani 1 1 d D . . H8'1 H 0.1778 -0.2723 0.7830 0.433 Uiso 1 1 calc R . . H8'2 H 0.1402 -0.2245 0.7245 0.433 Uiso 1 1 calc R . . H8'3 H 0.0988 -0.2650 0.7547 0.433 Uiso 1 1 calc R . . C10' C -0.131(2) 0.095(2) 0.915(2) 0.235(13) Uani 1 1 d . . . H10A H -0.0907 0.0723 0.9448 0.281 Uiso 1 1 calc R . . H10B H -0.1702 0.0688 0.9101 0.281 Uiso 1 1 calc R . . C5 C 0.413(2) -0.1350(17) 0.223(2) 0.278(14) Uani 1 1 d D . . H5A H 0.4183 -0.1266 0.2666 0.334 Uiso 1 1 calc R . . H5B H 0.4542 -0.1574 0.2265 0.334 Uiso 1 1 calc R . . C6 C 0.4138(18) -0.0785(18) 0.199(2) 0.278(14) Uani 1 1 d D . . H6A H 0.3719 -0.0565 0.1932 0.334 Uiso 1 1 calc R . . H6B H 0.4109 -0.0866 0.1556 0.334 Uiso 1 1 calc R . . C7 C 0.3571(19) -0.1853(19) 0.195(2) 0.278(14) Uani 1 1 d . . . H7A H 0.3150 -0.1623 0.1869 0.334 Uiso 1 1 calc R . . H7B H 0.3553 -0.1986 0.1536 0.334 Uiso 1 1 calc R . . C9 C 0.6296(18) 0.0968(17) 0.0849(15) 0.236(12) Uani 1 1 d D . . H9A H 0.5910 0.0703 0.0575 0.283 Uiso 1 1 calc R . . H9B H 0.6699 0.0719 0.0901 0.283 Uiso 1 1 calc R . . C10 C 0.6280(18) 0.1009(16) 0.1500(16) 0.236(12) Uani 1 1 d D . . H10C H 0.5881 0.1251 0.1473 0.283 Uiso 1 1 calc R . . H10D H 0.6680 0.1235 0.1805 0.283 Uiso 1 1 calc R . . C11 C 0.6292(18) 0.1582(16) 0.0490(16) 0.236(12) Uani 1 1 d D . . H11D H 0.5848 0.1785 0.0356 0.283 Uiso 1 1 calc R . . H11E H 0.6618 0.1887 0.0790 0.283 Uiso 1 1 calc R . . C12 C 0.6442(17) 0.1537(15) -0.0092(16) 0.236(12) Uani 1 1 d D . . H12C H 0.6364 0.1963 -0.0303 0.354 Uiso 1 1 calc R . . H12D H 0.6152 0.1211 -0.0384 0.354 Uiso 1 1 calc R . . H12E H 0.6907 0.1411 0.0037 0.354 Uiso 1 1 calc R . . C4 C 0.6662(13) 0.1223(19) 0.6223(11) 0.232(11) Uani 1 1 d D . . H4A H 0.7101 0.1271 0.6572 0.348 Uiso 1 1 calc R . . H4B H 0.6502 0.0776 0.6218 0.348 Uiso 1 1 calc R . . H4C H 0.6352 0.1531 0.6278 0.348 Uiso 1 1 calc R . . 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 Sn1 0.0865(12) 0.1038(14) 0.0774(15) 0.0031(11) 0.0345(10) 0.0330(10) Sn1' 0.0866(12) 0.1023(14) 0.0775(15) -0.0024(11) 0.0334(10) -0.0327(10) Sn3 0.0949(12) 0.0919(14) 0.0893(16) -0.0098(12) 0.0357(10) 0.0284(10) Sn3' 0.0948(12) 0.0895(14) 0.0896(16) 0.0098(11) 0.0337(10) -0.0292(10) Sn2 0.0930(12) 0.0811(12) 0.0702(14) 0.0074(10) 0.0260(9) 0.0279(9) Sn2' 0.0918(12) 0.0810(12) 0.0715(14) -0.0082(10) 0.0258(9) -0.0284(9) Ti4 0.0535(9) 0.0463(9) 0.0399(9) -0.001(3) 0.0235(7) 0.000(2) Ti3 0.055(2) 0.056(2) 0.026(2) 0.0000(19) 0.0176(16) -0.0029(17) Ti1 0.0573(9) 0.0432(9) 0.0392(9) 0.001(3) 0.0130(7) 0.001(2) Ti2 0.048(2) 0.056(2) 0.035(2) -0.004(2) 0.0175(16) -0.0008(17) Ti6 0.056(2) 0.057(2) 0.030(2) -0.001(2) 0.0195(16) 0.0006(18) Ti5 0.0458(19) 0.052(2) 0.034(2) 0.002(2) 0.0169(16) -0.0021(17) Cl1' 0.132(5) 0.107(5) 0.103(6) 0.007(5) 0.042(4) -0.039(4) Cl2' 0.130(5) 0.105(5) 0.081(6) -0.026(4) 0.039(4) -0.037(4) S2 0.163(6) 0.099(5) 0.087(6) 0.024(5) 0.063(5) 0.064(5) Cl1 0.130(5) 0.103(5) 0.110(7) -0.002(5) 0.045(5) 0.037(4) Cl2 0.139(5) 0.106(5) 0.078(6) 0.028(4) 0.049(4) 0.035(4) S2' 0.174(7) 0.094(5) 0.080(6) -0.027(4) 0.068(5) -0.067(5) S4' 0.112(5) 0.217(9) 0.064(6) -0.017(6) 0.026(4) -0.095(5) S3 0.088(4) 0.132(6) 0.054(5) 0.015(4) 0.019(3) 0.045(4) S5' 0.123(5) 0.109(6) 0.103(7) 0.025(5) 0.055(5) -0.019(4) S3' 0.087(4) 0.127(6) 0.059(5) -0.007(4) 0.022(3) -0.041(4) S4 0.120(6) 0.221(9) 0.066(6) 0.015(6) 0.029(4) 0.100(6) Cl3 0.087(4) 0.134(6) 0.177(9) -0.016(6) 0.038(5) 0.030(4) S1' 0.115(5) 0.142(6) 0.123(7) 0.006(6) 0.073(5) -0.021(5) S5 0.119(5) 0.113(6) 0.105(7) -0.028(5) 0.057(5) 0.019(4) O8 0.051(6) 0.053(8) 0.028(8) -0.001(7) 0.016(5) 0.000(6) O6 0.047(6) 0.062(8) 0.032(8) 0.003(7) 0.015(5) -0.008(6) Cl3' 0.086(4) 0.145(7) 0.164(8) 0.016(6) 0.032(4) -0.028(4) O4 0.058(7) 0.050(8) 0.034(8) -0.007(7) 0.023(6) 0.014(6) S1 0.119(5) 0.150(7) 0.122(8) -0.013(6) 0.080(5) 0.012(5) O7 0.054(7) 0.056(8) 0.035(9) 0.004(7) 0.022(6) 0.010(6) O2 0.052(7) 0.057(8) 0.035(8) 0.000(7) 0.023(6) 0.009(6) O1 0.046(6) 0.048(8) 0.029(8) 0.001(6) 0.014(5) 0.000(6) O5 0.048(6) 0.053(8) 0.029(8) 0.001(6) 0.011(5) -0.005(6) O3 0.060(7) 0.048(8) 0.034(9) 0.001(7) 0.013(6) -0.008(6) C17 0.24(3) 0.024(11) 0.31(4) -0.05(2) 0.24(3) -0.033(16) C15 0.15(2) 0.088(17) 0.106(18) -0.019(15) 0.072(17) -0.046(15) C18 0.058(10) 0.19(3) 0.051(10) 0.012(17) 0.042(8) -0.024(16) C33 0.058(5) 0.114(9) 0.072(7) 0.000(7) 0.014(5) 0.000(6) C42 0.090(5) 0.098(6) 0.033(4) 0.002(4) 0.033(3) 0.000(4) C29 0.28(4) 0.044(14) 0.34(6) 0.01(3) 0.29(5) -0.02(2) C21 0.026(7) 0.21(3) 0.043(10) -0.046(13) 0.004(7) 0.000(10) C26 0.089(5) 0.109(6) 0.030(4) 0.006(4) 0.030(3) -0.008(5) C22 0.052(9) 0.050(10) 0.16(2) -0.023(13) 0.022(12) -0.019(8) C28 0.044(12) 0.041(12) 0.26(4) -0.01(2) -0.015(16) -0.011(9) C31 0.100(17) 0.049(13) 0.12(2) 0.007(14) 0.021(16) 0.017(10) C25 0.089(5) 0.109(6) 0.030(4) 0.006(4) 0.030(3) -0.008(5) C34 0.058(5) 0.114(9) 0.072(7) 0.000(7) 0.014(5) 0.000(6) C36 0.058(5) 0.114(9) 0.072(7) 0.000(7) 0.014(5) 0.000(6) C40 0.090(5) 0.098(6) 0.033(4) 0.002(4) 0.033(3) 0.000(4) C32 0.16(2) 0.060(14) 0.053(16) -0.003(11) 0.028(14) 0.026(14) C19 0.058(11) 0.15(3) 0.20(3) -0.13(3) 0.044(18) -0.014(14) C30 0.32(5) 0.051(14) 0.038(13) 0.021(11) 0.05(2) 0.02(2) C20 0.050(9) 0.082(14) 0.13(2) 0.069(14) 0.022(11) 0.022(10) C38 0.090(5) 0.098(6) 0.033(4) 0.002(4) 0.033(3) 0.000(4) C16 0.095(14) 0.062(13) 0.049(12) -0.017(9) -0.001(9) -0.028(10) C24 0.089(5) 0.109(6) 0.030(4) 0.006(4) 0.030(3) -0.008(5) C35 0.058(5) 0.114(9) 0.072(7) 0.000(7) 0.014(5) 0.000(6) C13 0.076(14) 0.033(13) 0.43(7) -0.03(3) -0.02(3) 0.006(11) C27 0.089(5) 0.109(6) 0.030(4) 0.006(4) 0.030(3) -0.008(5) C39 0.090(5) 0.098(6) 0.033(4) 0.002(4) 0.033(3) 0.000(4) C23 0.089(5) 0.109(6) 0.030(4) 0.006(4) 0.030(3) -0.008(5) C37 0.058(5) 0.114(9) 0.072(7) 0.000(7) 0.014(5) 0.000(6) C41 0.090(5) 0.098(6) 0.033(4) 0.002(4) 0.033(3) 0.000(4) C14 0.31(4) 0.045(15) 0.049(14) 0.011(11) -0.02(2) -0.04(2) C1' 0.073(11) 0.116(15) 0.114(18) 0.015(13) -0.003(10) -0.051(10) C2' 0.15(2) 0.32(4) 0.085(19) 0.04(2) -0.019(15) -0.11(2) C3' 0.21(3) 0.15(2) 0.28(4) 0.14(3) -0.16(3) -0.07(2) C4' 0.43(7) 0.55(10) 0.14(4) 0.15(5) 0.06(4) 0.14(6) C5' 0.24(2) 0.29(3) 0.22(3) -0.03(2) -0.015(18) 0.08(2) C9' 0.270(16) 0.136(16) 0.32(4) 0.00(3) 0.14(3) -0.054(14) C11' 0.270(16) 0.136(16) 0.32(4) 0.00(3) 0.14(3) -0.054(14) C12' 0.270(16) 0.136(16) 0.32(4) 0.00(3) 0.14(3) -0.054(14) C1 0.175(14) 0.271(19) 0.17(2) 0.05(2) -0.005(14) 0.053(13) C2 0.175(14) 0.271(19) 0.17(2) 0.05(2) -0.005(14) 0.053(13) C3 0.175(14) 0.271(19) 0.17(2) 0.05(2) -0.005(14) 0.053(13) C8 0.27(2) 0.21(3) 0.25(3) 0.00(2) 0.01(2) -0.12(2) C6' 0.24(2) 0.29(3) 0.22(3) -0.03(2) -0.015(18) 0.08(2) C7' 0.24(2) 0.29(3) 0.22(3) -0.03(2) -0.015(18) 0.08(2) C8' 0.24(2) 0.29(3) 0.22(3) -0.03(2) -0.015(18) 0.08(2) C10' 0.270(16) 0.136(16) 0.32(4) 0.00(3) 0.14(3) -0.054(14) C5 0.27(2) 0.21(3) 0.25(3) 0.00(2) 0.01(2) -0.12(2) C6 0.27(2) 0.21(3) 0.25(3) 0.00(2) 0.01(2) -0.12(2) C7 0.27(2) 0.21(3) 0.25(3) 0.00(2) 0.01(2) -0.12(2) C9 0.245(16) 0.140(14) 0.39(4) 0.06(2) 0.20(2) 0.064(13) C10 0.245(16) 0.140(14) 0.39(4) 0.06(2) 0.20(2) 0.064(13) C11 0.245(16) 0.140(14) 0.39(4) 0.06(2) 0.20(2) 0.064(13) C12 0.245(16) 0.140(14) 0.39(4) 0.06(2) 0.20(2) 0.064(13) C4 0.175(14) 0.271(19) 0.17(2) 0.05(2) -0.005(14) 0.053(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Sn1 C1 2.11(3) . ? Sn1 S1 2.305(7) . ? Sn1 S2 2.353(8) . ? Sn1 Cl1 2.395(7) . ? Sn1' C1' 2.111(16) . ? Sn1' S1' 2.313(8) . ? Sn1' S2' 2.359(7) . ? Sn1' Cl1' 2.390(7) . ? Sn3 C10 2.13(3) . ? Sn3 S5 2.303(7) . ? Sn3 S4 2.352(8) . ? Sn3 Cl3 2.387(6) . ? Sn3 S3 2.884(6) . ? Sn3' C9' 2.21(4) . ? Sn3' S5' 2.317(7) . ? Sn3' S4' 2.343(8) . ? Sn3' Cl3' 2.376(6) . ? Sn3' S3' 2.887(6) . ? Sn2 C6 2.122(17) . ? Sn2 S4 2.369(6) . ? Sn2 S2 2.374(7) . ? Sn2 Cl2 2.541(7) . ? Sn2 S3 2.555(7) . ? Sn2' C5' 2.12(3) . ? Sn2' S2' 2.367(7) . ? Sn2' S4' 2.370(6) . ? Sn2' Cl2' 2.538(7) . ? Sn2' S3' 2.555(7) . ? Ti4 O7 1.946(11) . ? Ti4 O2 1.955(12) . ? Ti4 O8 1.964(11) . ? Ti4 O1 1.969(10) . ? Ti4 C29 2.28(2) . ? Ti4 C32 2.29(2) . ? Ti4 C28 2.30(2) . ? Ti4 C30 2.30(2) . ? Ti4 C31 2.31(2) . ? Ti4 Ti6 3.007(5) . ? Ti4 Ti2 3.008(4) . ? Ti4 Ti5 3.013(4) . ? Ti3 O2 1.955(11) . ? Ti3 O6 1.959(10) . ? Ti3 O5 1.968(11) . ? Ti3 O1 1.975(11) . ? Ti3 C27 2.307(14) . ? Ti3 C26 2.313(15) . ? Ti3 C25 2.319(15) . ? Ti3 C24 2.326(15) . ? Ti3 C23 2.334(14) . ? Ti3 Ti1 2.993(5) . ? Ti3 Ti5 2.994(4) . ? Ti3 Ti2 3.003(5) . ? Ti1 O3 1.939(11) . ? Ti1 O5 1.948(10) . ? Ti1 O6 1.950(12) . ? Ti1 O4 1.954(12) . ? Ti1 C13 2.289(16) . ? Ti1 C14 2.30(2) . ? Ti1 C17 2.32(2) . ? Ti1 C16 2.331(17) . ? Ti1 C15 2.33(2) . ? Ti1 Ti6 2.995(5) . ? Ti1 Ti5 3.008(4) . ? Ti2 O1 1.944(11) . ? Ti2 O8 1.952(11) . ? Ti2 O4 1.953(11) . ? Ti2 O5 1.964(11) . ? Ti2 C20 2.293(16) . ? Ti2 C18 2.308(18) . ? Ti2 C22 2.314(17) . ? Ti2 C19 2.33(2) . ? Ti2 C21 2.338(16) . ? Ti2 Ti6 2.991(4) . ? Ti6 O7 1.961(11) . ? Ti6 O8 1.964(10) . ? Ti6 O4 1.968(10) . ? Ti6 O3 1.969(11) . ? Ti6 C39 2.305(14) . ? Ti6 C38 2.309(14) . ? Ti6 C41 2.322(15) . ? Ti6 C40 2.323(15) . ? Ti6 C42 2.331(15) . ? Ti6 Ti5 3.002(5) . ? Ti5 O2 1.950(11) . ? Ti5 O6 1.960(11) . ? Ti5 O7 1.963(12) . ? Ti5 O3 1.974(12) . ? Ti5 C37 2.327(19) . ? Ti5 C34 2.333(19) . ? Ti5 C36 2.336(18) . ? Ti5 C35 2.344(18) . ? Ti5 C33 2.37(2) . ? S3 H3 1.2000 . ? S5' H5' 1.2000 . ? S3' H3' 1.2000 . ? S1' H1' 1.2001 . ? S5 H5 1.2000 . ? S1 H1 1.2000 . ? C17 C16 1.369(17) . ? C17 C13 1.371(18) . ? C17 H17 0.9300 . ? C15 C14 1.26(3) . ? C15 C16 1.353(17) . ? C15 H15 0.9300 . ? C18 C19 1.29(3) . ? C18 C22 1.31(3) . ? C18 H18 0.9300 . ? C33 C37 1.381(16) . ? C33 C34 1.388(16) . ? C33 H33 0.9300 . ? C42 C38 1.384(14) . ? C42 C41 1.388(15) . ? C42 H42 0.9300 . ? C29 C28 1.36(4) . ? C29 C30 1.37(4) . ? C29 H29 0.9300 . ? C21 C22 1.36(3) . ? C21 C20 1.40(3) . ? C21 H21 0.9300 . ? C26 C27 1.374(14) . ? C26 C25 1.377(14) . ? C26 H26 0.9300 . ? C22 H22 0.9300 . ? C28 C32 1.28(3) . ? C28 H28 0.9300 . ? C31 C32 1.27(3) . ? C31 C30 1.27(4) . ? C31 H31 0.9300 . ? C25 C24 1.385(15) . ? C25 H25 0.9300 . ? C34 C35 1.392(16) . ? C34 H34 0.9300 . ? C36 C37 1.393(16) . ? C36 C35 1.419(16) . ? C36 H36 0.9300 . ? C40 C39 1.375(14) . ? C40 C41 1.378(14) . ? C40 H40 0.9300 . ? C32 H32 0.9300 . ? C19 C20 1.34(3) . ? C19 H19 0.9300 . ? C30 H30 0.9300 . ? C20 H20 0.9300 . ? C38 C39 1.358(14) . ? C38 H38 0.9300 . ? C16 H16 0.9300 . ? C24 C23 1.365(14) . ? C24 H24 0.9300 . ? C35 H35 0.9300 . ? C13 C14 1.347(18) . ? C13 H13 0.9300 . ? C27 C23 1.401(15) . ? C27 H27 0.9300 . ? C39 H39 0.9300 . ? C23 H23 0.9300 . ? C37 H37 0.9300 . ? C41 H41 0.9300 . ? C14 H14 0.9300 . ? C1' C2' 1.504(16) . ? C1' H1'1 0.9700 . ? C1' H1'2 0.9700 . ? C2' C3' 1.44(2) . ? C2' H2'1 0.9700 . ? C2' H2'2 0.9700 . ? C3' C4' 1.531(19) . ? C3' H3'1 0.9700 . ? C3' H3'2 0.9700 . ? C4' H4'1 0.9600 . ? C4' H4'2 0.9600 . ? C4' H4'3 0.9600 . ? C4' H4'4 0.9600 . ? C4' H4'5 0.9600 . ? C4' H4'6 0.9600 . ? C5' C6' 1.450(19) . ? C5' H5'1 0.9700 . ? C5' H5'2 0.9700 . ? C9' C10' 1.42(5) . ? C9' H9'1 0.9700 . ? C9' H9'2 0.9700 . ? C11' C12' 1.499(19) . ? C11' H11A 0.9600 . ? C11' H11B 0.9600 . ? C11' H11C 0.9600 . ? C12' C10' 1.54(6) . ? C12' H12A 0.9700 . ? C12' H12B 0.9700 . ? C1 C2 1.483(18) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.519(13) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.556(18) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C8 C7 1.48(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C6' C7' 1.539(18) . ? C6' H6'1 0.9700 . ? C6' H6'2 0.9700 . ? C7' C8' 1.524(19) . ? C7' H7'1 0.9700 . ? C7' H7'2 0.9700 . ? C8' H8'1 0.9600 . ? C8' H8'2 0.9600 . ? C8' H8'3 0.9600 . ? C10' H10A 0.9700 . ? C10' H10B 0.9700 . ? C5 C6 1.26(4) . ? C5 C7 1.50(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C10 1.503(19) . ? C9 C11 1.48(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10C 0.9700 . ? C10 H10D 0.9700 . ? C11 C12 1.494(18) . ? C11 H11D 0.9700 . ? C11 H11E 0.9700 . ? C12 H12C 0.9600 . ? C12 H12D 0.9600 . ? C12 H12E 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? 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 C1 Sn1 S1 116.8(9) . . ? C1 Sn1 S2 125.6(8) . . ? S1 Sn1 S2 113.3(3) . . ? C1 Sn1 Cl1 99.3(11) . . ? S1 Sn1 Cl1 96.1(3) . . ? S2 Sn1 Cl1 95.2(3) . . ? C1' Sn1' S1' 116.1(7) . . ? C1' Sn1' S2' 126.0(6) . . ? S1' Sn1' S2' 113.7(3) . . ? C1' Sn1' Cl1' 99.0(6) . . ? S1' Sn1' Cl1' 96.2(3) . . ? S2' Sn1' Cl1' 95.3(3) . . ? C10 Sn3 S5 119.3(9) . . ? C10 Sn3 S4 125.0(8) . . ? S5 Sn3 S4 111.6(3) . . ? C10 Sn3 Cl3 98.8(10) . . ? S5 Sn3 Cl3 96.4(3) . . ? S4 Sn3 Cl3 94.8(3) . . ? C10 Sn3 S3 84.0(9) . . ? S5 Sn3 S3 84.1(2) . . ? S4 Sn3 S3 81.8(2) . . ? Cl3 Sn3 S3 176.4(3) . . ? C9' Sn3' S5' 116.9(12) . . ? C9' Sn3' S4' 127.0(12) . . ? S5' Sn3' S4' 112.2(3) . . ? C9' Sn3' Cl3' 98.9(11) . . ? S5' Sn3' Cl3' 95.9(3) . . ? S4' Sn3' Cl3' 94.7(3) . . ? C9' Sn3' S3' 84.4(11) . . ? S5' Sn3' S3' 84.2(2) . . ? S4' Sn3' S3' 81.8(2) . . ? Cl3' Sn3' S3' 176.2(3) . . ? C6 Sn2 S4 123.7(14) . . ? C6 Sn2 S2 120.2(13) . . ? S4 Sn2 S2 115.7(3) . . ? C6 Sn2 Cl2 98.9(14) . . ? S4 Sn2 Cl2 87.1(2) . . ? S2 Sn2 Cl2 90.1(2) . . ? C6 Sn2 S3 88.3(14) . . ? S4 Sn2 S3 88.9(2) . . ? S2 Sn2 S3 86.2(2) . . ? Cl2 Sn2 S3 172.8(2) . . ? C5' Sn2' S2' 117.2(12) . . ? C5' Sn2' S4' 127.2(13) . . ? S2' Sn2' S4' 115.3(3) . . ? C5' Sn2' Cl2' 97.8(12) . . ? S2' Sn2' Cl2' 90.2(2) . . ? S4' Sn2' Cl2' 87.2(2) . . ? C5' Sn2' S3' 89.3(12) . . ? S2' Sn2' S3' 86.2(2) . . ? S4' Sn2' S3' 88.9(2) . . ? Cl2' Sn2' S3' 172.9(2) . . ? O7 Ti4 O2 77.6(5) . . ? O7 Ti4 O8 78.1(4) . . ? O2 Ti4 O8 125.3(2) . . ? O7 Ti4 O1 125.3(2) . . ? O2 Ti4 O1 78.2(4) . . ? O8 Ti4 O1 77.3(4) . . ? O7 Ti4 C29 114.3(18) . . ? O2 Ti4 C29 146.2(8) . . ? O8 Ti4 C29 88.5(8) . . ? O1 Ti4 C29 113.0(18) . . ? O7 Ti4 C32 130.0(8) . . ? O2 Ti4 C32 93.2(8) . . ? O8 Ti4 C32 138.8(9) . . ? O1 Ti4 C32 99.6(7) . . ? C29 Ti4 C32 54.4(10) . . ? O7 Ti4 C28 145.8(9) . . ? O2 Ti4 C28 120.5(14) . . ? O8 Ti4 C28 106.8(12) . . ? O1 Ti4 C28 88.3(8) . . ? C29 Ti4 C28 34.6(11) . . ? C32 Ti4 C28 32.4(9) . . ? O7 Ti4 C30 88.5(9) . . ? O2 Ti4 C30 121.2(14) . . ? O8 Ti4 C30 106.2(13) . . ? O1 Ti4 C30 145.4(11) . . ? C29 Ti4 C30 34.8(11) . . ? C32 Ti4 C30 54.5(7) . . ? C28 Ti4 C30 57.4(10) . . ? O7 Ti4 C31 98.9(7) . . ? O2 Ti4 C31 93.9(8) . . ? O8 Ti4 C31 138.0(9) . . ? O1 Ti4 C31 131.1(8) . . ? C29 Ti4 C31 54.1(10) . . ? C32 Ti4 C31 32.0(7) . . ? C28 Ti4 C31 54.3(7) . . ? C30 Ti4 C31 32.0(10) . . ? O7 Ti4 Ti6 39.9(3) . . ? O2 Ti4 Ti6 96.3(3) . . ? O8 Ti4 Ti6 40.1(3) . . ? O1 Ti4 Ti6 96.3(3) . . ? C29 Ti4 Ti6 113.0(12) . . ? C32 Ti4 Ti6 162.8(6) . . ? C28 Ti4 Ti6 143.0(13) . . ? C30 Ti4 Ti6 108.3(7) . . ? C31 Ti4 Ti6 132.6(8) . . ? O7 Ti4 Ti2 96.7(3) . . ? O2 Ti4 Ti2 96.6(3) . . ? O8 Ti4 Ti2 39.7(3) . . ? O1 Ti4 Ti2 39.5(3) . . ? C29 Ti4 Ti2 112.2(11) . . ? C32 Ti4 Ti2 133.3(7) . . ? C28 Ti4 Ti2 108.5(6) . . ? C30 Ti4 Ti2 141.9(14) . . ? C31 Ti4 Ti2 162.8(6) . . ? Ti6 Ti4 Ti2 59.63(10) . . ? O7 Ti4 Ti5 39.8(4) . . ? O2 Ti4 Ti5 39.5(3) . . ? O8 Ti4 Ti5 97.1(3) . . ? O1 Ti4 Ti5 97.0(3) . . ? C29 Ti4 Ti5 150.0(18) . . ? C32 Ti4 Ti5 123.8(8) . . ? C28 Ti4 Ti5 156.1(11) . . ? C30 Ti4 Ti5 116.2(12) . . ? C31 Ti4 Ti5 106.9(6) . . ? Ti6 Ti4 Ti5 59.84(11) . . ? Ti2 Ti4 Ti5 89.81(6) . . ? O2 Ti3 O6 78.4(4) . . ? O2 Ti3 O5 125.8(5) . . ? O6 Ti3 O5 78.1(4) . . ? O2 Ti3 O1 78.1(4) . . ? O6 Ti3 O1 126.2(5) . . ? O5 Ti3 O1 77.9(5) . . ? O2 Ti3 C27 121.4(5) . . ? O6 Ti3 C27 144.9(5) . . ? O5 Ti3 C27 105.3(5) . . ? O1 Ti3 C27 88.0(5) . . ? O2 Ti3 C26 91.5(5) . . ? O6 Ti3 C26 129.7(5) . . ? O5 Ti3 C26 139.7(5) . . ? O1 Ti3 C26 98.6(5) . . ? C27 Ti3 C26 34.6(4) . . ? O2 Ti3 C25 92.7(5) . . ? O6 Ti3 C25 96.1(5) . . ? O5 Ti3 C25 137.8(5) . . ? O1 Ti3 C25 132.6(5) . . ? C27 Ti3 C25 57.4(5) . . ? C26 Ti3 C25 34.6(4) . . ? O2 Ti3 C24 123.5(5) . . ? O6 Ti3 C24 87.0(5) . . ? O5 Ti3 C24 103.1(5) . . ? O1 Ti3 C24 145.4(5) . . ? C27 Ti3 C24 58.0(5) . . ? C26 Ti3 C24 57.9(6) . . ? C25 Ti3 C24 34.7(4) . . ? O2 Ti3 C23 147.6(5) . . ? O6 Ti3 C23 112.6(5) . . ? O5 Ti3 C23 86.5(5) . . ? O1 Ti3 C23 113.1(5) . . ? C27 Ti3 C23 35.1(4) . . ? C26 Ti3 C23 57.5(6) . . ? C25 Ti3 C23 56.8(5) . . ? C24 Ti3 C23 34.1(4) . . ? O2 Ti3 Ti1 97.2(3) . . ? O6 Ti3 Ti1 39.9(3) . . ? O5 Ti3 Ti1 39.9(3) . . ? O1 Ti3 Ti1 97.2(4) . . ? C27 Ti3 Ti1 141.1(4) . . ? C26 Ti3 Ti1 163.2(4) . . ? C25 Ti3 Ti1 130.2(4) . . ? C24 Ti3 Ti1 105.4(4) . . ? C23 Ti3 Ti1 110.6(4) . . ? O2 Ti3 Ti5 39.9(3) . . ? O6 Ti3 Ti5 40.2(3) . . ? O5 Ti3 Ti5 97.4(3) . . ? O1 Ti3 Ti5 97.4(3) . . ? C27 Ti3 Ti5 157.2(4) . . ? C26 Ti3 Ti5 122.7(4) . . ? C25 Ti3 Ti5 104.5(4) . . ? C24 Ti3 Ti5 116.5(4) . . ? C23 Ti3 Ti5 149.3(4) . . ? Ti1 Ti3 Ti5 60.33(11) . . ? O2 Ti3 Ti2 96.7(4) . . ? O6 Ti3 Ti2 97.3(4) . . ? O5 Ti3 Ti2 40.2(3) . . ? O1 Ti3 Ti2 39.6(3) . . ? C27 Ti3 Ti2 107.5(4) . . ? C26 Ti3 Ti2 133.0(4) . . ? C25 Ti3 Ti2 164.9(4) . . ? C24 Ti3 Ti2 139.5(4) . . ? C23 Ti3 Ti2 111.1(4) . . ? Ti1 Ti3 Ti2 60.23(12) . . ? Ti5 Ti3 Ti2 90.25(13) . . ? O3 Ti1 O5 126.6(2) . . ? O3 Ti1 O6 78.0(5) . . ? O5 Ti1 O6 78.7(4) . . ? O3 Ti1 O4 78.8(5) . . ? O5 Ti1 O4 77.5(5) . . ? O6 Ti1 O4 126.3(2) . . ? O3 Ti1 C13 140.0(11) . . ? O5 Ti1 C13 90.5(9) . . ? O6 Ti1 C13 129.8(13) . . ? O4 Ti1 C13 97.8(11) . . ? O3 Ti1 C14 136.3(9) . . ? O5 Ti1 C14 93.9(7) . . ? O6 Ti1 C14 97.2(11) . . ? O4 Ti1 C14 131.7(12) . . ? C13 Ti1 C14 34.2(5) . . ? O3 Ti1 C17 105.4(10) . . ? O5 Ti1 C17 121.1(10) . . ? O6 Ti1 C17 144.1(6) . . ? O4 Ti1 C17 88.8(6) . . ? C13 Ti1 C17 34.6(5) . . ? C14 Ti1 C17 55.1(9) . . ? O3 Ti1 C16 87.5(6) . . ? O5 Ti1 C16 146.0(6) . . ? O6 Ti1 C16 112.6(7) . . ? O4 Ti1 C16 114.0(7) . . ? C13 Ti1 C16 57.1(7) . . ? C14 Ti1 C16 53.8(6) . . ? C17 Ti1 C16 34.2(5) . . ? O3 Ti1 C15 104.8(8) . . ? O5 Ti1 C15 121.6(7) . . ? O6 Ti1 C15 87.8(7) . . ? O4 Ti1 C15 145.1(7) . . ? C13 Ti1 C15 56.8(9) . . ? C14 Ti1 C15 31.7(9) . . ? C17 Ti1 C15 56.5(6) . . ? C16 Ti1 C15 33.8(4) . . ? O3 Ti1 Ti3 97.3(4) . . ? O5 Ti1 Ti3 40.4(3) . . ? O6 Ti1 Ti3 40.1(3) . . ? O4 Ti1 Ti3 97.1(3) . . ? C13 Ti1 Ti3 122.6(11) . . ? C14 Ti1 Ti3 106.5(7) . . ? C17 Ti1 Ti3 157.2(10) . . ? C16 Ti1 Ti3 148.9(6) . . ? C15 Ti1 Ti3 116.4(6) . . ? O3 Ti1 Ti6 40.3(3) . . ? O5 Ti1 Ti6 97.0(3) . . ? O6 Ti1 Ti6 97.1(3) . . ? O4 Ti1 Ti6 40.4(3) . . ? C13 Ti1 Ti6 133.0(12) . . ? C14 Ti1 Ti6 163.4(8) . . ? C17 Ti1 Ti6 108.4(8) . . ? C16 Ti1 Ti6 112.4(5) . . ? C15 Ti1 Ti6 141.2(7) . . ? Ti3 Ti1 Ti6 89.86(6) . . ? O3 Ti1 Ti5 40.2(4) . . ? O5 Ti1 Ti5 97.4(3) . . ? O6 Ti1 Ti5 39.8(3) . . ? O4 Ti1 Ti5 97.6(3) . . ? C13 Ti1 Ti5 163.9(9) . . ? C14 Ti1 Ti5 130.7(12) . . ? C17 Ti1 Ti5 141.3(9) . . ? C16 Ti1 Ti5 111.7(5) . . ? C15 Ti1 Ti5 107.3(7) . . ? Ti3 Ti1 Ti5 59.86(10) . . ? Ti6 Ti1 Ti5 60.02(10) . . ? O1 Ti2 O8 78.2(4) . . ? O1 Ti2 O4 126.5(4) . . ? O8 Ti2 O4 79.0(4) . . ? O1 Ti2 O5 78.7(5) . . ? O8 Ti2 O5 126.3(4) . . ? O4 Ti2 O5 77.2(5) . . ? O1 Ti2 C20 113.2(10) . . ? O8 Ti2 C20 145.8(6) . . ? O4 Ti2 C20 112.8(9) . . ? O5 Ti2 C20 87.9(6) . . ? O1 Ti2 C18 130.7(10) . . ? O8 Ti2 C18 92.8(8) . . ? O4 Ti2 C18 98.1(8) . . ? O5 Ti2 C18 137.7(9) . . ? C20 Ti2 C18 54.7(9) . . ? O1 Ti2 C22 98.2(8) . . ? O8 Ti2 C22 91.1(7) . . ? O4 Ti2 C22 129.9(9) . . ? O5 Ti2 C22 139.9(8) . . ? C20 Ti2 C22 56.2(7) . . ? C18 Ti2 C22 32.9(7) . . ? O1 Ti2 C19 144.1(7) . . ? O8 Ti2 C19 121.3(13) . . ? O4 Ti2 C19 88.5(6) . . ? O5 Ti2 C19 105.5(12) . . ? C20 Ti2 C19 33.7(8) . . ? C18 Ti2 C19 32.3(8) . . ? C22 Ti2 C19 55.3(8) . . ? O1 Ti2 C21 87.3(6) . . ? O8 Ti2 C21 120.1(9) . . ? O4 Ti2 C21 145.4(7) . . ? O5 Ti2 C21 106.3(8) . . ? C20 Ti2 C21 35.2(7) . . ? C18 Ti2 C21 55.6(8) . . ? C22 Ti2 C21 33.9(7) . . ? C19 Ti2 C21 57.1(8) . . ? O1 Ti2 Ti6 97.4(3) . . ? O8 Ti2 Ti6 40.4(3) . . ? O4 Ti2 Ti6 40.5(3) . . ? O5 Ti2 Ti6 96.8(3) . . ? C20 Ti2 Ti6 149.3(9) . . ? C18 Ti2 Ti6 106.4(6) . . ? C22 Ti2 Ti6 123.1(8) . . ? C19 Ti2 Ti6 117.0(9) . . ? C21 Ti2 Ti6 156.9(8) . . ? O1 Ti2 Ti3 40.3(3) . . ? O8 Ti2 Ti3 97.3(3) . . ? O4 Ti2 Ti3 96.8(3) . . ? O5 Ti2 Ti3 40.3(3) . . ? C20 Ti2 Ti3 112.2(7) . . ? C18 Ti2 Ti3 163.4(6) . . ? C22 Ti2 Ti3 133.3(8) . . ? C19 Ti2 Ti3 141.4(12) . . ? C21 Ti2 Ti3 107.8(5) . . ? Ti6 Ti2 Ti3 89.73(11) . . ? O1 Ti2 Ti4 40.1(3) . . ? O8 Ti2 Ti4 40.0(3) . . ? O4 Ti2 Ti4 97.8(3) . . ? O5 Ti2 Ti4 97.6(3) . . ? C20 Ti2 Ti4 149.3(9) . . ? C18 Ti2 Ti4 124.6(9) . . ? C22 Ti2 Ti4 105.3(5) . . ? C19 Ti2 Ti4 156.9(11) . . ? C21 Ti2 Ti4 115.3(7) . . ? Ti6 Ti2 Ti4 60.17(12) . . ? Ti3 Ti2 Ti4 60.15(12) . . ? O7 Ti6 O8 77.7(4) . . ? O7 Ti6 O4 126.0(5) . . ? O8 Ti6 O4 78.4(4) . . ? O7 Ti6 O3 78.9(5) . . ? O8 Ti6 O3 126.5(5) . . ? O4 Ti6 O3 77.8(5) . . ? O7 Ti6 C39 99.3(5) . . ? O8 Ti6 C39 140.0(5) . . ? O4 Ti6 C39 129.0(5) . . ? O3 Ti6 C39 91.0(5) . . ? O7 Ti6 C38 88.1(5) . . ? O8 Ti6 C38 106.0(5) . . ? O4 Ti6 C38 145.2(5) . . ? O3 Ti6 C38 120.6(5) . . ? C39 Ti6 C38 34.2(4) . . ? O7 Ti6 C41 145.3(5) . . ? O8 Ti6 C41 103.7(5) . . ? O4 Ti6 C41 87.5(5) . . ? O3 Ti6 C41 122.2(5) . . ? C39 Ti6 C41 57.0(5) . . ? C38 Ti6 C41 57.8(5) . . ? O7 Ti6 C40 133.2(5) . . ? O8 Ti6 C40 138.2(5) . . ? O4 Ti6 C40 95.4(5) . . ? O3 Ti6 C40 91.2(5) . . ? C39 Ti6 C40 34.6(4) . . ? C38 Ti6 C40 57.9(5) . . ? C41 Ti6 C40 34.5(4) . . ? O7 Ti6 C42 112.4(5) . . ? O8 Ti6 C42 86.9(5) . . ? O4 Ti6 C42 113.8(5) . . ? O3 Ti6 C42 146.6(5) . . ? C39 Ti6 C42 56.9(5) . . ? C38 Ti6 C42 34.7(4) . . ? C41 Ti6 C42 34.7(4) . . ? C40 Ti6 C42 57.6(5) . . ? O7 Ti6 Ti2 96.9(3) . . ? O8 Ti6 Ti2 40.1(3) . . ? O4 Ti6 Ti2 40.1(3) . . ? O3 Ti6 Ti2 97.3(3) . . ? C39 Ti6 Ti2 162.9(4) . . ? C38 Ti6 Ti2 142.0(4) . . ? C41 Ti6 Ti2 106.2(4) . . ? C40 Ti6 Ti2 129.9(4) . . ? C42 Ti6 Ti2 111.6(4) . . ? O7 Ti6 Ti1 97.4(4) . . ? O8 Ti6 Ti1 97.6(3) . . ? O4 Ti6 Ti1 40.0(3) . . ? O3 Ti6 Ti1 39.6(3) . . ? C39 Ti6 Ti1 122.2(4) . . ? C38 Ti6 Ti1 156.3(4) . . ? C41 Ti6 Ti1 116.5(4) . . ? C40 Ti6 Ti1 103.5(4) . . ? C42 Ti6 Ti1 150.1(4) . . ? Ti2 Ti6 Ti1 60.35(11) . . ? O7 Ti6 Ti5 40.1(3) . . ? O8 Ti6 Ti5 97.4(3) . . ? O4 Ti6 Ti5 97.4(4) . . ? O3 Ti6 Ti5 40.5(4) . . ? C39 Ti6 Ti5 105.5(4) . . ? C38 Ti6 Ti5 115.7(4) . . ? C41 Ti6 Ti5 158.9(4) . . ? C40 Ti6 Ti5 124.3(4) . . ? C42 Ti6 Ti5 148.7(4) . . ? Ti2 Ti6 Ti5 90.33(13) . . ? Ti1 Ti6 Ti5 60.21(12) . . ? O2 Ti5 O6 78.5(4) . . ? O2 Ti5 O7 77.3(5) . . ? O6 Ti5 O7 125.5(4) . . ? O2 Ti5 O3 125.4(4) . . ? O6 Ti5 O3 77.0(5) . . ? O7 Ti5 O3 78.8(5) . . ? O2 Ti5 C37 126.3(6) . . ? O6 Ti5 C37 89.3(6) . . ? O7 Ti5 C37 143.3(6) . . ? O3 Ti5 C37 101.4(6) . . ? O2 Ti5 C34 89.7(6) . . ? O6 Ti5 C34 126.8(6) . . ? O7 Ti5 C34 101.0(6) . . ? O3 Ti5 C34 143.0(6) . . ? C37 Ti5 C34 57.1(7) . . ? O2 Ti5 C36 147.4(6) . . ? O6 Ti5 C36 116.8(6) . . ? O7 Ti5 C36 109.7(6) . . ? O3 Ti5 C36 87.0(6) . . ? C37 Ti5 C36 34.8(4) . . ? C34 Ti5 C36 57.9(7) . . ? O2 Ti5 C35 117.5(6) . . ? O6 Ti5 C35 147.0(6) . . ? O7 Ti5 C35 87.2(6) . . ? O3 Ti5 C35 109.4(6) . . ? C37 Ti5 C35 57.8(7) . . ? C34 Ti5 C35 34.6(4) . . ? C36 Ti5 C35 35.3(4) . . ? O2 Ti5 C33 94.3(6) . . ? O6 Ti5 C33 94.5(6) . . ? O7 Ti5 C33 135.2(6) . . ? O3 Ti5 C33 135.5(6) . . ? C37 Ti5 C33 34.2(4) . . ? C34 Ti5 C33 34.3(4) . . ? C36 Ti5 C33 57.7(7) . . ? C35 Ti5 C33 57.6(7) . . ? O2 Ti5 Ti3 40.0(3) . . ? O6 Ti5 Ti3 40.2(3) . . ? O7 Ti5 Ti3 96.6(3) . . ? O3 Ti5 Ti3 96.5(3) . . ? C37 Ti5 Ti3 119.5(5) . . ? C34 Ti5 Ti3 120.0(5) . . ? C36 Ti5 Ti3 153.6(5) . . ? C35 Ti5 Ti3 154.1(5) . . ? C33 Ti5 Ti3 104.6(5) . . ? O2 Ti5 Ti6 96.6(3) . . ? O6 Ti5 Ti6 96.7(3) . . ? O7 Ti5 Ti6 40.1(3) . . ? O3 Ti5 Ti6 40.3(3) . . ? C37 Ti5 Ti6 137.0(5) . . ? C34 Ti5 Ti6 136.4(6) . . ? C36 Ti5 Ti6 109.0(6) . . ? C35 Ti5 Ti6 108.9(6) . . ? C33 Ti5 Ti6 165.8(5) . . ? Ti3 Ti5 Ti6 89.69(11) . . ? O2 Ti5 Ti1 96.8(3) . . ? O6 Ti5 Ti1 39.6(4) . . ? O7 Ti5 Ti1 96.9(3) . . ? O3 Ti5 Ti1 39.3(3) . . ? C37 Ti5 Ti1 106.1(5) . . ? C34 Ti5 Ti1 161.9(6) . . ? C36 Ti5 Ti1 113.3(5) . . ? C35 Ti5 Ti1 145.4(5) . . ? C33 Ti5 Ti1 127.9(6) . . ? Ti3 Ti5 Ti1 59.81(12) . . ? Ti6 Ti5 Ti1 59.77(13) . . ? Sn1 S2 Sn2 103.5(3) . . ? Sn1' S2' Sn2' 103.6(2) . . ? Sn3' S4' Sn2' 103.5(2) . . ? Sn2 S3 Sn3 85.63(16) . . ? Sn2 S3 H3 137.2 . . ? Sn3 S3 H3 137.2 . . ? Sn3' S5' H5' 109.5 . . ? Sn2' S3' Sn3' 85.51(17) . . ? Sn2' S3' H3' 137.3 . . ? Sn3' S3' H3' 137.2 . . ? Sn3 S4 Sn2 103.4(3) . . ? Sn1' S1' H1' 109.5 . . ? Sn3 S5 H5 109.4 . . ? Ti2 O8 Ti4 100.3(5) . . ? Ti2 O8 Ti6 99.6(5) . . ? Ti4 O8 Ti6 99.9(4) . . ? Ti1 O6 Ti3 99.9(4) . . ? Ti1 O6 Ti5 100.6(5) . . ? Ti3 O6 Ti5 99.6(5) . . ? Ti1 O4 Ti2 100.7(5) . . ? Ti1 O4 Ti6 99.6(4) . . ? Ti2 O4 Ti6 99.4(5) . . ? Sn1 S1 H1 109.4 . . ? Ti4 O7 Ti6 100.7(4) . . ? Ti4 O7 Ti5 100.9(5) . . ? Ti6 O7 Ti5 99.8(5) . . ? Ti5 O2 Ti3 100.1(5) . . ? Ti5 O2 Ti4 101.0(5) . . ? Ti3 O2 Ti4 100.8(4) . . ? Ti2 O1 Ti4 100.5(5) . . ? Ti2 O1 Ti3 100.1(5) . . ? Ti4 O1 Ti3 99.6(4) . . ? Ti1 O5 Ti2 100.5(5) . . ? Ti1 O5 Ti3 99.7(4) . . ? Ti2 O5 Ti3 99.6(5) . . ? Ti1 O3 Ti6 100.1(4) . . ? Ti1 O3 Ti5 100.5(5) . . ? Ti6 O3 Ti5 99.2(5) . . ? C16 C17 C13 107.4(19) . . ? C16 C17 Ti1 73.4(11) . . ? C13 C17 Ti1 71.6(11) . . ? C16 C17 H17 126.5 . . ? C13 C17 H17 126.1 . . ? Ti1 C17 H17 120.6 . . ? C14 C15 C16 106(2) . . ? C14 C15 Ti1 72.7(14) . . ? C16 C15 Ti1 73.2(12) . . ? C14 C15 H15 127.0 . . ? C16 C15 H15 126.6 . . ? Ti1 C15 H15 119.1 . . ? C19 C18 C22 112(2) . . ? C19 C18 Ti2 74.6(13) . . ? C22 C18 Ti2 73.8(12) . . ? C19 C18 H18 124.0 . . ? C22 C18 H18 124.1 . . ? Ti2 C18 H18 119.0 . . ? C37 C33 C34 107(2) . . ? C37 C33 Ti5 71.3(12) . . ? C34 C33 Ti5 71.4(12) . . ? C37 C33 H33 126.7 . . ? C34 C33 H33 126.4 . . ? Ti5 C33 H33 122.5 . . ? C38 C42 C41 107.6(15) . . ? C38 C42 Ti6 71.7(8) . . ? C41 C42 Ti6 72.3(9) . . ? C38 C42 H42 126.2 . . ? C41 C42 H42 126.2 . . ? Ti6 C42 H42 121.6 . . ? C28 C29 C30 108(2) . . ? C28 C29 Ti4 73.2(16) . . ? C30 C29 Ti4 73.3(15) . . ? C28 C29 H29 125.1 . . ? C30 C29 H29 127.1 . . ? Ti4 C29 H29 118.8 . . ? C22 C21 C20 103.7(19) . . ? C22 C21 Ti2 72.1(10) . . ? C20 C21 Ti2 70.6(10) . . ? C22 C21 H21 128.0 . . ? C20 C21 H21 128.3 . . ? Ti2 C21 H21 121.1 . . ? C27 C26 C25 107.8(16) . . ? C27 C26 Ti3 72.4(8) . . ? C25 C26 Ti3 72.9(9) . . ? C27 C26 H26 126.1 . . ? C25 C26 H26 126.1 . . ? Ti3 C26 H26 120.3 . . ? C18 C22 C21 109(2) . . ? C18 C22 Ti2 73.3(10) . . ? C21 C22 Ti2 74.0(11) . . ? C18 C22 H22 125.6 . . ? C21 C22 H22 125.7 . . ? Ti2 C22 H22 119.0 . . ? C32 C28 C29 105(2) . . ? C32 C28 Ti4 73.6(13) . . ? C29 C28 Ti4 72.2(17) . . ? C32 C28 H28 126.9 . . ? C29 C28 H28 128.5 . . ? Ti4 C28 H28 118.9 . . ? C32 C31 C30 112(3) . . ? C32 C31 Ti4 73.2(13) . . ? C30 C31 Ti4 73.6(16) . . ? C32 C31 H31 124.4 . . ? C30 C31 H31 123.7 . . ? Ti4 C31 H31 120.6 . . ? C26 C25 C24 108.9(16) . . ? C26 C25 Ti3 72.5(9) . . ? C24 C25 Ti3 72.9(9) . . ? C26 C25 H25 125.5 . . ? C24 C25 H25 125.6 . . ? Ti3 C25 H25 120.8 . . ? C33 C34 C35 110(2) . . ? C33 C34 Ti5 74.2(12) . . ? C35 C34 Ti5 73.1(11) . . ? C33 C34 H34 125.4 . . ? C35 C34 H34 125.1 . . ? Ti5 C34 H34 119.0 . . ? C37 C36 C35 107(2) . . ? C37 C36 Ti5 72.3(11) . . ? C35 C36 Ti5 72.7(10) . . ? C37 C36 H36 126.5 . . ? C35 C36 H36 126.7 . . ? Ti5 C36 H36 120.2 . . ? C39 C40 C41 106.6(15) . . ? C39 C40 Ti6 72.0(8) . . ? C41 C40 Ti6 72.7(8) . . ? C39 C40 H40 126.7 . . ? C41 C40 H40 126.7 . . ? Ti6 C40 H40 120.5 . . ? C31 C32 C28 111(3) . . ? C31 C32 Ti4 74.8(14) . . ? C28 C32 Ti4 74.0(15) . . ? C31 C32 H32 123.9 . . ? C28 C32 H32 124.7 . . ? Ti4 C32 H32 118.3 . . ? C18 C19 C20 107(2) . . ? C18 C19 Ti2 73.0(14) . . ? C20 C19 Ti2 71.7(12) . . ? C18 C19 H19 126.6 . . ? C20 C19 H19 126.4 . . ? Ti2 C19 H19 120.4 . . ? C31 C30 C29 104(3) . . ? C31 C30 Ti4 74.4(14) . . ? C29 C30 Ti4 71.9(16) . . ? C31 C30 H30 128.7 . . ? C29 C30 H30 127.1 . . ? Ti4 C30 H30 118.6 . . ? C19 C20 C21 109(2) . . ? C19 C20 Ti2 74.6(13) . . ? C21 C20 Ti2 74.2(9) . . ? C19 C20 H20 125.7 . . ? C21 C20 H20 125.6 . . ? Ti2 C20 H20 117.7 . . ? C39 C38 C42 107.3(15) . . ? C39 C38 Ti6 72.7(9) . . ? C42 C38 Ti6 73.5(8) . . ? C39 C38 H38 126.4 . . ? C42 C38 H38 126.4 . . ? Ti6 C38 H38 119.2 . . ? C15 C16 C17 108.0(18) . . ? C15 C16 Ti1 73.1(12) . . ? C17 C16 Ti1 72.3(11) . . ? C15 C16 H16 126.2 . . ? C17 C16 H16 125.8 . . ? Ti1 C16 H16 120.5 . . ? C23 C24 C25 107.3(16) . . ? C23 C24 Ti3 73.3(8) . . ? C25 C24 Ti3 72.4(9) . . ? C23 C24 H24 126.3 . . ? C25 C24 H24 126.4 . . ? Ti3 C24 H24 119.8 . . ? C34 C35 C36 107(2) . . ? C34 C35 Ti5 72.2(11) . . ? C36 C35 Ti5 72.0(10) . . ? C34 C35 H35 126.7 . . ? C36 C35 H35 126.4 . . ? Ti5 C35 H35 121.1 . . ? C14 C13 C17 103(2) . . ? C14 C13 Ti1 73.2(13) . . ? C17 C13 Ti1 73.8(12) . . ? C14 C13 H13 128.1 . . ? C17 C13 H13 128.4 . . ? Ti1 C13 H13 117.2 . . ? C26 C27 C23 107.4(15) . . ? C26 C27 Ti3 73.0(8) . . ? C23 C27 Ti3 73.5(8) . . ? C26 C27 H27 126.3 . . ? C23 C27 H27 126.3 . . ? Ti3 C27 H27 119.2 . . ? C38 C39 C40 110.2(15) . . ? C38 C39 Ti6 73.0(8) . . ? C40 C39 Ti6 73.4(8) . . ? C38 C39 H39 124.9 . . ? C40 C39 H39 124.9 . . ? Ti6 C39 H39 120.3 . . ? C24 C23 C27 108.5(15) . . ? C24 C23 Ti3 72.6(8) . . ? C27 C23 Ti3 71.4(8) . . ? C24 C23 H23 125.8 . . ? C27 C23 H23 125.7 . . ? Ti3 C23 H23 121.9 . . ? C33 C37 C36 110(2) . . ? C33 C37 Ti5 74.5(12) . . ? C36 C37 Ti5 73.0(11) . . ? C33 C37 H37 124.9 . . ? C36 C37 H37 125.3 . . ? Ti5 C37 H37 119.3 . . ? C40 C41 C42 108.4(15) . . ? C40 C41 Ti6 72.8(8) . . ? C42 C41 Ti6 73.0(9) . . ? C40 C41 H41 125.8 . . ? C42 C41 H41 125.8 . . ? Ti6 C41 H41 120.1 . . ? C15 C14 C13 115(2) . . ? C15 C14 Ti1 75.6(14) . . ? C13 C14 Ti1 72.6(12) . . ? C15 C14 H14 122.6 . . ? C13 C14 H14 122.8 . . ? Ti1 C14 H14 120.6 . . ? C2' C1' Sn1' 115.3(13) . . ? C2' C1' H1'1 108.7 . . ? Sn1' C1' H1'1 108.6 . . ? C2' C1' H1'2 108.2 . . ? Sn1' C1' H1'2 108.3 . . ? H1'1 C1' H1'2 107.5 . . ? C3' C2' C1' 119(2) . . ? C3' C2' H2'1 107.6 . . ? C1' C2' H2'1 107.7 . . ? C3' C2' H2'2 107.6 . . ? C1' C2' H2'2 107.2 . . ? H2'1 C2' H2'2 107.0 . . ? C2' C3' C4' 109(3) . . ? C2' C3' H3'1 109.9 . . ? C4' C3' H3'1 110.5 . . ? C2' C3' H3'2 109.9 . . ? C4' C3' H3'2 108.9 . . ? H3'1 C3' H3'2 108.2 . . ? C3' C4' H4'1 109.6 . . ? C3' C4' H4'2 110.2 . . ? H4'1 C4' H4'2 109.5 . . ? C3' C4' H4'3 108.6 . . ? H4'1 C4' H4'3 109.5 . . ? H4'2 C4' H4'3 109.5 . . ? C3' C4' H4'4 109.3 . . ? H4'1 C4' H4'4 141.1 . . ? H4'2 C4' H4'4 56.3 . . ? H4'3 C4' H4'4 56.3 . . ? C3' C4' H4'5 108.8 . . ? H4'1 C4' H4'5 56.3 . . ? H4'2 C4' H4'5 141.1 . . ? H4'3 C4' H4'5 56.3 . . ? H4'4 C4' H4'5 109.5 . . ? C3' C4' H4'6 110.3 . . ? H4'1 C4' H4'6 56.3 . . ? H4'2 C4' H4'6 56.3 . . ? H4'3 C4' H4'6 141.1 . . ? H4'4 C4' H4'6 109.5 . . ? H4'5 C4' H4'6 109.5 . . ? C6' C5' Sn2' 120(2) . . ? C6' C5' H5'1 110.5 . . ? Sn2' C5' H5'1 108.6 . . ? C6' C5' H5'2 104.1 . . ? Sn2' C5' H5'2 105.5 . . ? H5'1 C5' H5'2 107.0 . . ? C10' C9' Sn3' 105(3) . . ? C10' C9' H9'1 115.7 . . ? Sn3' C9' H9'1 111.9 . . ? C10' C9' H9'2 106.8 . . ? Sn3' C9' H9'2 108.8 . . ? H9'1 C9' H9'2 108.5 . . ? C12' C11' H11A 108.9 . . ? C12' C11' H11B 109.0 . . ? H11A C11' H11B 109.5 . . ? C12' C11' H11C 110.6 . . ? H11A C11' H11C 109.5 . . ? H11B C11' H11C 109.5 . . ? C10' C12' C11' 107(4) . . ? C10' C12' H12A 107.9 . . ? C11' C12' H12A 109.7 . . ? C10' C12' H12B 112.5 . . ? C11' C12' H12B 111.1 . . ? H12A C12' H12B 108.4 . . ? C2 C1 Sn1 113.5(18) . . ? C2 C1 H1A 108.3 . . ? Sn1 C1 H1A 108.6 . . ? C2 C1 H1B 109.4 . . ? Sn1 C1 H1B 109.2 . . ? H1A C1 H1B 107.7 . . ? C1 C2 C3 120(3) . . ? C1 C2 H2A 107.9 . . ? C3 C2 H2A 107.5 . . ? C1 C2 H2B 106.8 . . ? C3 C2 H2B 107.1 . . ? H2A C2 H2B 106.9 . . ? C2 C3 C4 110.1(18) . . ? C2 C3 H3A 109.8 . . ? C4 C3 H3A 109.6 . . ? C2 C3 H3B 109.4 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.1 . . ? C7 C8 H8A 109.1 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.6 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5' C6' C7' 114(3) . . ? C5' C6' H6'1 105.3 . . ? C7' C6' H6'1 108.4 . . ? C5' C6' H6'2 111.7 . . ? C7' C6' H6'2 109.6 . . ? H6'1 C6' H6'2 107.5 . . ? C8' C7' C6' 105(3) . . ? C8' C7' H7'1 110.6 . . ? C6' C7' H7'1 111.7 . . ? C8' C7' H7'2 110.8 . . ? C6' C7' H7'2 110.0 . . ? H7'1 C7' H7'2 108.7 . . ? C7' C8' H8'1 109.1 . . ? C7' C8' H8'2 109.7 . . ? H8'1 C8' H8'2 109.5 . . ? C7' C8' H8'3 109.6 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? C9' C10' C12' 110(4) . . ? C9' C10' H10A 105.6 . . ? C12' C10' H10A 107.0 . . ? C9' C10' H10B 114.6 . . ? C12' C10' H10B 111.6 . . ? H10A C10' H10B 107.9 . . ? C6 C5 C7 125(4) . . ? C6 C5 H5A 110.3 . . ? C7 C5 H5A 106.4 . . ? C6 C5 H5B 102.4 . . ? C7 C5 H5B 105.0 . . ? H5A C5 H5B 106.2 . . ? C5 C6 Sn2 123(3) . . ? C5 C6 H6A 102.6 . . ? Sn2 C6 H6A 104.7 . . ? C5 C6 H6B 110.4 . . ? Sn2 C6 H6B 108.2 . . ? H6A C6 H6B 106.2 . . ? C8 C7 C5 121(4) . . ? C8 C7 H7A 107.0 . . ? C5 C7 H7A 106.2 . . ? C8 C7 H7B 107.1 . . ? C5 C7 H7B 107.6 . . ? H7A C7 H7B 106.7 . . ? C10 C9 C11 120(3) . . ? C10 C9 H9A 109.1 . . ? C11 C9 H9A 108.5 . . ? C10 C9 H9B 104.6 . . ? C11 C9 H9B 106.4 . . ? H9A C9 H9B 107.2 . . ? C9 C10 Sn3 106(2) . . ? C9 C10 H10C 107.6 . . ? Sn3 C10 H10C 109.8 . . ? C9 C10 H10D 112.5 . . ? Sn3 C10 H10D 111.8 . . ? H10C C10 H10D 109.0 . . ? C12 C11 C9 119(3) . . ? C12 C11 H11D 107.6 . . ? C9 C11 H11D 106.5 . . ? C12 C11 H11E 107.4 . . ? C9 C11 H11E 108.4 . . ? H11D C11 H11E 107.2 . . ? C11 C12 H12C 110.4 . . ? C11 C12 H12D 108.8 . . ? H12C C12 H12D 109.5 . . ? C11 C12 H12E 109.2 . . ? H12C C12 H12E 109.5 . . ? H12D C12 H12E 109.5 . . ? C3 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.6 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.798 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.118 # Attachment '- Orthorhombic.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 788689' #TrackingRef '- Orthorhombic.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H90 Cl2 O8 S12 Sn6 Ti6' _chemical_formula_weight 2322.42 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 19.115(3) _cell_length_b 19.488(3) _cell_length_c 21.356(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7955.1(19) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 898 _cell_measurement_theta_min 2.156 _cell_measurement_theta_max 28.541 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.939 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4544 _exptl_absorpt_coefficient_mu 2.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4821 _exptl_absorpt_correction_T_max 0.8907 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 126469 _diffrn_reflns_av_R_equivalents 0.1675 _diffrn_reflns_av_sigmaI/netI 0.1049 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 32.83 _reflns_number_total 14022 _reflns_number_gt 8171 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis-Pro oxford diffraction Ltd' _computing_cell_refinement 'CrysAlis-Pro oxford diffraction Ltd' _computing_data_reduction 'CrysAlis-Pro oxford diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. ; _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^)+(0.1836P)^2^+136.5626P] 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 riding-model _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14022 _refine_ls_number_parameters 280 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1387 _refine_ls_R_factor_gt 0.0836 _refine_ls_wR_factor_ref 0.1940 _refine_ls_wR_factor_gt 0.1605 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _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 Sn01 Sn 0.29539(11) 0.15005(10) 0.72035(8) 0.0352(5) Uani 1 1 d . . . Sn02 Sn 0.29138(9) 0.28036(9) 0.84643(8) 0.0266(4) Uani 1 1 d . . . Sn03 Sn 0.15079(10) 0.28040(10) 0.72524(9) 0.0341(5) Uani 1 1 d . . . Ti01 Ti 0.5028(2) 0.9937(2) 0.90098(19) 0.0255(10) Uani 1 1 d . . . Ti03 Ti 0.6104(2) 0.9926(2) 1.0027(2) 0.0245(9) Uani 1 1 d . . . Ti02 Ti 0.5078(2) 1.1090(2) 0.9946(2) 0.0241(9) Uani 1 1 d . . . S03 S 0.2753(3) 0.2663(3) 0.9598(3) 0.0300(15) Uani 1 1 d . . . H03 H 0.2348 0.3087 0.9786 0.045 Uiso 1 1 calc R . . S06 S 0.1769(5) 0.1666(4) 0.6914(4) 0.046(2) Uani 1 1 d . . . S02 S 0.3201(4) 0.1631(4) 0.8292(4) 0.0359(16) Uani 1 1 d . . . S01 S 0.2832(4) 0.0262(4) 0.7238(5) 0.051(2) Uani 1 1 d . . . H01 H 0.2467 0.0076 0.6813 0.076 Uiso 1 1 calc R . . S04 S 0.1702(3) 0.3064(4) 0.8337(4) 0.0392(18) Uani 1 1 d . . . S05 S 0.0272(4) 0.2586(5) 0.7370(4) 0.053(2) Uani 1 1 d . . . H05 H 0.0056 0.2888 0.7819 0.079 Uiso 1 1 calc R . . O03 O 0.5699(8) 1.0544(8) 0.9383(7) 0.0238(18) Uani 1 1 d . . . C26 C 0.7130(16) 0.9308(17) 1.0140(14) 0.046(4) Uani 1 1 d . . . H015 H 0.7102 0.8845 1.0241 0.055 Uiso 1 1 calc R . . O04 O 0.5620(8) 0.9271(8) 0.9454(7) 0.0238(18) Uani 1 1 d . . . O01 O 0.4324(8) 0.9376(8) 0.9454(7) 0.0238(18) Uani 1 1 d . . . O02 O 0.4407(8) 1.0639(8) 0.9379(7) 0.0238(18) Uani 1 1 d . . . C24 C 0.7198(16) 1.0413(17) 1.0223(17) 0.051(4) Uani 1 1 d . . . H020 H 0.7244 1.0853 1.0385 0.062 Uiso 1 1 calc R . . C02 C 0.4198(17) 0.1020(16) 0.6357(13) 0.053(4) Uani 1 1 d D . . H02A H 0.3913 0.0609 0.6324 0.063 Uiso 1 1 calc R . . H02B H 0.4499 0.0970 0.6720 0.063 Uiso 1 1 calc R . . C01 C 0.3727(18) 0.1635(16) 0.6447(13) 0.053(4) Uani 1 1 d D . . H02C H 0.3481 0.1725 0.6059 0.063 Uiso 1 1 calc R . . H02D H 0.4013 0.2033 0.6540 0.063 Uiso 1 1 calc R . . C21 C 0.5700(19) 1.2106(19) 1.0111(14) 0.055(3) Uani 1 1 d . . . H023 H 0.6146 1.2110 1.0286 0.065 Uiso 1 1 calc R . . C17 C 0.569(2) 0.9977(19) 0.8081(14) 0.055(3) Uani 1 1 d . . . H024 H 0.6166 1.0068 0.8075 0.065 Uiso 1 1 calc R . . C16 C 0.5211(17) 1.0432(17) 0.8053(16) 0.051(4) Uani 1 1 d . . . H026 H 0.5289 1.0903 0.8063 0.062 Uiso 1 1 calc R . . C06 C 0.3449(18) 0.4302(14) 0.8411(14) 0.053(4) Uani 1 1 d D . . H02E H 0.3242 0.4344 0.7999 0.063 Uiso 1 1 calc R . . H02F H 0.3088 0.4394 0.8719 0.063 Uiso 1 1 calc R . . C19 C 0.4578(18) 1.2161(16) 1.0044(16) 0.051(4) Uani 1 1 d . . . H030 H 0.4104 1.2193 1.0139 0.062 Uiso 1 1 calc R . . C27 C 0.7153(18) 0.9573(19) 0.9528(15) 0.055(3) Uani 1 1 d . . . H032 H 0.7159 0.9314 0.9162 0.065 Uiso 1 1 calc R . . C25 C 0.7155(18) 0.9847(19) 1.0577(15) 0.055(3) Uani 1 1 d . . . H036 H 0.7144 0.9817 1.1012 0.065 Uiso 1 1 calc R . . C08 C 0.3777(19) 0.5567(16) 0.8403(15) 0.063(11) Uani 1 1 d D . . H04A H 0.4171 0.5869 0.8449 0.095 Uiso 1 1 calc R . . H04B H 0.3434 0.5672 0.8717 0.095 Uiso 1 1 calc R . . H04C H 0.3575 0.5627 0.7995 0.095 Uiso 1 1 calc R . . C23 C 0.7165(16) 1.0262(16) 0.9560(15) 0.046(4) Uani 1 1 d . . . H042 H 0.7155 1.0573 0.9230 0.055 Uiso 1 1 calc R . . Cl01 Cl 0.3015(4) 0.2999(4) 0.7174(4) 0.048(2) Uani 1 1 d . . . C05 C 0.3720(13) 0.3572(13) 0.8500(15) 0.043(7) Uani 1 1 d D . . H04D H 0.3956 0.3542 0.8901 0.052 Uiso 1 1 calc R . . H04E H 0.4062 0.3475 0.8176 0.052 Uiso 1 1 calc R . . C15 C 0.4557(19) 1.0125(19) 0.8006(14) 0.055(3) Uani 1 1 d . . . H047 H 0.4123 1.0327 0.7937 0.065 Uiso 1 1 calc R . . C18 C 0.4842(18) 1.2130(19) 0.9453(14) 0.055(3) Uani 1 1 d . . . H048 H 0.4579 1.2148 0.9087 0.065 Uiso 1 1 calc R . . C07 C 0.4019(18) 0.4822(14) 0.8479(14) 0.053(4) Uani 1 1 d D . . H05A H 0.4377 0.4727 0.8169 0.063 Uiso 1 1 calc R . . H05B H 0.4231 0.4770 0.8889 0.063 Uiso 1 1 calc R . . C09 C 0.1554(18) 0.3559(14) 0.653(2) 0.065(8) Uani 1 1 d . . . H00A H 0.1798 0.3958 0.6691 0.078 Uiso 1 1 calc R . . H00B H 0.1829 0.3377 0.6187 0.078 Uiso 1 1 calc R . . C20 C 0.5090(16) 1.2140(16) 1.0469(15) 0.046(4) Uani 1 1 d . . . H002 H 0.5050 1.2147 1.0903 0.055 Uiso 1 1 calc R . . C22 C 0.5584(17) 1.2067(15) 0.9482(17) 0.051(4) Uani 1 1 d . . . H003 H 0.5904 1.2014 0.9157 0.062 Uiso 1 1 calc R . . C10 C 0.0861(18) 0.3785(15) 0.628(2) 0.065(8) Uani 1 1 d . . . H00C H 0.0583 0.3387 0.6168 0.078 Uiso 1 1 calc R . . H00D H 0.0610 0.4041 0.6597 0.078 Uiso 1 1 calc R . . C13 C 0.5401(18) 0.934(2) 0.8122(14) 0.055(3) Uani 1 1 d . . . H005 H 0.5638 0.8925 0.8164 0.065 Uiso 1 1 calc R . . C03 C 0.462(2) 0.1087(19) 0.5805(17) 0.065(10) Uani 1 1 d . . . H00E H 0.4978 0.0733 0.5806 0.078 Uiso 1 1 calc R . . H00F H 0.4856 0.1529 0.5813 0.078 Uiso 1 1 calc R . . C14 C 0.4728(19) 0.943(2) 0.8090(14) 0.055(3) Uani 1 1 d . . . H007 H 0.4401 0.9073 0.8119 0.065 Uiso 1 1 calc R . . C11 C 0.0962(17) 0.422(2) 0.5723(18) 0.066(12) Uani 1 1 d . . . H00G H 0.1347 0.4529 0.5808 0.079 Uiso 1 1 calc R . . H00H H 0.0545 0.4495 0.5668 0.079 Uiso 1 1 calc R . . C12 C 0.111(2) 0.3856(18) 0.5111(19) 0.078(13) Uani 1 1 d . . . H00I H 0.1168 0.4190 0.4785 0.117 Uiso 1 1 calc R . . H00J H 0.0728 0.3558 0.5010 0.117 Uiso 1 1 calc R . . H00K H 0.1532 0.3591 0.5151 0.117 Uiso 1 1 calc R . . C04 C 0.4185(18) 0.1029(18) 0.5192(13) 0.053(4) Uani 1 1 d . . . H01A H 0.4491 0.1061 0.4837 0.079 Uiso 1 1 calc R . . H01B H 0.3848 0.1394 0.5177 0.079 Uiso 1 1 calc R . . H01C H 0.3946 0.0595 0.5184 0.079 Uiso 1 1 calc R . . 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 Sn01 0.0441(11) 0.0334(10) 0.0280(9) -0.0162(8) 0.0020(9) 0.0059(9) Sn02 0.0255(8) 0.0267(9) 0.0276(8) -0.0070(7) -0.0041(7) 0.0101(8) Sn03 0.0398(11) 0.0301(10) 0.0325(9) -0.0008(9) -0.0108(8) 0.0029(9) Ti01 0.031(2) 0.024(2) 0.0206(19) -0.0025(18) -0.0044(18) -0.0031(19) Ti03 0.024(2) 0.026(2) 0.024(2) 0.0055(19) -0.0061(17) -0.0036(18) Ti02 0.029(2) 0.018(2) 0.026(2) 0.0009(18) -0.0009(18) -0.0010(18) S03 0.033(4) 0.019(3) 0.038(4) -0.007(3) -0.006(3) 0.007(2) S06 0.062(5) 0.033(4) 0.042(4) 0.005(3) -0.025(4) -0.017(4) S02 0.019(3) 0.031(4) 0.057(5) -0.008(3) -0.003(3) -0.002(3) S01 0.042(5) 0.026(4) 0.085(6) -0.023(4) -0.003(4) 0.003(3) S04 0.013(3) 0.043(4) 0.061(5) -0.028(4) -0.004(3) 0.005(3) S05 0.028(4) 0.062(6) 0.069(6) 0.001(5) -0.012(4) 0.003(4) O03 0.018(4) 0.023(5) 0.030(4) -0.003(4) -0.009(4) 0.002(4) C26 0.053(11) 0.042(10) 0.043(10) 0.008(8) 0.013(8) 0.004(9) O04 0.018(4) 0.023(5) 0.030(4) -0.003(4) -0.009(4) 0.002(4) O01 0.018(4) 0.023(5) 0.030(4) -0.003(4) -0.009(4) 0.002(4) O02 0.018(4) 0.023(5) 0.030(4) -0.003(4) -0.009(4) 0.002(4) C24 0.048(10) 0.035(9) 0.071(11) 0.016(8) 0.004(8) -0.003(7) C02 0.074(11) 0.061(10) 0.023(6) -0.001(7) -0.004(7) -0.007(8) C01 0.074(11) 0.061(10) 0.023(6) -0.001(7) -0.004(7) -0.007(8) C21 0.059(8) 0.072(9) 0.033(5) -0.002(6) -0.006(5) 0.003(7) C17 0.059(8) 0.072(9) 0.033(5) -0.002(6) -0.006(5) 0.003(7) C16 0.048(10) 0.035(9) 0.071(11) 0.016(8) 0.004(8) -0.003(7) C06 0.074(11) 0.061(10) 0.023(6) -0.001(7) -0.004(7) -0.007(8) C19 0.048(10) 0.035(9) 0.071(11) 0.016(8) 0.004(8) -0.003(7) C27 0.059(8) 0.072(9) 0.033(5) -0.002(6) -0.006(5) 0.003(7) C25 0.059(8) 0.072(9) 0.033(5) -0.002(6) -0.006(5) 0.003(7) C08 0.07(2) 0.08(3) 0.039(17) -0.026(18) 0.001(16) 0.05(2) C23 0.053(11) 0.042(10) 0.043(10) 0.008(8) 0.013(8) 0.004(9) Cl01 0.039(4) 0.045(4) 0.060(5) -0.039(4) -0.006(3) -0.012(3) C05 0.015(12) 0.06(2) 0.055(18) -0.016(16) -0.002(12) -0.013(12) C15 0.059(8) 0.072(9) 0.033(5) -0.002(6) -0.006(5) 0.003(7) C18 0.059(8) 0.072(9) 0.033(5) -0.002(6) -0.006(5) 0.003(7) C07 0.074(11) 0.061(10) 0.023(6) -0.001(7) -0.004(7) -0.007(8) C09 0.059(16) 0.017(10) 0.12(2) 0.016(13) -0.045(16) 0.001(10) C20 0.053(11) 0.042(10) 0.043(10) 0.008(8) 0.013(8) 0.004(9) C22 0.048(10) 0.035(9) 0.071(11) 0.016(8) 0.004(8) -0.003(7) C10 0.059(16) 0.017(10) 0.12(2) 0.016(13) -0.045(16) 0.001(10) C13 0.059(8) 0.072(9) 0.033(5) -0.002(6) -0.006(5) 0.003(7) C03 0.06(2) 0.05(2) 0.08(3) 0.01(2) 0.01(2) -0.014(19) C14 0.059(8) 0.072(9) 0.033(5) -0.002(6) -0.006(5) 0.003(7) C11 0.037(19) 0.08(3) 0.08(3) 0.03(2) -0.029(18) -0.025(18) C12 0.13(4) 0.027(19) 0.08(3) 0.000(19) -0.03(3) -0.02(2) C04 0.074(11) 0.061(10) 0.023(6) -0.001(7) -0.004(7) -0.007(8) _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 Sn01 C01 2.20(3) . ? Sn01 S06 2.370(9) . ? Sn01 S02 2.385(8) . ? Sn01 S01 2.426(8) . ? Sn02 C05 2.15(3) . ? Sn02 S02 2.378(7) . ? Sn02 S04 2.387(7) . ? Sn02 S03 2.456(7) . ? Sn02 Cl01 2.789(9) . ? Sn03 C09 2.13(3) . ? Sn03 S06 2.386(9) . ? Sn03 S04 2.399(8) . ? Sn03 S05 2.413(8) . ? Ti01 O03 1.917(16) . ? Ti01 O04 1.965(16) . ? Ti01 O02 1.975(16) . ? Ti01 O01 1.976(17) . ? Ti01 C14 2.28(3) . ? Ti01 C16 2.29(3) . ? Ti01 C13 2.34(3) . ? Ti01 C17 2.35(3) . ? Ti01 C15 2.35(3) . ? Ti01 Ti03 2.992(6) . ? Ti01 Ti03 2.998(7) 5_677 ? Ti01 Ti02 3.003(6) 5_677 ? Ti03 O01 1.935(17) 5_677 ? Ti03 O02 1.943(17) 5_677 ? Ti03 O03 1.987(16) . ? Ti03 O04 1.996(16) . ? Ti03 C26 2.31(3) . ? Ti03 C25 2.33(3) . ? Ti03 C24 2.33(3) . ? Ti03 C23 2.35(3) . ? Ti03 C27 2.37(3) . ? Ti03 Ti01 2.998(7) 5_677 ? Ti03 Ti02 3.004(6) . ? Ti02 O01 1.943(16) 5_677 ? Ti02 O02 1.970(16) . ? Ti02 O04 1.979(17) 5_677 ? Ti02 O03 1.998(17) . ? Ti02 C19 2.30(3) . ? Ti02 C18 2.33(4) . ? Ti02 C20 2.33(3) . ? Ti02 C21 2.34(4) . ? Ti02 C22 2.36(3) . ? Ti02 Ti01 3.003(6) 5_677 ? Ti02 Ti03 3.005(6) 5_677 ? S03 H03 1.2000 . ? S01 H01 1.2000 . ? S05 H05 1.2000 . ? C26 C27 1.41(4) . ? C26 C25 1.40(4) . ? C26 H015 0.9300 . ? O04 Ti02 1.979(17) 5_677 ? O01 Ti03 1.935(17) 5_677 ? O01 Ti02 1.943(16) 5_677 ? O02 Ti03 1.943(17) 5_677 ? C24 C25 1.34(4) . ? C24 C23 1.45(5) . ? C24 H020 0.9300 . ? C02 C01 1.512(19) . ? C02 C03 1.44(4) . ? C02 H02A 0.9700 . ? C02 H02B 0.9700 . ? C01 H02C 0.9700 . ? C01 H02D 0.9700 . ? C21 C22 1.36(4) . ? C21 C20 1.40(4) . ? C21 H023 0.9300 . ? C17 C16 1.27(4) . ? C17 C13 1.36(5) . ? C17 H024 0.9300 . ? C16 C15 1.39(5) . ? C16 H026 0.9300 . ? C06 C07 1.49(4) . ? C06 C05 1.526(18) . ? C06 H02E 0.9700 . ? C06 H02F 0.9700 . ? C19 C20 1.34(4) . ? C19 C18 1.36(4) . ? C19 H030 0.9300 . ? C27 C23 1.35(5) . ? C27 H032 0.9300 . ? C25 H036 0.9300 . ? C08 C07 1.533(18) . ? C08 H04A 0.9600 . ? C08 H04B 0.9600 . ? C08 H04C 0.9600 . ? C23 H042 0.9300 . ? C05 H04D 0.9700 . ? C05 H04E 0.9700 . ? C15 C14 1.41(5) . ? C15 H047 0.9300 . ? C18 C22 1.42(5) . ? C18 H048 0.9300 . ? C07 H05A 0.9700 . ? C07 H05B 0.9700 . ? C09 C10 1.50(4) . ? C09 H00A 0.9700 . ? C09 H00B 0.9700 . ? C20 H002 0.9300 . ? C22 H003 0.9300 . ? C10 C11 1.47(5) . ? C10 H00C 0.9700 . ? C10 H00D 0.9700 . ? C13 C14 1.30(5) . ? C13 H005 0.9300 . ? C03 C04 1.56(5) . ? C03 H00E 0.9700 . ? C03 H00F 0.9700 . ? C14 H007 0.9300 . ? C11 C12 1.51(5) . ? C11 H00G 0.9700 . ? C11 H00H 0.9700 . ? C12 H00I 0.9600 . ? C12 H00J 0.9600 . ? C12 H00K 0.9600 . ? C04 H01A 0.9600 . ? C04 H01B 0.9600 . ? C04 H01C 0.9600 . ? 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 C01 Sn01 S06 115.7(8) . . ? C01 Sn01 S02 124.7(9) . . ? S06 Sn01 S02 115.4(3) . . ? C01 Sn01 S01 101.8(8) . . ? S06 Sn01 S01 92.9(3) . . ? S02 Sn01 S01 95.5(3) . . ? C05 Sn02 S02 120.6(7) . . ? C05 Sn02 S04 123.4(7) . . ? S02 Sn02 S04 114.2(2) . . ? C05 Sn02 S03 97.6(9) . . ? S02 Sn02 S03 94.3(2) . . ? S04 Sn02 S03 90.9(3) . . ? C05 Sn02 Cl01 83.7(9) . . ? S02 Sn02 Cl01 87.8(2) . . ? S04 Sn02 Cl01 85.7(3) . . ? S03 Sn02 Cl01 176.5(2) . . ? C09 Sn03 S06 114.4(11) . . ? C09 Sn03 S04 123.1(10) . . ? S06 Sn03 S04 117.2(3) . . ? C09 Sn03 S05 103.7(9) . . ? S06 Sn03 S05 94.1(3) . . ? S04 Sn03 S05 95.1(3) . . ? O03 Ti01 O04 79.8(7) . . ? O03 Ti01 O02 79.0(7) . . ? O04 Ti01 O02 127.6(7) . . ? O03 Ti01 O01 126.7(7) . . ? O04 Ti01 O01 78.2(7) . . ? O02 Ti01 O01 77.4(7) . . ? O03 Ti01 C14 142.9(11) . . ? O04 Ti01 C14 105.8(10) . . ? O02 Ti01 C14 119.7(10) . . ? O01 Ti01 C14 90.0(11) . . ? O03 Ti01 C16 90.5(10) . . ? O04 Ti01 C16 128.5(10) . . ? O02 Ti01 C16 99.0(10) . . ? O01 Ti01 C16 140.0(10) . . ? C14 Ti01 C16 56.8(13) . . ? O03 Ti01 C13 116.2(10) . . ? O04 Ti01 C13 83.5(10) . . ? O02 Ti01 C13 148.5(10) . . ? O01 Ti01 C13 108.7(10) . . ? C14 Ti01 C13 32.7(11) . . ? C16 Ti01 C13 55.9(12) . . ? O03 Ti01 C17 88.3(10) . . ? O04 Ti01 C17 96.9(10) . . ? O02 Ti01 C17 129.5(10) . . ? O01 Ti01 C17 142.0(10) . . ? C14 Ti01 C17 54.7(13) . . ? C16 Ti01 C17 31.9(11) . . ? C13 Ti01 C17 33.8(12) . . ? O03 Ti01 C15 122.5(10) . . ? O04 Ti01 C15 139.7(10) . . ? O02 Ti01 C15 91.5(10) . . ? O01 Ti01 C15 105.2(10) . . ? C14 Ti01 C15 35.5(12) . . ? C16 Ti01 C15 34.8(12) . . ? C13 Ti01 C15 57.0(12) . . ? C17 Ti01 C15 55.4(12) . . ? O03 Ti01 Ti03 40.8(5) . . ? O04 Ti01 Ti03 41.3(5) . . ? O02 Ti01 Ti03 97.4(5) . . ? O01 Ti01 Ti03 96.7(5) . . ? C14 Ti01 Ti03 142.8(9) . . ? C16 Ti01 Ti03 123.2(9) . . ? C13 Ti01 Ti03 112.1(9) . . ? C17 Ti01 Ti03 104.1(9) . . ? C15 Ti01 Ti03 157.7(9) . . ? O03 Ti01 Ti03 98.2(5) . 5_677 ? O04 Ti01 Ti03 98.3(5) . 5_677 ? O02 Ti01 Ti03 39.7(5) . 5_677 ? O01 Ti01 Ti03 39.5(5) . 5_677 ? C14 Ti01 Ti03 116.7(9) . 5_677 ? C16 Ti01 Ti03 133.3(9) . 5_677 ? C13 Ti01 Ti03 145.2(9) . 5_677 ? C17 Ti01 Ti03 164.3(9) . 5_677 ? C15 Ti01 Ti03 109.5(9) . 5_677 ? Ti03 Ti01 Ti03 89.94(16) . 5_677 ? O03 Ti01 Ti02 98.5(5) . 5_677 ? O04 Ti01 Ti02 40.6(5) . 5_677 ? O02 Ti01 Ti02 97.2(5) . 5_677 ? O01 Ti01 Ti02 39.6(4) . 5_677 ? C14 Ti01 Ti02 109.4(10) . 5_677 ? C16 Ti01 Ti02 162.8(9) . 5_677 ? C13 Ti01 Ti02 106.9(9) . 5_677 ? C17 Ti01 Ti02 133.2(9) . 5_677 ? C15 Ti01 Ti02 139.0(9) . 5_677 ? Ti03 Ti01 Ti02 60.17(15) . 5_677 ? Ti03 Ti01 Ti02 60.08(15) 5_677 5_677 ? O01 Ti03 O02 79.1(7) 5_677 5_677 ? O01 Ti03 O03 78.8(7) 5_677 . ? O02 Ti03 O03 126.8(7) 5_677 . ? O01 Ti03 O04 127.2(7) 5_677 . ? O02 Ti03 O04 78.8(7) 5_677 . ? O03 Ti03 O04 77.4(7) . . ? O01 Ti03 C26 131.6(9) 5_677 . ? O02 Ti03 C26 93.6(9) 5_677 . ? O03 Ti03 C26 135.9(9) . . ? O04 Ti03 C26 97.1(10) . . ? O01 Ti03 C25 97.1(10) 5_677 . ? O02 Ti03 C25 93.9(10) 5_677 . ? O03 Ti03 C25 136.5(10) . . ? O04 Ti03 C25 131.7(10) . . ? C26 Ti03 C25 35.2(11) . . ? O01 Ti03 C24 89.5(10) 5_677 . ? O02 Ti03 C24 124.4(10) 5_677 . ? O03 Ti03 C24 103.1(9) . . ? O04 Ti03 C24 141.7(10) . . ? C26 Ti03 C24 55.5(11) . . ? C25 Ti03 C24 33.4(11) . . ? O01 Ti03 C23 114.4(9) 5_677 . ? O02 Ti03 C23 150.2(9) 5_677 . ? O03 Ti03 C23 82.7(9) . . ? O04 Ti03 C23 108.5(9) . . ? C26 Ti03 C23 57.2(11) . . ? C25 Ti03 C23 59.3(11) . . ? C24 Ti03 C23 35.9(11) . . ? O01 Ti03 C27 145.0(10) 5_677 . ? O02 Ti03 C27 123.6(10) 5_677 . ? O03 Ti03 C27 101.2(9) . . ? O04 Ti03 C27 86.0(10) . . ? C26 Ti03 C27 34.9(10) . . ? C25 Ti03 C27 58.6(11) . . ? C24 Ti03 C27 56.0(12) . . ? C23 Ti03 C27 33.1(11) . . ? O01 Ti03 Ti01 96.9(5) 5_677 . ? O02 Ti03 Ti01 97.6(5) 5_677 . ? O03 Ti03 Ti01 39.1(5) . . ? O04 Ti03 Ti01 40.6(5) . . ? C26 Ti03 Ti01 131.4(8) . . ? C25 Ti03 Ti01 163.4(8) . . ? C24 Ti03 Ti01 138.0(8) . . ? C23 Ti03 Ti01 106.4(8) . . ? C27 Ti03 Ti01 104.8(8) . . ? O01 Ti03 Ti01 40.5(5) 5_677 5_677 ? O02 Ti03 Ti01 40.5(5) 5_677 5_677 ? O03 Ti03 Ti01 98.0(5) . 5_677 ? O04 Ti03 Ti01 98.2(5) . 5_677 ? C26 Ti03 Ti01 125.9(7) . 5_677 ? C25 Ti03 Ti01 106.4(8) . 5_677 ? C24 Ti03 Ti01 119.2(9) . 5_677 ? C23 Ti03 Ti01 152.7(8) . 5_677 ? C27 Ti03 Ti01 160.8(8) . 5_677 ? Ti01 Ti03 Ti01 90.06(16) . 5_677 ? O01 Ti03 Ti02 39.3(5) 5_677 . ? O02 Ti03 Ti02 97.8(5) 5_677 . ? O03 Ti03 Ti02 41.2(5) . . ? O04 Ti03 Ti02 98.3(5) . . ? C26 Ti03 Ti02 162.3(9) . . ? C25 Ti03 Ti02 129.9(9) . . ? C24 Ti03 Ti02 106.8(8) . . ? C23 Ti03 Ti02 109.2(8) . . ? C27 Ti03 Ti02 138.2(9) . . ? Ti01 Ti03 Ti02 60.25(15) . . ? Ti01 Ti03 Ti02 60.05(15) 5_677 . ? O01 Ti02 O02 125.4(7) 5_677 . ? O01 Ti02 O04 78.6(7) 5_677 5_677 ? O02 Ti02 O04 78.5(7) . 5_677 ? O01 Ti02 O03 78.4(7) 5_677 . ? O02 Ti02 O03 77.2(6) . . ? O04 Ti02 O03 127.0(7) 5_677 . ? O01 Ti02 C19 127.4(10) 5_677 . ? O02 Ti02 C19 101.0(10) . . ? O04 Ti02 C19 89.1(9) 5_677 . ? O03 Ti02 C19 141.5(10) . . ? O01 Ti02 C18 145.0(10) 5_677 . ? O02 Ti02 C18 89.2(10) . . ? O04 Ti02 C18 118.2(10) 5_677 . ? O03 Ti02 C18 107.8(9) . . ? C19 Ti02 C18 34.1(10) . . ? O01 Ti02 C20 95.1(9) 5_677 . ? O02 Ti02 C20 133.9(9) . . ? O04 Ti02 C20 90.6(9) 5_677 . ? O03 Ti02 C20 138.6(9) . . ? C19 Ti02 C20 33.5(11) . . ? C18 Ti02 C20 56.9(11) . . ? O01 Ti02 C21 89.8(10) 5_677 . ? O02 Ti02 C21 143.3(9) . . ? O04 Ti02 C21 123.2(9) 5_677 . ? O03 Ti02 C21 103.8(10) . . ? C19 Ti02 C21 55.2(12) . . ? C18 Ti02 C21 55.2(12) . . ? C20 Ti02 C21 34.8(10) . . ? O01 Ti02 C22 114.5(10) 5_677 . ? O02 Ti02 C22 111.7(10) . . ? O04 Ti02 C22 146.9(10) 5_677 . ? O03 Ti02 C22 86.1(10) . . ? C19 Ti02 C22 58.4(12) . . ? C18 Ti02 C22 35.4(11) . . ? C20 Ti02 C22 59.2(11) . . ? C21 Ti02 C22 33.8(11) . . ? O01 Ti02 Ti01 40.4(5) 5_677 5_677 ? O02 Ti02 Ti01 96.6(5) . 5_677 ? O04 Ti02 Ti01 40.2(5) 5_677 5_677 ? O03 Ti02 Ti01 97.6(5) . 5_677 ? C19 Ti02 Ti01 120.6(8) . 5_677 ? C18 Ti02 Ti01 154.6(8) . 5_677 ? C20 Ti02 Ti01 103.3(8) . 5_677 ? C21 Ti02 Ti01 119.2(8) . 5_677 ? C22 Ti02 Ti01 151.6(9) . 5_677 ? O01 Ti02 Ti03 39.1(5) 5_677 . ? O02 Ti02 Ti03 97.1(5) . . ? O04 Ti02 Ti03 97.7(5) 5_677 . ? O03 Ti02 Ti03 40.9(5) . . ? C19 Ti02 Ti03 161.6(9) . . ? C18 Ti02 Ti03 144.1(9) . . ? C20 Ti02 Ti03 128.9(8) . . ? C21 Ti02 Ti03 107.4(9) . . ? C22 Ti02 Ti03 111.5(8) . . ? Ti01 Ti02 Ti03 59.87(15) 5_677 . ? O01 Ti02 Ti03 97.0(5) 5_677 5_677 ? O02 Ti02 Ti03 39.5(5) . 5_677 ? O04 Ti02 Ti03 41.1(5) 5_677 5_677 ? O03 Ti02 Ti03 96.2(5) . 5_677 ? C19 Ti02 Ti03 106.5(8) . 5_677 ? C18 Ti02 Ti03 115.9(9) . 5_677 ? C20 Ti02 Ti03 125.3(8) . 5_677 ? C21 Ti02 Ti03 159.8(9) . 5_677 ? C22 Ti02 Ti03 148.2(8) . 5_677 ? Ti01 Ti02 Ti03 59.73(15) 5_677 5_677 ? Ti03 Ti02 Ti03 89.57(17) . 5_677 ? Sn02 S03 H03 109.5 . . ? Sn01 S06 Sn03 104.3(3) . . ? Sn02 S02 Sn01 102.0(3) . . ? Sn01 S01 H01 109.5 . . ? Sn02 S04 Sn03 102.4(3) . . ? Sn03 S05 H05 109.5 . . ? Ti01 O03 Ti03 100.0(7) . . ? Ti01 O03 Ti02 100.4(7) . . ? Ti03 O03 Ti02 97.9(7) . . ? C27 C26 C25 110(3) . . ? C27 C26 Ti03 74.9(19) . . ? C25 C26 Ti03 73.1(19) . . ? C27 C26 H015 125.0 . . ? C25 C26 H015 125.0 . . ? Ti03 C26 H015 118.8 . . ? Ti01 O04 Ti02 99.2(7) . 5_677 ? Ti01 O04 Ti03 98.1(7) . . ? Ti02 O04 Ti03 98.2(7) 5_677 . ? Ti03 O01 Ti02 101.5(7) 5_677 5_677 ? Ti03 O01 Ti01 100.1(7) 5_677 . ? Ti02 O01 Ti01 100.0(7) 5_677 . ? Ti03 O02 Ti02 100.3(7) 5_677 . ? Ti03 O02 Ti01 99.8(7) 5_677 . ? Ti02 O02 Ti01 99.4(7) . . ? C25 C24 C23 113(3) . . ? C25 C24 Ti03 73(2) . . ? C23 C24 Ti03 72.8(18) . . ? C25 C24 H020 123.7 . . ? C23 C24 H020 123.7 . . ? Ti03 C24 H020 121.7 . . ? C01 C02 C03 112(3) . . ? C01 C02 H02A 109.3 . . ? C03 C02 H02A 109.3 . . ? C01 C02 H02B 109.3 . . ? C03 C02 H02B 109.3 . . ? H02A C02 H02B 108.0 . . ? C02 C01 Sn01 113(2) . . ? C02 C01 H02C 108.9 . . ? Sn01 C01 H02C 108.9 . . ? C02 C01 H02D 108.9 . . ? Sn01 C01 H02D 108.9 . . ? H02C C01 H02D 107.7 . . ? C22 C21 C20 114(3) . . ? C22 C21 Ti02 74(2) . . ? C20 C21 Ti02 72(2) . . ? C22 C21 H023 123.0 . . ? C20 C21 H023 123.0 . . ? Ti02 C21 H023 122.2 . . ? C16 C17 C13 110(4) . . ? C16 C17 Ti01 71(2) . . ? C13 C17 Ti01 73(2) . . ? C16 C17 H024 124.8 . . ? C13 C17 H024 124.8 . . ? Ti01 C17 H024 123.0 . . ? C17 C16 C15 110(3) . . ? C17 C16 Ti01 77(2) . . ? C15 C16 Ti01 75.3(19) . . ? C17 C16 H026 124.8 . . ? C15 C16 H026 124.8 . . ? Ti01 C16 H026 114.9 . . ? C07 C06 C05 112(3) . . ? C07 C06 H02E 109.2 . . ? C05 C06 H02E 109.2 . . ? C07 C06 H02F 109.2 . . ? C05 C06 H02F 109.2 . . ? H02E C06 H02F 107.9 . . ? C20 C19 C18 111(3) . . ? C20 C19 Ti02 74(2) . . ? C18 C19 Ti02 74(2) . . ? C20 C19 H030 124.6 . . ? C18 C19 H030 124.6 . . ? Ti02 C19 H030 118.9 . . ? C23 C27 C26 109(3) . . ? C23 C27 Ti03 73(2) . . ? C26 C27 Ti03 70.2(18) . . ? C23 C27 H032 125.7 . . ? C26 C27 H032 125.7 . . ? Ti03 C27 H032 123.1 . . ? C24 C25 C26 104(3) . . ? C24 C25 Ti03 73(2) . . ? C26 C25 Ti03 71.7(18) . . ? C24 C25 H036 128.0 . . ? C26 C25 H036 128.0 . . ? Ti03 C25 H036 119.2 . . ? C07 C08 H04A 109.5 . . ? C07 C08 H04B 109.5 . . ? H04A C08 H04B 109.5 . . ? C07 C08 H04C 109.5 . . ? H04A C08 H04C 109.5 . . ? H04B C08 H04C 109.5 . . ? C27 C23 C24 105(3) . . ? C27 C23 Ti03 74(2) . . ? C24 C23 Ti03 71.3(17) . . ? C27 C23 H042 127.6 . . ? C24 C23 H042 127.6 . . ? Ti03 C23 H042 119.0 . . ? C06 C05 Sn02 113.7(19) . . ? C06 C05 H04D 108.8 . . ? Sn02 C05 H04D 108.8 . . ? C06 C05 H04E 108.8 . . ? Sn02 C05 H04E 108.8 . . ? H04D C05 H04E 107.7 . . ? C16 C15 C14 101(3) . . ? C16 C15 Ti01 69.9(19) . . ? C14 C15 Ti01 69.2(18) . . ? C16 C15 H047 129.3 . . ? C14 C15 H047 129.3 . . ? Ti01 C15 H047 123.5 . . ? C19 C18 C22 110(3) . . ? C19 C18 Ti02 72(2) . . ? C22 C18 Ti02 73.4(19) . . ? C19 C18 H048 125.2 . . ? C22 C18 H048 125.2 . . ? Ti02 C18 H048 121.1 . . ? C06 C07 C08 114(3) . . ? C06 C07 H05A 108.7 . . ? C08 C07 H05A 108.7 . . ? C06 C07 H05B 108.7 . . ? C08 C07 H05B 108.7 . . ? H05A C07 H05B 107.6 . . ? C10 C09 Sn03 115(3) . . ? C10 C09 H00A 108.5 . . ? Sn03 C09 H00A 108.5 . . ? C10 C09 H00B 108.5 . . ? Sn03 C09 H00B 108.5 . . ? H00A C09 H00B 107.5 . . ? C19 C20 C21 104(3) . . ? C19 C20 Ti02 72(2) . . ? C21 C20 Ti02 73(2) . . ? C19 C20 H002 128.0 . . ? C21 C20 H002 128.0 . . ? Ti02 C20 H002 119.2 . . ? C21 C22 C18 101(3) . . ? C21 C22 Ti02 72(2) . . ? C18 C22 Ti02 71.2(19) . . ? C21 C22 H003 129.3 . . ? C18 C22 H003 129.3 . . ? Ti02 C22 H003 119.6 . . ? C11 C10 C09 110(3) . . ? C11 C10 H00C 109.7 . . ? C09 C10 H00C 109.7 . . ? C11 C10 H00D 109.7 . . ? C09 C10 H00D 109.7 . . ? H00C C10 H00D 108.2 . . ? C14 C13 C17 106(4) . . ? C14 C13 Ti01 71(2) . . ? C17 C13 Ti01 74(2) . . ? C14 C13 H005 127.0 . . ? C17 C13 H005 127.0 . . ? Ti01 C13 H005 120.2 . . ? C02 C03 C04 112(3) . . ? C02 C03 H00E 109.1 . . ? C04 C03 H00E 109.1 . . ? C02 C03 H00F 109.1 . . ? C04 C03 H00F 109.1 . . ? H00E C03 H00F 107.8 . . ? C13 C14 C15 111(4) . . ? C13 C14 Ti01 76(2) . . ? C15 C14 Ti01 75(2) . . ? C13 C14 H007 124.4 . . ? C15 C14 H007 124.4 . . ? Ti01 C14 H007 115.8 . . ? C10 C11 C12 117(3) . . ? C10 C11 H00G 108.0 . . ? C12 C11 H00G 108.0 . . ? C10 C11 H00H 108.0 . . ? C12 C11 H00H 108.0 . . ? H00G C11 H00H 107.3 . . ? C11 C12 H00I 109.5 . . ? C11 C12 H00J 109.5 . . ? H00I C12 H00J 109.5 . . ? C11 C12 H00K 109.5 . . ? H00I C12 H00K 109.5 . . ? H00J C12 H00K 109.5 . . ? C03 C04 H01A 109.5 . . ? C03 C04 H01B 109.5 . . ? H01A C04 H01B 109.5 . . ? C03 C04 H01C 109.5 . . ? H01A C04 H01C 109.5 . . ? H01B C04 H01C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.365 _refine_diff_density_min -2.019 _refine_diff_density_rms 0.405