# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1093 data_(C5H4SiMe3)2Ti(SCCBu)2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H44 S2 Si2 Ti' _chemical_formula_weight 548.83 _chemical_melting_point ? _chemical_compound_source ? 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' 'Si' 'Si' 0.0817 0.0704 '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' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.470(6) _cell_length_b 14.170(7) _cell_length_c 21.405(11) _cell_angle_alpha 94.04(3) _cell_angle_beta 104.40(3) _cell_angle_gamma 106.26(4) _cell_volume 3197.9(28) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needles _exptl_crystal_colour 'deep brown' _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.140 _exptl_crystal_density_method ? _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.487 _exptl_absorpt_correction_type ? _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 MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9746 _diffrn_reflns_av_R_equivalents 0.1162 _diffrn_reflns_av_sigmaI/netI 0.3482 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 23.53 _reflns_number_total 9454 _reflns_number_observed 3174 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2927 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6527 _refine_ls_number_parameters 547 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2820 _refine_ls_R_factor_obs 0.0902 _refine_ls_wR_factor_all 0.1703 _refine_ls_wR_factor_obs 0.1122 _refine_ls_goodness_of_fit_all 0.967 _refine_ls_goodness_of_fit_obs 1.185 _refine_ls_restrained_S_all 0.989 _refine_ls_restrained_S_obs 1.185 _refine_ls_shift/esd_max 0.014 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ti1 Ti 0.3455(2) 0.65356(15) 0.27042(10) 0.0270(6) Uani 1 d . . S1 S 0.4097(3) 0.8004(2) 0.3535(2) 0.0314(9) Uani 1 d . . S2 S 0.2918(3) 0.7477(2) 0.1817(2) 0.0341(9) Uani 1 d . . Si1 Si 0.3030(4) 0.5936(3) 0.4403(2) 0.0426(11) Uani 1 d . . Si2 Si 0.4006(3) 0.5740(3) 0.1048(2) 0.0387(10) Uani 1 d . . C1 C 0.1656(10) 0.6350(8) 0.3099(6) 0.028(2) Uani 1 d . . H1A H 0.1426(10) 0.6893(8) 0.3273(6) 0.033 Uiso 1 d R . C2 C 0.1240(10) 0.5899(9) 0.2445(6) 0.038(4) Uani 1 d . . H2A H 0.0641(10) 0.6059(9) 0.2103(6) 0.046 Uiso 1 d R . C3 C 0.1710(10) 0.5086(8) 0.2408(6) 0.037(3) Uani 1 d . . H3A H 0.1497(10) 0.4597(8) 0.2031(6) 0.044 Uiso 1 d R . C4 C 0.2383(10) 0.5048(8) 0.3039(6) 0.032(3) Uani 1 d . . H4A H 0.2745(10) 0.4528(8) 0.3156(6) 0.039 Uiso 1 d R . C5 C 0.2410(10) 0.5823(8) 0.3491(6) 0.031(3) Uani 1 d . . C6 C 0.2290(11) 0.4696(8) 0.4602(6) 0.061(4) Uani 1 d . . H6A H 0.2553(11) 0.4208(8) 0.4388(6) 0.091 Uiso 1 d R . H6B H 0.2556(11) 0.4707(8) 0.5066(6) 0.091 Uiso 1 d R . H6C H 0.1385(11) 0.4531(8) 0.4457(6) 0.091 Uiso 1 d R . C7 C 0.2519(11) 0.6900(8) 0.4801(6) 0.058(4) Uani 1 d . . H7A H 0.2838(11) 0.6956(8) 0.5265(6) 0.087 Uiso 1 d R . H7B H 0.2859(11) 0.7524(8) 0.4664(6) 0.087 Uiso 1 d R . H7C H 0.1612(11) 0.6723(8) 0.4681(6) 0.087 Uiso 1 d R . C8 C 0.4778(9) 0.6186(8) 0.4663(5) 0.046(4) Uani 1 d . . H8A H 0.4988(9) 0.5667(8) 0.4445(5) 0.069 Uiso 1 d R . H8B H 0.5190(9) 0.6814(8) 0.4553(5) 0.069 Uiso 1 d R . H8C H 0.5056(9) 0.6200(8) 0.5127(5) 0.069 Uiso 1 d R . C9 C 0.4438(9) 0.5391(8) 0.2402(5) 0.028(2) Uani 1 d . . H9A H 0.4030(9) 0.4688(8) 0.2280(5) 0.033 Uiso 1 d R . C10 C 0.5112(10) 0.5848(8) 0.3033(5) 0.032(3) Uani 1 d . . H10A H 0.5254(10) 0.5521(8) 0.3410(5) 0.038 Uiso 1 d R . C11 C 0.5662(9) 0.6848(7) 0.3005(6) 0.030(3) Uani 1 d . . H11A H 0.6261(9) 0.7328(7) 0.3361(6) 0.036 Uiso 1 d R . C12 C 0.5287(9) 0.6996(8) 0.2355(5) 0.022(3) Uani 1 d . . H12A H 0.5580(9) 0.7600(8) 0.2185(5) 0.026 Uiso 1 d R . C13 C 0.4521(10) 0.6071(8) 0.1956(6) 0.030(3) Uani 1 d . . C14 C 0.2249(10) 0.5187(8) 0.0726(5) 0.045(4) Uani 1 d . . H14A H 0.1970(10) 0.4614(8) 0.0929(5) 0.068 Uiso 1 d R . H14B H 0.1852(10) 0.5671(8) 0.0823(5) 0.068 Uiso 1 d R . H14C H 0.2022(10) 0.4993(8) 0.0262(5) 0.068 Uiso 1 d R . C15 C 0.4753(12) 0.4794(8) 0.0884(6) 0.060(4) Uani 1 d . . H15A H 0.5655(12) 0.5078(8) 0.1049(6) 0.091 Uiso 1 d R . H15B H 0.4471(12) 0.4237(8) 0.1099(6) 0.091 Uiso 1 d R . H15C H 0.4530(12) 0.4577(8) 0.0423(6) 0.091 Uiso 1 d R . C16 C 0.4611(10) 0.6853(8) 0.0686(6) 0.042(4) Uani 1 d . . H16A H 0.5514(10) 0.7116(8) 0.0861(6) 0.063 Uiso 1 d R . H16B H 0.4401(10) 0.6671(8) 0.0222(6) 0.063 Uiso 1 d R . H16C H 0.4230(10) 0.7348(8) 0.0782(6) 0.063 Uiso 1 d R . C17 C 0.5418(11) 0.8807(8) 0.3441(5) 0.030(2) Uani 1 d . . C18 C 0.6349(11) 0.9378(8) 0.3399(6) 0.037(3) Uani 1 d . . C19 C 0.7549(11) 1.0011(9) 0.3293(6) 0.037(3) Uani 1 d . . C20 C 0.8505(10) 0.9446(10) 0.3397(7) 0.067(5) Uani 1 d . . H20A H 0.8192(10) 0.8840(10) 0.3093(7) 0.101 Uiso 1 d R . H20B H 0.9293(10) 0.9844(10) 0.3346(7) 0.101 Uiso 1 d R . H20C H 0.8632(10) 0.9292(10) 0.3834(7) 0.101 Uiso 1 d R . C21 C 0.8073(10) 1.0965(9) 0.3768(7) 0.071(5) Uani 1 d . . H21A H 0.7479(10) 1.1335(9) 0.3694(7) 0.106 Uiso 1 d R . H21B H 0.8202(10) 1.0805(9) 0.4204(7) 0.106 Uiso 1 d R . H21C H 0.8863(10) 1.1358(9) 0.3715(7) 0.106 Uiso 1 d R . C22 C 0.7285(11) 1.0229(10) 0.2584(6) 0.073(5) Uani 1 d . . H22A H 0.6681(11) 1.0590(10) 0.2514(6) 0.109 Uiso 1 d R . H22B H 0.8048(11) 1.0612(10) 0.2499(6) 0.109 Uiso 1 d R . H22C H 0.6941(11) 0.9606(10) 0.2297(6) 0.109 Uiso 1 d R . C23 C 0.1441(11) 0.7610(8) 0.1681(5) 0.030(2) Uani 1 d . . C24 C 0.0453(13) 0.7699(11) 0.1534(8) 0.080(4) Uani 1 d . . C25 C -0.0894(11) 0.7610(8) 0.1347(6) 0.039(3) Uani 1 d . . C26 C -0.1148(11) 0.8485(10) 0.1060(7) 0.080(4) Uani 1 d . . H26A H -0.0864(11) 0.8523(10) 0.0674(7) 0.121 Uiso 1 d R . H26B H -0.2023(11) 0.8454(10) 0.0951(7) 0.121 Uiso 1 d R . H26C H -0.0654(11) 0.9063(10) 0.1376(7) 0.121 Uiso 1 d R . C27 C -0.1629(13) 0.6720(15) 0.0870(10) 0.217(14) Uani 1 d . . H27A H -0.1368(13) 0.6722(15) 0.0477(10) 0.325 Uiso 1 d R . H27B H -0.1465(13) 0.6179(15) 0.1084(10) 0.325 Uiso 1 d R . H27C H -0.2518(13) 0.6643(15) 0.0764(10) 0.325 Uiso 1 d R . C28 C -0.1419(14) 0.7571(16) 0.1918(9) 0.178(11) Uani 1 d . . H28A H -0.1326(14) 0.6987(16) 0.2100(9) 0.267 Uiso 1 d R . H28B H -0.0925(14) 0.8151(16) 0.2232(9) 0.267 Uiso 1 d R . H28C H -0.2294(14) 0.7543(16) 0.1807(9) 0.267 Uiso 1 d R . Ti2 Ti 0.3018(2) 0.17089(14) 0.26556(10) 0.0265(6) Uani 1 d . . S3 S 0.2717(3) 0.2577(2) 0.1712(2) 0.0333(9) Uani 1 d . . S4 S 0.4188(3) 0.3197(2) 0.3456(2) 0.0324(9) Uani 1 d . . Si3 Si 0.2528(4) 0.0638(3) 0.4238(2) 0.0496(12) Uani 1 d . . Si4 Si 0.3547(3) 0.0753(3) 0.0981(2) 0.0377(10) Uani 1 d . . C29 C 0.1697(9) 0.1919(8) 0.3333(5) 0.032(3) Uani 1 d . . H29A H 0.1948(9) 0.2459(8) 0.3684(5) 0.038 Uiso 1 d R . C30 C 0.1037(10) 0.1923(9) 0.2683(6) 0.042(2) Uani 1 d . . H30A H 0.0718(10) 0.2446(9) 0.2526(6) 0.051 Uiso 1 d R . C31 C 0.0841(10) 0.0983(9) 0.2353(6) 0.042(3) Uani 1 d . . H31A H 0.0329(10) 0.0746(9) 0.1911(6) 0.050 Uiso 1 d R . C32 C 0.1332(10) 0.0418(9) 0.2771(6) 0.042(3) Uani 1 d . . H32A H 0.1223(10) -0.0279(9) 0.2676(6) 0.050 Uiso 1 d R . C33 C 0.1917(10) 0.0999(8) 0.3421(6) 0.035(2) Uani 1 d . . C34 C 0.4282(11) 0.1018(9) 0.4549(6) 0.064(4) Uani 1 d . . H34A H 0.4617(11) 0.1729(9) 0.4599(6) 0.096 Uiso 1 d R . H34B H 0.4527(11) 0.0800(9) 0.4962(6) 0.096 Uiso 1 d R . H34C H 0.4608(11) 0.0721(9) 0.4241(6) 0.096 Uiso 1 d R . C35 C 0.1937(13) 0.1264(10) 0.4832(6) 0.085(5) Uani 1 d . . H35A H 0.2305(13) 0.1970(10) 0.4869(6) 0.127 Uiso 1 d R . H35B H 0.1032(13) 0.1094(10) 0.4683(6) 0.127 Uiso 1 d R . H35C H 0.2178(13) 0.1059(10) 0.5250(6) 0.127 Uiso 1 d R . C36 C 0.1859(11) -0.0750(9) 0.4139(7) 0.077(5) Uani 1 d . . H36A H 0.2145(11) -0.0977(9) 0.4545(7) 0.116 Uiso 1 d R . H36B H 0.0952(11) -0.0934(9) 0.4012(7) 0.116 Uiso 1 d R . H36C H 0.2132(11) -0.1050(9) 0.3809(7) 0.116 Uiso 1 d R . C37 C 0.3439(11) 0.0264(8) 0.2262(6) 0.040(3) Uani 1 d . . H37A H 0.2805(11) -0.0363(8) 0.2075(6) 0.047 Uiso 1 d R . C38 C 0.4096(11) 0.0542(9) 0.2924(6) 0.042(2) Uani 1 d . . H38A H 0.4008(11) 0.0135(9) 0.3260(6) 0.051 Uiso 1 d R . C39 C 0.4991(11) 0.1448(8) 0.2987(6) 0.036(2) Uani 1 d . . H39A H 0.5652(11) 0.1777(8) 0.3377(6) 0.043 Uiso 1 d R . C40 C 0.4861(11) 0.1768(9) 0.2359(5) 0.036(2) Uani 1 d . . H40A H 0.5411(11) 0.2340(9) 0.2250(5) 0.043 Uiso 1 d R . C41 C 0.3930(10) 0.0977(8) 0.1892(6) 0.035(2) Uani 1 d . . C42 C 0.4294(11) -0.0232(9) 0.0832(6) 0.058(4) Uani 1 d . . H42A H 0.3911(11) -0.0810(9) 0.1005(6) 0.087 Uiso 1 d R . H42B H 0.4160(11) -0.0403(9) 0.0373(6) 0.087 Uiso 1 d R . H42C H 0.5185(11) 0.0007(9) 0.1047(6) 0.087 Uiso 1 d R . C43 C 0.4290(11) 0.1878(8) 0.0637(6) 0.058(4) Uani 1 d . . H43A H 0.3913(11) 0.2387(8) 0.0710(6) 0.088 Uiso 1 d R . H43B H 0.5181(11) 0.2118(8) 0.0851(6) 0.088 Uiso 1 d R . H43C H 0.4156(11) 0.1709(8) 0.0177(6) 0.088 Uiso 1 d R . C44 C 0.1824(10) 0.0266(9) 0.0605(6) 0.064(4) Uani 1 d . . H44A H 0.1452(10) 0.0777(9) 0.0679(6) 0.096 Uiso 1 d R . H44B H 0.1654(10) 0.0074(9) 0.0145(6) 0.096 Uiso 1 d R . H44C H 0.1466(10) -0.0300(9) 0.0795(6) 0.096 Uiso 1 d R . C45 C 0.1284(11) 0.2686(8) 0.1434(5) 0.029(2) Uani 1 d . . C46 C 0.0247(11) 0.2744(8) 0.1201(6) 0.035(3) Uani 1 d . . C47 C -0.1082(12) 0.2732(10) 0.0851(7) 0.049(4) Uani 1 d . . C48 C -0.1243(13) 0.3732(11) 0.1079(8) 0.102(6) Uani 1 d . . H48A H -0.1143(13) 0.3832(11) 0.1540(8) 0.152 Uiso 1 d R . H48B H -0.0603(13) 0.4245(11) 0.0975(8) 0.152 Uiso 1 d R . H48C H -0.2064(13) 0.3756(11) 0.0848(8) 0.152 Uiso 1 d R . C49 C -0.2002(11) 0.1871(11) 0.1014(8) 0.098(6) Uani 1 d . . H49A H -0.1891(11) 0.1940(11) 0.1477(8) 0.146 Uiso 1 d R . H49B H -0.2850(11) 0.1847(11) 0.0793(8) 0.146 Uiso 1 d R . H49C H -0.1853(11) 0.1268(11) 0.0873(8) 0.146 Uiso 1 d R . C50 C -0.1264(11) 0.2629(10) 0.0134(6) 0.068(4) Uani 1 d . . H50A H -0.1189(11) 0.2000(10) -0.0015(6) 0.103 Uiso 1 d R . H50B H -0.2085(11) 0.2667(10) -0.0086(6) 0.103 Uiso 1 d R . H50C H -0.0624(11) 0.3156(10) 0.0042(6) 0.103 Uiso 1 d R . C51 C 0.5651(11) 0.3686(8) 0.3374(5) 0.029(2) Uani 1 d . . C52 C 0.6670(11) 0.4054(8) 0.3329(6) 0.038(3) Uani 1 d . . C53 C 0.7904(12) 0.4509(10) 0.3208(7) 0.051(4) Uani 1 d . . C54 C 0.8646(12) 0.3791(11) 0.3216(9) 0.121(8) Uani 1 d . . H54A H 0.8189(12) 0.3226(11) 0.2883(9) 0.181 Uiso 1 d R . H54B H 0.9444(12) 0.4116(11) 0.3142(9) 0.181 Uiso 1 d R . H54C H 0.8788(12) 0.3576(11) 0.3636(9) 0.181 Uiso 1 d R . C55 C 0.7704(13) 0.4857(12) 0.2543(7) 0.104(6) Uani 1 d . . H55A H 0.7224(13) 0.4287(12) 0.2218(7) 0.156 Uiso 1 d R . H55B H 0.7236(13) 0.5324(12) 0.2532(7) 0.156 Uiso 1 d R . H55C H 0.8495(13) 0.5164(12) 0.2457(7) 0.156 Uiso 1 d R . C56 C 0.8656(13) 0.5400(13) 0.3731(8) 0.133(8) Uani 1 d . . H56A H 0.8195(13) 0.5871(13) 0.3729(8) 0.199 Uiso 1 d R . H56B H 0.8798(13) 0.5172(13) 0.4147(8) 0.199 Uiso 1 d R . H56C H 0.9454(13) 0.5712(13) 0.3653(8) 0.199 Uiso 1 d 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 Ti1 0.0261(14) 0.0300(14) 0.0271(15) 0.0098(12) 0.0104(12) 0.0081(11) S1 0.030(2) 0.029(2) 0.035(2) 0.001(2) 0.014(2) 0.005(2) S2 0.028(2) 0.038(2) 0.038(2) 0.013(2) 0.010(2) 0.012(2) Si1 0.054(3) 0.044(2) 0.032(2) 0.010(2) 0.016(2) 0.013(2) Si2 0.052(3) 0.034(2) 0.032(2) 0.006(2) 0.018(2) 0.010(2) C1 0.025(5) 0.023(5) 0.041(6) 0.000(5) 0.017(5) 0.008(4) C2 0.013(7) 0.050(9) 0.041(9) 0.014(8) 0.002(7) -0.003(7) C3 0.028(8) 0.032(8) 0.030(8) 0.003(7) 0.001(7) -0.014(6) C4 0.034(8) 0.015(7) 0.045(9) 0.007(7) 0.015(7) 0.001(6) C5 0.032(8) 0.034(8) 0.031(8) 0.015(7) 0.022(7) 0.002(6) C6 0.084(11) 0.062(10) 0.045(9) 0.027(8) 0.027(9) 0.022(8) C7 0.084(11) 0.067(10) 0.046(9) 0.019(8) 0.035(9) 0.043(9) C8 0.045(9) 0.061(9) 0.031(8) 0.011(7) 0.006(7) 0.017(7) C9 0.025(5) 0.023(5) 0.041(6) 0.000(5) 0.017(5) 0.008(4) C10 0.034(8) 0.035(8) 0.028(8) 0.012(7) 0.001(7) 0.017(6) C11 0.026(7) 0.013(7) 0.051(9) -0.001(6) 0.006(7) 0.011(6) C12 0.023(7) 0.020(7) 0.032(8) 0.009(6) 0.016(6) 0.014(6) C13 0.044(8) 0.026(8) 0.034(8) 0.008(7) 0.028(7) 0.015(7) C14 0.061(10) 0.040(9) 0.026(8) -0.010(7) 0.011(7) 0.008(7) C15 0.098(11) 0.041(9) 0.055(10) 0.005(8) 0.052(9) 0.016(8) C16 0.046(9) 0.059(9) 0.039(9) 0.014(8) 0.025(7) 0.030(7) C17 0.045(6) 0.024(5) 0.023(5) 0.005(4) 0.012(5) 0.009(5) C18 0.042(9) 0.021(7) 0.046(9) 0.002(7) 0.015(7) 0.007(7) C19 0.028(8) 0.033(8) 0.046(9) 0.001(7) 0.014(7) 0.001(7) C20 0.039(9) 0.097(12) 0.095(13) 0.056(11) 0.050(9) 0.027(9) C21 0.025(8) 0.067(11) 0.093(13) 0.018(10) 0.004(9) -0.017(8) C22 0.064(10) 0.092(12) 0.094(13) 0.064(10) 0.061(10) 0.028(9) C23 0.045(6) 0.024(5) 0.023(5) 0.005(4) 0.012(5) 0.009(5) C24 0.032(7) 0.081(9) 0.125(11) 0.041(8) 0.005(7) 0.021(6) C25 0.025(8) 0.024(8) 0.055(10) -0.001(7) 0.003(7) -0.002(6) C26 0.032(7) 0.081(9) 0.125(11) 0.041(8) 0.005(7) 0.021(6) C27 0.015(10) 0.236(25) 0.296(30) -0.220(22) -0.045(14) 0.019(13) C28 0.070(14) 0.377(34) 0.148(19) 0.089(21) 0.084(14) 0.103(17) Ti2 0.0243(14) 0.0245(14) 0.0303(15) 0.0068(12) 0.0071(12) 0.0067(11) S3 0.032(2) 0.036(2) 0.036(2) 0.013(2) 0.012(2) 0.013(2) S4 0.026(2) 0.037(2) 0.031(2) 0.005(2) 0.005(2) 0.008(2) Si3 0.053(3) 0.065(3) 0.040(3) 0.020(2) 0.021(2) 0.024(2) Si4 0.041(2) 0.038(2) 0.038(3) 0.008(2) 0.018(2) 0.011(2) C29 0.015(7) 0.058(9) 0.026(8) 0.011(7) 0.011(6) 0.011(6) C30 0.041(6) 0.047(6) 0.051(7) 0.024(5) 0.011(5) 0.031(5) C31 0.018(5) 0.043(7) 0.059(8) 0.009(5) 0.014(5) -0.005(4) C32 0.018(5) 0.043(7) 0.059(8) 0.009(5) 0.014(5) -0.005(4) C33 0.033(6) 0.026(6) 0.055(7) 0.016(5) 0.021(5) 0.012(5) C34 0.067(11) 0.070(11) 0.040(10) 0.000(8) 0.002(8) 0.013(9) C35 0.111(13) 0.131(14) 0.047(10) 0.029(10) 0.046(10) 0.068(12) C36 0.062(10) 0.067(11) 0.115(14) 0.051(10) 0.027(10) 0.028(9) C37 0.048(9) 0.024(7) 0.043(9) 0.002(7) 0.012(7) 0.008(6) C38 0.041(6) 0.047(6) 0.051(7) 0.024(5) 0.011(5) 0.031(5) C39 0.043(6) 0.039(6) 0.035(6) 0.015(5) 0.009(5) 0.027(5) C40 0.043(6) 0.039(6) 0.035(6) 0.015(5) 0.009(5) 0.027(5) C41 0.033(6) 0.026(6) 0.055(7) 0.016(5) 0.021(5) 0.012(5) C42 0.079(11) 0.058(10) 0.038(9) 0.007(8) 0.013(8) 0.024(8) C43 0.087(11) 0.044(9) 0.057(11) 0.027(8) 0.036(9) 0.022(8) C44 0.050(10) 0.069(11) 0.066(11) 0.001(9) 0.017(8) 0.007(8) C45 0.044(6) 0.024(5) 0.024(5) 0.001(4) 0.011(5) 0.017(5) C46 0.031(8) 0.029(8) 0.042(9) -0.001(6) 0.006(7) 0.010(7) C47 0.039(9) 0.053(10) 0.044(10) -0.009(8) -0.003(8) 0.015(8) C48 0.070(12) 0.096(14) 0.125(16) -0.026(12) -0.016(11) 0.052(11) C49 0.031(9) 0.119(15) 0.127(16) 0.041(13) 0.007(10) 0.006(10) C50 0.041(9) 0.101(13) 0.042(10) -0.023(9) -0.021(8) 0.026(9) C51 0.044(6) 0.024(5) 0.024(5) 0.001(4) 0.011(5) 0.017(5) C52 0.028(8) 0.039(8) 0.038(9) 0.002(7) 0.009(7) -0.003(7) C53 0.023(8) 0.055(10) 0.057(11) 0.008(9) 0.005(8) -0.008(7) C54 0.039(11) 0.132(16) 0.222(23) 0.091(16) 0.054(13) 0.044(11) C55 0.080(13) 0.164(18) 0.076(13) 0.024(13) 0.046(11) 0.027(12) C56 0.065(12) 0.172(19) 0.115(16) -0.040(15) 0.061(12) -0.052(12) _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 C12 2.342(9) . ? Ti1 C3 2.347(10) . ? Ti1 C2 2.350(11) . ? Ti1 C10 2.350(10) . ? Ti1 C11 2.354(10) . ? Ti1 C9 2.358(10) . ? Ti1 C1 2.374(10) . ? Ti1 C4 2.381(10) . ? Ti1 C13 2.402(10) . ? Ti1 C5 2.421(10) . ? Ti1 S2 2.451(4) . ? Ti1 S1 2.451(4) . ? S1 C17 1.688(11) . ? S2 C23 1.712(12) . ? Si1 C6 1.855(10) . ? Si1 C7 1.861(11) . ? Si1 C8 1.864(11) . ? Si1 C5 1.883(12) . ? Si2 C15 1.838(11) . ? Si2 C16 1.843(10) . ? Si2 C13 1.868(12) . ? Si2 C14 1.871(11) . ? C1 C2 1.402(15) . ? C1 C5 1.448(13) . ? C2 C3 1.407(14) . ? C3 C4 1.391(14) . ? C4 C5 1.402(14) . ? C9 C10 1.386(14) . ? C9 C13 1.404(12) . ? C10 C11 1.392(12) . ? C11 C12 1.400(13) . ? C12 C13 1.429(14) . ? C17 C18 1.174(13) . ? C18 C19 1.498(14) . ? C19 C21 1.51(2) . ? C19 C20 1.513(14) . ? C19 C22 1.542(15) . ? C23 C24 1.144(14) . ? C24 C25 1.46(2) . ? C25 C27 1.46(2) . ? C25 C26 1.490(14) . ? C25 C28 1.49(2) . ? Ti2 C31 2.318(11) . ? Ti2 C39 2.339(11) . ? Ti2 C40 2.336(11) . ? Ti2 C32 2.339(10) . ? Ti2 C38 2.350(10) . ? Ti2 C37 2.376(11) . ? Ti2 C30 2.389(11) . ? Ti2 C29 2.402(10) . ? Ti2 C33 2.416(11) . ? Ti2 S4 2.438(4) . ? Ti2 S3 2.439(4) . ? Ti2 C41 2.462(12) . ? S3 C45 1.658(12) . ? S4 C51 1.685(12) . ? Si3 C34 1.859(12) . ? Si3 C35 1.863(12) . ? Si3 C36 1.876(12) . ? Si3 C33 1.878(12) . ? Si4 C44 1.843(11) . ? Si4 C41 1.873(13) . ? Si4 C42 1.877(11) . ? Si4 C43 1.878(10) . ? C29 C30 1.410(14) . ? C29 C33 1.412(13) . ? C30 C31 1.395(15) . ? C31 C32 1.364(14) . ? C32 C33 1.46(2) . ? C37 C38 1.398(14) . ? C37 C41 1.407(13) . ? C38 C39 1.374(14) . ? C39 C40 1.436(13) . ? C40 C41 1.427(15) . ? C45 C46 1.199(13) . ? C46 C47 1.516(15) . ? C47 C50 1.487(15) . ? C47 C49 1.50(2) . ? C47 C48 1.54(2) . ? C51 C52 1.171(13) . ? C52 C53 1.477(15) . ? C53 C54 1.50(2) . ? C53 C56 1.52(2) . ? C53 C55 1.52(2) . ? 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 C12 Ti1 C3 131.1(4) . . ? C12 Ti1 C2 149.1(4) . . ? C3 Ti1 C2 34.9(3) . . ? C12 Ti1 C10 57.5(3) . . ? C3 Ti1 C10 100.4(4) . . ? C2 Ti1 C10 134.0(4) . . ? C12 Ti1 C11 34.7(3) . . ? C3 Ti1 C11 134.1(4) . . ? C2 Ti1 C11 168.5(4) . . ? C10 Ti1 C11 34.4(3) . . ? C12 Ti1 C9 56.6(3) . . ? C3 Ti1 C9 80.5(4) . . ? C2 Ti1 C9 114.2(4) . . ? C10 Ti1 C9 34.2(3) . . ? C11 Ti1 C9 56.6(4) . . ? C12 Ti1 C1 170.7(4) . . ? C3 Ti1 C1 57.4(4) . . ? C2 Ti1 C1 34.5(4) . . ? C10 Ti1 C1 128.3(4) . . ? C11 Ti1 C1 144.9(4) . . ? C9 Ti1 C1 132.6(4) . . ? C12 Ti1 C4 132.6(4) . . ? C3 Ti1 C4 34.2(3) . . ? C2 Ti1 C4 56.8(4) . . ? C10 Ti1 C4 79.3(4) . . ? C11 Ti1 C4 112.2(4) . . ? C9 Ti1 C4 77.0(4) . . ? C1 Ti1 C4 56.1(4) . . ? C12 Ti1 C13 35.0(3) . . ? C3 Ti1 C13 96.2(4) . . ? C2 Ti1 C13 119.2(5) . . ? C10 Ti1 C13 58.1(4) . . ? C11 Ti1 C13 58.2(4) . . ? C9 Ti1 C13 34.3(3) . . ? C1 Ti1 C13 152.6(4) . . ? C4 Ti1 C13 107.1(4) . . ? C12 Ti1 C5 149.0(4) . . ? C3 Ti1 C5 58.2(4) . . ? C2 Ti1 C5 58.5(4) . . ? C10 Ti1 C5 93.2(4) . . ? C11 Ti1 C5 115.0(4) . . ? C9 Ti1 C5 105.8(4) . . ? C1 Ti1 C5 35.1(3) . . ? C4 Ti1 C5 33.9(3) . . ? C13 Ti1 C5 139.2(4) . . ? C12 Ti1 S2 76.3(3) . . ? C3 Ti1 S2 101.7(3) . . ? C2 Ti1 S2 81.5(3) . . ? C10 Ti1 S2 132.3(3) . . ? C11 Ti1 S2 107.8(3) . . ? C9 Ti1 S2 110.8(3) . . ? C1 Ti1 S2 99.1(3) . . ? C4 Ti1 S2 135.2(3) . . ? C13 Ti1 S2 77.9(3) . . ? C5 Ti1 S2 134.2(3) . . ? C12 Ti1 S1 95.5(3) . . ? C3 Ti1 S1 133.2(3) . . ? C2 Ti1 S1 106.6(3) . . ? C10 Ti1 S1 102.3(3) . . ? C11 Ti1 S1 80.3(3) . . ? C9 Ti1 S1 135.2(3) . . ? C1 Ti1 S1 76.5(3) . . ? C4 Ti1 S1 113.2(3) . . ? C13 Ti1 S1 130.5(3) . . ? C5 Ti1 S1 80.1(3) . . ? S2 Ti1 S1 92.30(13) . . ? C17 S1 Ti1 107.7(4) . . ? C23 S2 Ti1 114.2(3) . . ? C6 Si1 C7 110.3(5) . . ? C6 Si1 C8 107.7(5) . . ? C7 Si1 C8 112.8(6) . . ? C6 Si1 C5 105.1(5) . . ? C7 Si1 C5 109.2(5) . . ? C8 Si1 C5 111.5(5) . . ? C15 Si2 C16 110.2(5) . . ? C15 Si2 C13 104.6(5) . . ? C16 Si2 C13 109.0(5) . . ? C15 Si2 C14 108.9(6) . . ? C16 Si2 C14 112.0(5) . . ? C13 Si2 C14 111.8(5) . . ? C2 C1 C5 109.9(10) . . ? C2 C1 Ti1 71.8(6) . . ? C5 C1 Ti1 74.2(6) . . ? C1 C2 C3 107.5(11) . . ? C1 C2 Ti1 73.7(6) . . ? C3 C2 Ti1 72.5(6) . . ? C4 C3 C2 107.0(11) . . ? C4 C3 Ti1 74.2(6) . . ? C2 C3 Ti1 72.7(6) . . ? C3 C4 C5 112.2(11) . . ? C3 C4 Ti1 71.6(6) . . ? C5 C4 Ti1 74.6(6) . . ? C4 C5 C1 103.4(10) . . ? C4 C5 Si1 125.2(9) . . ? C1 C5 Si1 130.5(9) . . ? C4 C5 Ti1 71.5(6) . . ? C1 C5 Ti1 70.7(5) . . ? Si1 C5 Ti1 130.0(5) . . ? C10 C9 C13 111.6(10) . . ? C10 C9 Ti1 72.6(6) . . ? C13 C9 Ti1 74.6(6) . . ? C9 C10 C11 107.2(10) . . ? C9 C10 Ti1 73.2(6) . . ? C11 C10 Ti1 72.9(6) . . ? C10 C11 C12 107.8(10) . . ? C10 C11 Ti1 72.6(6) . . ? C12 C11 Ti1 72.2(6) . . ? C11 C12 C13 109.7(9) . . ? C11 C12 Ti1 73.1(6) . . ? C13 C12 Ti1 74.8(6) . . ? C9 C13 C12 103.8(10) . . ? C9 C13 Si2 125.5(9) . . ? C12 C13 Si2 129.6(8) . . ? C9 C13 Ti1 71.1(6) . . ? C12 C13 Ti1 70.2(6) . . ? Si2 C13 Ti1 131.3(6) . . ? C18 C17 S1 177.5(12) . . ? C17 C18 C19 173.3(13) . . ? C18 C19 C21 110.2(10) . . ? C18 C19 C20 108.8(9) . . ? C21 C19 C20 109.3(11) . . ? C18 C19 C22 109.3(10) . . ? C21 C19 C22 110.7(10) . . ? C20 C19 C22 108.5(10) . . ? C24 C23 S2 174.0(13) . . ? C23 C24 C25 169.1(15) . . ? C24 C25 C27 111.2(12) . . ? C24 C25 C26 112.4(10) . . ? C27 C25 C26 107.9(13) . . ? C24 C25 C28 112.1(12) . . ? C27 C25 C28 108.4(13) . . ? C26 C25 C28 104.5(12) . . ? C31 Ti2 C39 146.0(4) . . ? C31 Ti2 C40 144.0(5) . . ? C39 Ti2 C40 35.8(3) . . ? C31 Ti2 C32 34.1(3) . . ? C39 Ti2 C32 114.5(4) . . ? C40 Ti2 C32 133.9(4) . . ? C31 Ti2 C38 111.9(4) . . ? C39 Ti2 C38 34.1(3) . . ? C40 Ti2 C38 58.4(4) . . ? C32 Ti2 C38 81.5(4) . . ? C31 Ti2 C37 94.6(4) . . ? C39 Ti2 C37 56.5(4) . . ? C40 Ti2 C37 57.1(4) . . ? C32 Ti2 C37 77.2(4) . . ? C38 Ti2 C37 34.4(4) . . ? C31 Ti2 C30 34.4(4) . . ? C39 Ti2 C30 161.1(4) . . ? C40 Ti2 C30 162.4(4) . . ? C32 Ti2 C30 57.2(4) . . ? C38 Ti2 C30 137.5(4) . . ? C37 Ti2 C30 128.9(4) . . ? C31 Ti2 C29 56.4(4) . . ? C39 Ti2 C29 127.0(4) . . ? C40 Ti2 C29 158.9(4) . . ? C32 Ti2 C29 56.5(4) . . ? C38 Ti2 C29 115.3(4) . . ? C37 Ti2 C29 130.9(4) . . ? C30 Ti2 C29 34.2(3) . . ? C31 Ti2 C33 58.3(4) . . ? C39 Ti2 C33 104.6(4) . . ? C40 Ti2 C33 139.4(4) . . ? C32 Ti2 C33 35.7(4) . . ? C38 Ti2 C33 82.8(4) . . ? C37 Ti2 C33 98.0(4) . . ? C30 Ti2 C33 58.2(4) . . ? C29 Ti2 C33 34.1(3) . . ? C31 Ti2 S4 125.3(3) . . ? C39 Ti2 S4 79.7(3) . . ? C40 Ti2 S4 89.6(3) . . ? C32 Ti2 S4 125.0(3) . . ? C38 Ti2 S4 105.8(3) . . ? C37 Ti2 S4 136.2(3) . . ? C30 Ti2 S4 91.8(3) . . ? C29 Ti2 S4 72.4(3) . . ? C33 Ti2 S4 90.2(3) . . ? C31 Ti2 S3 87.3(3) . . ? C39 Ti2 S3 114.9(3) . . ? C40 Ti2 S3 79.8(3) . . ? C32 Ti2 S3 119.7(3) . . ? C38 Ti2 S3 131.8(3) . . ? C37 Ti2 S3 103.9(3) . . ? C30 Ti2 S3 82.6(3) . . ? C29 Ti2 S3 112.1(3) . . ? C33 Ti2 S3 140.5(3) . . ? S4 Ti2 S3 95.94(13) . . ? C31 Ti2 C41 109.7(4) . . ? C39 Ti2 C41 57.4(4) . . ? C40 Ti2 C41 34.5(3) . . ? C32 Ti2 C41 106.1(4) . . ? C38 Ti2 C41 57.4(4) . . ? C37 Ti2 C41 33.8(3) . . ? C30 Ti2 C41 139.0(4) . . ? C29 Ti2 C41 162.6(4) . . ? C33 Ti2 C41 131.8(4) . . ? S4 Ti2 C41 123.8(3) . . ? S3 Ti2 C41 74.7(3) . . ? C45 S3 Ti2 115.5(4) . . ? C51 S4 Ti2 110.6(4) . . ? C34 Si3 C35 107.7(6) . . ? C34 Si3 C36 109.9(6) . . ? C35 Si3 C36 111.4(6) . . ? C34 Si3 C33 114.5(5) . . ? C35 Si3 C33 107.2(5) . . ? C36 Si3 C33 106.2(6) . . ? C44 Si4 C41 111.0(5) . . ? C44 Si4 C42 109.6(6) . . ? C41 Si4 C42 102.7(5) . . ? C44 Si4 C43 111.7(6) . . ? C41 Si4 C43 112.8(6) . . ? C42 Si4 C43 108.6(5) . . ? C30 C29 C33 111.9(11) . . ? C30 C29 Ti2 72.4(6) . . ? C33 C29 Ti2 73.5(6) . . ? C31 C30 C29 105.4(10) . . ? C31 C30 Ti2 70.0(6) . . ? C29 C30 Ti2 73.4(6) . . ? C32 C31 C30 110.3(12) . . ? C32 C31 Ti2 73.8(7) . . ? C30 C31 Ti2 75.5(7) . . ? C31 C32 C33 109.5(11) . . ? C31 C32 Ti2 72.1(6) . . ? C33 C32 Ti2 75.1(6) . . ? C29 C33 C32 102.8(11) . . ? C29 C33 Si3 124.2(10) . . ? C32 C33 Si3 131.9(9) . . ? C29 C33 Ti2 72.4(6) . . ? C32 C33 Ti2 69.3(6) . . ? Si3 C33 Ti2 130.7(5) . . ? C38 C37 C41 110.9(11) . . ? C38 C37 Ti2 71.7(7) . . ? C41 C37 Ti2 76.5(7) . . ? C39 C38 C37 107.2(10) . . ? C39 C38 Ti2 72.5(6) . . ? C37 C38 Ti2 73.8(6) . . ? C38 C39 C40 108.8(11) . . ? C38 C39 Ti2 73.4(6) . . ? C40 C39 Ti2 72.0(6) . . ? C41 C40 C39 107.5(10) . . ? C41 C40 Ti2 77.6(7) . . ? C39 C40 Ti2 72.2(6) . . ? C37 C41 C40 105.2(11) . . ? C37 C41 Si4 123.6(10) . . ? C40 C41 Si4 130.6(8) . . ? C37 C41 Ti2 69.8(7) . . ? C40 C41 Ti2 67.9(7) . . ? Si4 C41 Ti2 133.5(5) . . ? C46 C45 S3 176.6(11) . . ? C45 C46 C47 174.1(13) . . ? C50 C47 C49 110.1(12) . . ? C50 C47 C46 110.1(11) . . ? C49 C47 C46 108.3(10) . . ? C50 C47 C48 108.5(11) . . ? C49 C47 C48 111.8(12) . . ? C46 C47 C48 108.0(11) . . ? C52 C51 S4 177.8(11) . . ? C51 C52 C53 174.8(14) . . ? C52 C53 C54 111.8(11) . . ? C52 C53 C56 108.8(12) . . ? C54 C53 C56 109.3(13) . . ? C52 C53 C55 109.9(11) . . ? C54 C53 C55 108.0(13) . . ? C56 C53 C55 108.9(12) . . ? _refine_diff_density_max 0.655 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.082 #=END data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C57.50 H60 F10 P Pt S2 Si Ti' _chemical_formula_weight 1307.22 _chemical_melting_point ? _chemical_compound_source ? 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.904(2) _cell_length_b 14.0690(10) _cell_length_c 18.090(2) _cell_angle_alpha 70.180(10) _cell_angle_beta 71.420(10) _cell_angle_gamma 74.910(10) _cell_volume 2885.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method ? _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 2.749 _exptl_absorpt_correction_type ? _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 MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10495 _diffrn_reflns_av_R_equivalents 0.0788 _diffrn_reflns_av_sigmaI/netI 0.1286 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9885 _reflns_number_observed 6683 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1003 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+0.0714P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8882 _refine_ls_number_parameters 685 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1217 _refine_ls_R_factor_obs 0.0672 _refine_ls_wR_factor_all 0.2064 _refine_ls_wR_factor_obs 0.1538 _refine_ls_goodness_of_fit_all 1.049 _refine_ls_goodness_of_fit_obs 1.124 _refine_ls_restrained_S_all 1.230 _refine_ls_restrained_S_obs 1.124 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.21026(4) 0.06035(4) 0.21984(3) 0.02347(15) Uani 1 d . . Ti1 Ti 0.3685(2) 0.2309(2) 0.25260(12) 0.0257(5) Uani 1 d . . S1 S 0.1812(2) 0.1759(2) 0.2963(2) 0.0264(7) Uani 1 d . . S2 S 0.2943(3) 0.3466(2) 0.3332(2) 0.0339(7) Uani 1 d . . P1 P 0.3288(3) -0.0372(2) 0.2979(2) 0.0255(7) Uani 1 d . . Si1 Si 0.5046(3) 0.4738(3) 0.1695(2) 0.0440(10) Uani 1 d . . F2 F -0.0511(7) 0.0972(8) 0.2699(7) 0.078(3) Uani 1 d . . F3 F -0.2051(8) 0.2104(10) 0.1879(10) 0.139(6) Uani 1 d . . F4 F -0.1451(12) 0.3235(10) 0.0318(10) 0.163(7) Uani 1 d . . F5 F 0.0725(13) 0.3175(9) -0.0448(7) 0.129(5) Uani 1 d . . F6 F 0.2261(8) 0.2094(7) 0.0330(5) 0.063(2) Uani 1 d . . F8 F 0.0941(7) -0.1296(6) 0.2563(5) 0.057(2) Uani 1 d . . F9 F 0.1223(8) -0.2617(7) 0.1720(6) 0.080(3) Uani 1 d . . F10 F 0.2755(8) -0.2496(7) 0.0264(6) 0.073(3) Uani 1 d . . F11 F 0.4003(7) -0.0980(7) -0.0333(5) 0.064(2) Uani 1 d . . F12 F 0.3768(6) 0.0330(6) 0.0492(4) 0.046(2) Uani 1 d . . C1 C 0.0946(10) 0.1457(9) 0.1576(7) 0.031(3) Uani 1 d . . C2 C -0.0152(12) 0.1474(12) 0.1931(12) 0.059(5) Uani 1 d . . C3 C -0.0978(13) 0.2080(16) 0.1469(16) 0.079(6) Uani 1 d . . C4 C -0.0652(20) 0.2662(17) 0.0682(17) 0.090(8) Uani 1 d . . C5 C 0.0394(21) 0.2628(13) 0.0335(13) 0.081(7) Uani 1 d . . C6 C 0.1207(12) 0.2059(11) 0.0750(9) 0.044(4) Uani 1 d . . C7 C 0.2357(10) -0.0425(9) 0.1576(8) 0.035(3) Uani 1 d . . C8 C 0.1730(10) -0.1192(10) 0.1851(8) 0.036(3) Uani 1 d . . C9 C 0.1860(12) -0.1903(10) 0.1428(9) 0.045(4) Uani 1 d . . C10 C 0.2621(12) -0.1833(11) 0.0700(9) 0.046(4) Uani 1 d . . C11 C 0.3257(11) -0.1053(11) 0.0381(8) 0.044(4) Uani 1 d . . C12 C 0.3100(10) -0.0396(9) 0.0828(7) 0.032(3) Uani 1 d . . C13 C 0.2585(10) -0.0893(9) 0.4016(7) 0.029(3) Uani 1 d . . C14 C 0.1460(10) -0.0909(10) 0.4219(8) 0.038(3) Uani 1 d . . H14A H 0.1085(10) -0.0647(10) 0.3792(8) 0.046 Uiso 1 d R . C15 C 0.0853(12) -0.1289(11) 0.5018(8) 0.049(4) Uani 1 d . . H15A H 0.0076(12) -0.1298(11) 0.5135(8) 0.059 Uiso 1 d R . C16 C 0.1395(12) -0.1659(11) 0.5640(8) 0.052(4) Uani 1 d . . H16A H 0.0997(12) -0.1927(11) 0.6192(8) 0.062 Uiso 1 d R . C17 C 0.2525(12) -0.1634(11) 0.5450(7) 0.048(4) Uani 1 d . . H17A H 0.2897(12) -0.1879(11) 0.5879(7) 0.057 Uiso 1 d R . C18 C 0.3112(12) -0.1266(10) 0.4665(7) 0.040(3) Uani 1 d . . H18A H 0.3889(12) -0.1253(10) 0.4549(7) 0.048 Uiso 1 d R . C19 C 0.4348(10) -0.1388(9) 0.2663(7) 0.032(3) Uani 1 d . . C20 C 0.4554(11) -0.2351(9) 0.3195(8) 0.044(4) Uani 1 d . . H20A H 0.4109(11) -0.2502(9) 0.3746(8) 0.053 Uiso 1 d R . C21 C 0.5412(12) -0.3107(10) 0.2920(8) 0.045(4) Uani 1 d . . H21A H 0.5541(12) -0.3782(10) 0.3281(8) 0.054 Uiso 1 d R . C22 C 0.6073(12) -0.2881(10) 0.2139(9) 0.048(4) Uani 1 d . . H22A H 0.6681(12) -0.3383(10) 0.1963(9) 0.058 Uiso 1 d R . C23 C 0.5848(11) -0.1903(10) 0.1605(8) 0.043(3) Uani 1 d . . H23A H 0.6284(11) -0.1749(10) 0.1052(8) 0.052 Uiso 1 d R . C24 C 0.4997(9) -0.1168(9) 0.1870(7) 0.031(3) Uani 1 d . . H24A H 0.4853(9) -0.0499(9) 0.1505(7) 0.038 Uiso 1 d R . C25 C 0.4104(10) 0.0463(8) 0.3044(7) 0.028(3) Uani 1 d . . C26 C 0.5031(9) 0.0815(9) 0.2462(7) 0.032(3) Uani 1 d . . H26A H 0.5396(9) 0.0596(9) 0.1981(7) 0.038 Uiso 1 d R . C27 C 0.5419(10) 0.1459(9) 0.2735(8) 0.034(3) Uani 1 d . . H27A H 0.6100(10) 0.1727(9) 0.2488(8) 0.041 Uiso 1 d R . C28 C 0.4708(10) 0.1497(8) 0.3497(7) 0.030(3) Uani 1 d . . H28A H 0.4814(10) 0.1822(8) 0.3850(7) 0.036 Uiso 1 d R . C29 C 0.3865(10) 0.0908(8) 0.3701(7) 0.029(3) Uani 1 d . . H29A H 0.3310(10) 0.0760(8) 0.4205(7) 0.035 Uiso 1 d R . C30 C 0.4354(10) 0.3809(8) 0.1556(7) 0.030(3) Uani 1 d . . C31 C 0.3225(10) 0.3910(8) 0.1598(7) 0.030(3) Uani 1 d . . H31A H 0.2661(10) 0.4462(8) 0.1743(7) 0.036 Uiso 1 d R . C32 C 0.3057(10) 0.3152(9) 0.1319(6) 0.031(3) Uani 1 d . . H32A H 0.2376(10) 0.3102(9) 0.1236(6) 0.037 Uiso 1 d R . C33 C 0.4089(10) 0.2530(10) 0.1124(7) 0.038(3) Uani 1 d . . H33A H 0.4240(10) 0.1989(10) 0.0873(7) 0.046 Uiso 1 d R . C34 C 0.4891(11) 0.2945(10) 0.1239(7) 0.037(3) Uani 1 d . . H34A H 0.5678(11) 0.2721(10) 0.1089(7) 0.045 Uiso 1 d R . C35 C 0.5808(12) 0.4138(10) 0.2492(9) 0.048(4) Uani 1 d . . H35A H 0.6147(12) 0.4640(10) 0.2539(9) 0.073 Uiso 1 d R . H35B H 0.5304(12) 0.3876(10) 0.3002(9) 0.073 Uiso 1 d R . H35C H 0.6372(12) 0.3586(10) 0.2349(9) 0.073 Uiso 1 d R . C36 C 0.6054(14) 0.5191(14) 0.0735(9) 0.073(5) Uani 1 d . . H36A H 0.6424(14) 0.5668(14) 0.0785(9) 0.109 Uiso 1 d R . H36B H 0.6590(14) 0.4617(14) 0.0604(9) 0.109 Uiso 1 d R . H36C H 0.5675(14) 0.5523(14) 0.0312(9) 0.109 Uiso 1 d R . C37 C 0.3991(16) 0.5814(12) 0.1939(13) 0.088(7) Uani 1 d . . H37A H 0.4329(16) 0.6298(12) 0.2012(13) 0.131 Uiso 1 d R . H37B H 0.3633(16) 0.6144(12) 0.1504(13) 0.131 Uiso 1 d R . H37C H 0.3451(16) 0.5563(12) 0.2431(13) 0.131 Uiso 1 d R . C38 C 0.0887(10) 0.2833(9) 0.2683(7) 0.030(3) Uani 1 d . . C39 C 0.0229(10) 0.3592(9) 0.2541(7) 0.031(3) Uani 1 d . . C40 C -0.0557(10) 0.4547(9) 0.2345(8) 0.037(3) Uani 1 d . . C41 C -0.1527(12) 0.4624(12) 0.3084(9) 0.063(5) Uani 1 d . . H41A H -0.1252(12) 0.4609(12) 0.3523(9) 0.094 Uiso 1 d R . H41B H -0.2034(12) 0.5252(12) 0.2952(9) 0.094 Uiso 1 d R . H41C H -0.1903(12) 0.4053(12) 0.3242(9) 0.094 Uiso 1 d R . C42 C -0.1011(13) 0.4578(11) 0.1638(9) 0.054(4) Uani 1 d . . H42A H -0.1367(13) 0.3994(11) 0.1794(9) 0.080 Uiso 1 d R . H42B H -0.1539(13) 0.5195(11) 0.1523(9) 0.080 Uiso 1 d R . H42C H -0.0411(13) 0.4560(11) 0.1162(9) 0.080 Uiso 1 d R . C43 C 0.0007(13) 0.5475(9) 0.2112(9) 0.054(4) Uani 1 d . . H43A H 0.0287(13) 0.5450(9) 0.2552(9) 0.081 Uiso 1 d R . H43B H 0.0611(13) 0.5460(9) 0.1637(9) 0.081 Uiso 1 d R . H43C H -0.0517(13) 0.6095(9) 0.1998(9) 0.081 Uiso 1 d R . C44 C 0.2733(10) 0.2843(9) 0.4318(7) 0.033(3) Uani 1 d . . C45 C 0.2576(10) 0.2405(9) 0.5030(7) 0.033(3) Uani 1 d . . C46 C 0.2420(11) 0.1854(10) 0.5900(7) 0.043(3) Uani 1 d . . C47 C 0.3567(14) 0.1307(15) 0.6069(10) 0.086(7) Uani 1 d . . H47A H 0.4034(14) 0.1806(15) 0.5925(10) 0.130 Uiso 1 d R . H47B H 0.3477(14) 0.0939(15) 0.6633(10) 0.130 Uiso 1 d R . H47C H 0.3903(14) 0.0835(15) 0.5745(10) 0.130 Uiso 1 d R . C48 C 0.1889(16) 0.2638(14) 0.6398(10) 0.080(6) Uani 1 d . . H48A H 0.2381(16) 0.3117(14) 0.6252(10) 0.120 Uiso 1 d R . H48B H 0.1191(16) 0.3000(14) 0.6283(10) 0.120 Uiso 1 d R . H48C H 0.1773(16) 0.2287(14) 0.6967(10) 0.120 Uiso 1 d R . C49 C 0.1637(17) 0.1062(14) 0.6127(11) 0.088(6) Uani 1 d . . H49A H 0.0932(17) 0.1420(14) 0.6024(11) 0.132 Uiso 1 d R . H49B H 0.1961(17) 0.0589(14) 0.5804(11) 0.132 Uiso 1 d R . H49C H 0.1535(17) 0.0693(14) 0.6692(11) 0.132 Uiso 1 d R . C50 C -0.2088(19) -0.0239(22) 0.1520(13) 0.038(7) Uani 0.50 d P . C51 C -0.0387(18) 0.0129(17) 0.0332(14) 0.027(4) Uani 0.50 d P . C52 C 0.1183(19) 0.0541(16) -0.0853(14) 0.027(4) Uani 0.50 d P . C53 C 0.5580(30) -0.5008(27) 0.5129(16) 0.056(9) Uani 0.50 d P . C54 C 0.4519(17) -0.4239(11) 0.5214(9) 0.059(4) Uani 1 d . . C55 C 0.3647(34) -0.4445(35) 0.5069(20) 0.073(11) Uani 0.50 d P . C56 C 0.3503(20) -0.5119(19) 0.4757(14) 0.102(7) Uani 1 d . . C57 C 0.4562(32) -0.5857(27) 0.4643(19) 0.065(10) Uani 0.50 d P . C58 C -0.0958(51) 0.4290(51) 0.6010(36) 0.123(21) Uani 0.50 d P . C59 C -0.0720(27) 0.3632(21) 0.5480(25) 0.149(13) Uani 1 d . . C60 C -0.0071(47) 0.3998(45) 0.4797(40) 0.102(7) Uani 0.50 d P . C61 C 0.0452(19) 0.4808(32) 0.4354(15) 0.116(10) Uani 1 d . . C62 C 0.0161(46) 0.5407(41) 0.4885(41) 0.102(7) Uani 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 Pt1 0.0244(2) 0.0234(2) 0.0218(2) -0.0059(2) -0.0060(2) -0.0031(2) Ti1 0.0255(11) 0.0262(11) 0.0247(11) -0.0044(9) -0.0090(9) -0.0034(9) S1 0.027(2) 0.024(2) 0.026(2) -0.0049(12) -0.0072(12) -0.0012(12) S2 0.042(2) 0.031(2) 0.030(2) -0.0094(13) -0.0137(14) -0.0023(14) P1 0.029(2) 0.022(2) 0.020(2) -0.0029(12) -0.0060(13) -0.0011(13) Si1 0.050(2) 0.035(2) 0.051(2) -0.001(2) -0.024(2) -0.015(2) F2 0.047(5) 0.092(8) 0.100(8) -0.057(7) 0.020(5) -0.029(5) F3 0.032(6) 0.150(12) 0.290(19) -0.140(13) -0.050(8) 0.009(6) F4 0.181(13) 0.123(11) 0.277(18) -0.091(12) -0.217(14) 0.066(10) F5 0.236(16) 0.083(8) 0.091(9) 0.009(7) -0.124(10) -0.006(9) F6 0.083(7) 0.064(6) 0.031(4) 0.000(4) -0.014(4) -0.010(5) F8 0.064(5) 0.054(5) 0.057(5) -0.025(4) 0.009(4) -0.035(4) F9 0.094(7) 0.058(6) 0.112(8) -0.041(6) -0.022(6) -0.034(6) F10 0.093(7) 0.067(6) 0.088(7) -0.059(6) -0.027(6) -0.006(5) F11 0.062(5) 0.090(7) 0.043(5) -0.042(5) -0.003(4) 0.000(5) F12 0.047(5) 0.047(5) 0.037(4) -0.011(4) -0.005(4) -0.008(4) C1 0.034(7) 0.027(7) 0.042(7) -0.014(6) -0.019(6) -0.003(5) C2 0.029(8) 0.048(10) 0.120(15) -0.055(10) -0.023(9) 0.009(7) C3 0.026(9) 0.088(15) 0.155(20) -0.084(15) -0.034(11) 0.018(9) C4 0.085(16) 0.083(15) 0.150(22) -0.060(15) -0.093(17) 0.019(13) C5 0.133(19) 0.053(11) 0.094(15) -0.026(10) -0.096(15) 0.016(12) C6 0.054(9) 0.043(8) 0.048(9) -0.015(7) -0.032(8) 0.001(7) C7 0.028(7) 0.029(7) 0.038(7) -0.008(6) -0.005(6) 0.004(6) C8 0.031(7) 0.034(7) 0.042(8) -0.019(6) -0.001(6) -0.002(6) C9 0.053(9) 0.036(8) 0.062(10) -0.019(7) -0.023(8) -0.014(7) C10 0.054(9) 0.047(9) 0.045(8) -0.024(7) -0.025(7) 0.007(7) C11 0.041(8) 0.060(10) 0.030(7) -0.023(7) -0.010(6) 0.011(7) C12 0.035(7) 0.027(7) 0.034(7) -0.012(6) -0.012(6) 0.005(6) C13 0.035(7) 0.030(7) 0.022(6) -0.007(5) -0.004(5) -0.009(6) C14 0.040(8) 0.036(8) 0.040(8) -0.007(6) -0.011(6) -0.013(6) C15 0.053(9) 0.050(9) 0.030(7) -0.001(6) 0.001(6) -0.014(7) C16 0.061(10) 0.044(9) 0.033(8) -0.003(6) 0.008(7) -0.014(7) C17 0.067(10) 0.052(9) 0.014(6) -0.001(6) -0.006(6) -0.009(8) C18 0.048(8) 0.038(8) 0.031(7) -0.007(6) -0.008(6) -0.008(6) C19 0.035(7) 0.037(7) 0.028(6) -0.016(6) -0.010(5) 0.002(6) C20 0.057(9) 0.028(7) 0.031(7) 0.001(6) -0.010(6) 0.005(6) C21 0.070(10) 0.022(7) 0.044(8) -0.008(6) -0.024(7) 0.003(7) C22 0.047(8) 0.038(8) 0.060(10) -0.023(7) -0.023(7) 0.018(7) C23 0.038(8) 0.049(9) 0.040(8) -0.009(7) -0.008(6) -0.008(7) C24 0.022(6) 0.031(7) 0.036(7) -0.010(5) -0.007(5) 0.004(5) C25 0.036(7) 0.022(6) 0.022(6) -0.004(5) -0.012(5) 0.003(5) C26 0.025(6) 0.033(7) 0.034(7) -0.009(6) -0.003(5) -0.006(5) C27 0.031(7) 0.022(6) 0.045(8) 0.003(5) -0.010(6) -0.010(5) C28 0.040(7) 0.019(6) 0.034(7) -0.002(5) -0.023(6) 0.000(5) C29 0.038(7) 0.019(6) 0.025(6) 0.007(5) -0.020(5) 0.001(5) C30 0.035(7) 0.018(6) 0.033(7) 0.001(5) -0.010(5) -0.006(5) C31 0.040(7) 0.015(6) 0.033(7) -0.003(5) -0.013(6) -0.001(5) C32 0.028(6) 0.041(7) 0.019(6) 0.003(5) -0.007(5) -0.011(6) C33 0.037(7) 0.053(9) 0.018(6) -0.010(6) 0.005(5) -0.012(6) C34 0.040(7) 0.037(8) 0.028(7) 0.001(6) -0.001(6) -0.018(6) C35 0.049(9) 0.038(8) 0.064(10) -0.012(7) -0.027(7) -0.003(7) C36 0.087(13) 0.084(13) 0.058(10) 0.008(9) -0.025(9) -0.060(11) C37 0.099(14) 0.037(9) 0.158(20) -0.033(11) -0.087(14) 0.011(9) C38 0.031(7) 0.029(7) 0.033(7) -0.010(5) -0.014(5) 0.000(6) C39 0.035(7) 0.032(7) 0.029(6) -0.009(5) -0.011(5) -0.007(6) C40 0.040(7) 0.030(7) 0.053(8) -0.012(6) -0.030(6) -0.004(6) C41 0.047(9) 0.057(10) 0.071(11) -0.021(8) -0.024(8) 0.030(8) C42 0.068(10) 0.042(9) 0.081(11) -0.033(8) -0.048(9) -0.002(7) C43 0.071(10) 0.021(7) 0.073(11) -0.008(7) -0.044(9) 0.011(7) C44 0.045(8) 0.036(7) 0.028(7) -0.018(6) -0.018(6) 0.000(6) C45 0.033(7) 0.030(7) 0.032(7) -0.012(6) -0.010(5) 0.008(5) C46 0.048(8) 0.046(8) 0.023(7) 0.002(6) -0.010(6) -0.002(7) C47 0.071(12) 0.101(15) 0.052(10) 0.012(10) -0.030(9) 0.018(11) C48 0.097(14) 0.092(14) 0.053(10) -0.041(10) -0.027(10) 0.016(11) C49 0.120(17) 0.074(13) 0.061(12) 0.000(10) -0.001(11) -0.054(13) C50 0.030(13) 0.071(19) 0.009(11) -0.010(12) -0.009(10) 0.000(13) C51 0.034(10) 0.018(8) 0.039(10) -0.010(7) -0.033(8) 0.012(7) C52 0.034(10) 0.018(8) 0.039(10) -0.010(7) -0.033(8) 0.012(7) C53 0.068(23) 0.052(21) 0.015(14) 0.020(13) -0.002(14) -0.005(19) C54 0.099(14) 0.031(8) 0.042(9) -0.010(7) -0.010(9) -0.012(9) C55 0.068(25) 0.097(32) 0.043(20) 0.004(20) -0.014(19) -0.027(26) C56 0.098(14) 0.102(17) 0.114(16) 0.003(13) -0.063(12) -0.030(13) C57 0.089(27) 0.057(22) 0.050(20) 0.017(17) -0.024(18) -0.049(21) C58 0.148(51) 0.134(49) 0.140(51) -0.080(44) -0.090(43) 0.010(40) C59 0.142(25) 0.112(22) 0.219(35) 0.011(24) -0.135(26) -0.029(19) C60 0.098(14) 0.102(17) 0.114(16) 0.003(13) -0.063(12) -0.030(13) C61 0.059(14) 0.190(31) 0.087(18) -0.042(21) -0.054(13) 0.047(17) C62 0.098(14) 0.102(17) 0.114(16) 0.003(13) -0.063(12) -0.030(13) _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 Pt1 C7 2.023(13) . ? Pt1 C1 2.039(12) . ? Pt1 P1 2.277(3) . ? Pt1 S1 2.360(3) . ? Ti1 C27 2.328(12) . ? Ti1 C28 2.337(11) . ? Ti1 C33 2.348(12) . ? Ti1 C26 2.363(12) . ? Ti1 S2 2.366(4) . ? Ti1 C31 2.370(11) . ? Ti1 C34 2.376(11) . ? Ti1 C29 2.386(10) . ? Ti1 C32 2.389(11) . ? Ti1 C30 2.397(11) . ? Ti1 C25 2.421(11) . ? Ti1 S1 2.532(4) . ? S1 C38 1.700(12) . ? S2 C44 1.668(12) . ? P1 C13 1.791(11) . ? P1 C19 1.811(12) . ? P1 C25 1.821(12) . ? Si1 C37 1.83(2) . ? Si1 C36 1.83(2) . ? Si1 C35 1.846(13) . ? Si1 C30 1.883(13) . ? F2 C2 1.32(2) . ? F3 C3 1.34(2) . ? F4 C4 1.34(2) . ? F5 C5 1.35(2) . ? F6 C6 1.33(2) . ? F8 C8 1.353(14) . ? F9 C9 1.33(2) . ? F10 C10 1.359(15) . ? F11 C11 1.331(14) . ? F12 C12 1.363(14) . ? C1 C2 1.35(2) . ? C1 C6 1.43(2) . ? C2 C3 1.47(2) . ? C3 C4 1.37(3) . ? C4 C5 1.29(3) . ? C5 C6 1.40(2) . ? C7 C8 1.38(2) . ? C7 C12 1.38(2) . ? C8 C9 1.40(2) . ? C9 C10 1.36(2) . ? C10 C11 1.40(2) . ? C11 C12 1.36(2) . ? C13 C14 1.38(2) . ? C13 C18 1.42(2) . ? C14 C15 1.40(2) . ? C15 C16 1.39(2) . ? C16 C17 1.39(2) . ? C17 C18 1.37(2) . ? C19 C20 1.39(2) . ? C19 C24 1.39(2) . ? C20 C21 1.41(2) . ? C21 C22 1.38(2) . ? C22 C23 1.41(2) . ? C23 C24 1.38(2) . ? C25 C26 1.39(2) . ? C25 C29 1.44(2) . ? C26 C27 1.42(2) . ? C27 C28 1.40(2) . ? C28 C29 1.42(2) . ? C30 C31 1.41(2) . ? C30 C34 1.44(2) . ? C31 C32 1.41(2) . ? C32 C33 1.40(2) . ? C33 C34 1.41(2) . ? C38 C39 1.19(2) . ? C39 C40 1.47(2) . ? C40 C41 1.52(2) . ? C40 C43 1.53(2) . ? C40 C42 1.55(2) . ? C44 C45 1.20(2) . ? C45 C46 1.47(2) . ? C46 C48 1.54(2) . ? C46 C47 1.55(2) . ? C46 C49 1.56(2) . ? C50 C52 1.48(3) 2 ? C51 C51 1.38(5) 2 ? C51 C52 1.46(3) 2 ? C52 C51 1.46(3) 2 ? C52 C50 1.48(3) 2 ? C53 C55 1.13(5) 2_646 ? C53 C56 1.33(4) 2_646 ? C53 C57 1.36(5) 2_646 ? C53 C54 1.45(4) 2_646 ? C53 C54 1.51(4) . ? C53 C53 1.70(7) 2_646 ? C54 C57 1.34(4) 2_646 ? C54 C55 1.35(4) . ? C54 C53 1.45(4) 2_646 ? C55 C53 1.13(5) 2_646 ? C55 C56 1.33(5) . ? C56 C53 1.33(4) 2_646 ? C56 C57 1.49(5) . ? C57 C54 1.34(4) 2_646 ? C57 C53 1.36(5) 2_646 ? C58 C61 1.44(7) 2_566 ? C58 C59 1.46(5) . ? C58 C62 1.60(9) 2_566 ? C59 C60 1.28(6) . ? C59 C62 1.54(5) 2_566 ? C60 C62 1.13(8) 2_566 ? C60 C61 1.35(6) . ? C61 C62 1.33(7) 2_566 ? C61 C62 1.39(7) . ? C61 C58 1.44(7) 2_566 ? C62 C60 1.13(8) 2_566 ? C62 C62 1.21(10) 2_566 ? C62 C61 1.33(7) 2_566 ? C62 C59 1.55(5) 2_566 ? C62 C58 1.60(10) 2_566 ? 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 C7 Pt1 C1 87.0(5) . . ? C7 Pt1 P1 94.6(4) . . ? C1 Pt1 P1 175.7(4) . . ? C7 Pt1 S1 178.1(4) . . ? C1 Pt1 S1 94.5(3) . . ? P1 Pt1 S1 83.92(11) . . ? C27 Ti1 C28 34.9(4) . . ? C27 Ti1 C33 98.7(4) . . ? C28 Ti1 C33 133.5(4) . . ? C27 Ti1 C26 35.2(4) . . ? C28 Ti1 C26 57.5(4) . . ? C33 Ti1 C26 82.0(4) . . ? C27 Ti1 S2 108.5(3) . . ? C28 Ti1 S2 82.1(3) . . ? C33 Ti1 S2 132.9(4) . . ? C26 Ti1 S2 139.5(3) . . ? C27 Ti1 C31 128.8(4) . . ? C28 Ti1 C31 142.6(4) . . ? C33 Ti1 C31 57.5(4) . . ? C26 Ti1 C31 136.0(4) . . ? S2 Ti1 C31 75.6(3) . . ? C27 Ti1 C34 78.0(4) . . ? C28 Ti1 C34 109.9(4) . . ? C33 Ti1 C34 34.8(4) . . ? C26 Ti1 C34 80.6(4) . . ? S2 Ti1 C34 115.3(3) . . ? C31 Ti1 C34 56.7(4) . . ? C27 Ti1 C29 58.7(4) . . ? C28 Ti1 C29 34.9(4) . . ? C33 Ti1 C29 136.2(5) . . ? C26 Ti1 C29 57.7(4) . . ? S2 Ti1 C29 90.9(3) . . ? C31 Ti1 C29 166.0(4) . . ? C34 Ti1 C29 135.1(4) . . ? C27 Ti1 C32 132.2(4) . . ? C28 Ti1 C32 166.7(4) . . ? C33 Ti1 C32 34.5(4) . . ? C26 Ti1 C32 114.5(4) . . ? S2 Ti1 C32 104.8(3) . . ? C31 Ti1 C32 34.5(4) . . ? C34 Ti1 C32 56.9(4) . . ? C29 Ti1 C32 152.9(4) . . ? C27 Ti1 C30 94.7(4) . . ? C28 Ti1 C30 113.2(4) . . ? C33 Ti1 C30 58.7(4) . . ? C26 Ti1 C30 111.6(4) . . ? S2 Ti1 C30 80.9(3) . . ? C31 Ti1 C30 34.3(4) . . ? C34 Ti1 C30 35.0(4) . . ? C29 Ti1 C30 148.1(4) . . ? C32 Ti1 C30 57.9(4) . . ? C27 Ti1 C25 57.7(4) . . ? C28 Ti1 C25 57.3(4) . . ? C33 Ti1 C25 101.7(4) . . ? C26 Ti1 C25 33.8(4) . . ? S2 Ti1 C25 125.2(3) . . ? C31 Ti1 C25 157.4(4) . . ? C34 Ti1 C25 112.4(4) . . ? C29 Ti1 C25 34.8(4) . . ? C32 Ti1 C25 123.2(4) . . ? C30 Ti1 C25 145.4(4) . . ? C27 Ti1 S1 133.1(3) . . ? C28 Ti1 S1 112.4(3) . . ? C33 Ti1 S1 99.4(3) . . ? C26 Ti1 S1 106.5(3) . . ? S2 Ti1 S1 89.39(12) . . ? C31 Ti1 S1 97.1(3) . . ? C34 Ti1 S1 133.4(3) . . ? C29 Ti1 S1 78.8(3) . . ? C32 Ti1 S1 79.5(3) . . ? C30 Ti1 S1 131.4(3) . . ? C25 Ti1 S1 76.4(3) . . ? C38 S1 Pt1 112.2(4) . . ? C38 S1 Ti1 106.6(4) . . ? Pt1 S1 Ti1 102.51(12) . . ? C44 S2 Ti1 111.1(4) . . ? C13 P1 C19 107.4(6) . . ? C13 P1 C25 103.5(5) . . ? C19 P1 C25 102.3(5) . . ? C13 P1 Pt1 112.8(4) . . ? C19 P1 Pt1 120.7(4) . . ? C25 P1 Pt1 108.2(4) . . ? C37 Si1 C36 110.1(9) . . ? C37 Si1 C35 110.2(8) . . ? C36 Si1 C35 107.7(7) . . ? C37 Si1 C30 108.7(7) . . ? C36 Si1 C30 107.6(7) . . ? C35 Si1 C30 112.5(6) . . ? C2 C1 C6 114.8(13) . . ? C2 C1 Pt1 121.1(11) . . ? C6 C1 Pt1 124.1(9) . . ? F2 C2 C1 121.2(14) . . ? F2 C2 C3 118.3(15) . . ? C1 C2 C3 120.5(18) . . ? F3 C3 C4 122.3(20) . . ? F3 C3 C2 116.7(21) . . ? C4 C3 C2 120.7(16) . . ? C5 C4 F4 123.8(26) . . ? C5 C4 C3 119.0(18) . . ? F4 C4 C3 117.3(24) . . ? C4 C5 F5 119.6(18) . . ? C4 C5 C6 122.1(20) . . ? F5 C5 C6 118.4(21) . . ? F6 C6 C5 116.6(15) . . ? F6 C6 C1 120.5(11) . . ? C5 C6 C1 122.8(16) . . ? C8 C7 C12 113.8(12) . . ? C8 C7 Pt1 121.5(9) . . ? C12 C7 Pt1 124.5(10) . . ? F8 C8 C7 120.6(11) . . ? F8 C8 C9 116.0(11) . . ? C7 C8 C9 123.3(12) . . ? F9 C9 C10 120.1(13) . . ? F9 C9 C8 120.5(13) . . ? C10 C9 C8 119.3(13) . . ? F10 C10 C9 121.1(14) . . ? F10 C10 C11 119.2(13) . . ? C9 C10 C11 119.7(13) . . ? F11 C11 C12 122.1(14) . . ? F11 C11 C10 120.0(13) . . ? C12 C11 C10 117.9(12) . . ? C11 C12 F12 114.9(11) . . ? C11 C12 C7 125.8(13) . . ? F12 C12 C7 119.3(11) . . ? C14 C13 C18 116.8(11) . . ? C14 C13 P1 119.6(9) . . ? C18 C13 P1 123.5(9) . . ? C13 C14 C15 122.8(12) . . ? C16 C15 C14 119.1(13) . . ? C15 C16 C17 119.1(12) . . ? C18 C17 C16 121.3(13) . . ? C17 C18 C13 120.9(13) . . ? C20 C19 C24 119.8(11) . . ? C20 C19 P1 122.1(9) . . ? C24 C19 P1 118.0(9) . . ? C19 C20 C21 119.7(12) . . ? C22 C21 C20 120.4(12) . . ? C21 C22 C23 119.2(12) . . ? C24 C23 C22 120.4(12) . . ? C23 C24 C19 120.5(11) . . ? C26 C25 C29 108.0(11) . . ? C26 C25 P1 126.7(9) . . ? C29 C25 P1 125.2(9) . . ? C26 C25 Ti1 70.8(7) . . ? C29 C25 Ti1 71.3(6) . . ? P1 C25 Ti1 121.7(5) . . ? C25 C26 C27 109.4(11) . . ? C25 C26 Ti1 75.4(7) . . ? C27 C26 Ti1 71.0(7) . . ? C28 C27 C26 106.6(10) . . ? C28 C27 Ti1 72.9(7) . . ? C26 C27 Ti1 73.8(7) . . ? C27 C28 C29 110.0(11) . . ? C27 C28 Ti1 72.2(7) . . ? C29 C28 Ti1 74.4(6) . . ? C28 C29 C25 105.9(11) . . ? C28 C29 Ti1 70.7(6) . . ? C25 C29 Ti1 73.9(6) . . ? C31 C30 C34 104.8(11) . . ? C31 C30 Si1 127.4(9) . . ? C34 C30 Si1 126.9(9) . . ? C31 C30 Ti1 71.8(6) . . ? C34 C30 Ti1 71.7(6) . . ? Si1 C30 Ti1 129.1(6) . . ? C30 C31 C32 110.6(11) . . ? C30 C31 Ti1 73.9(6) . . ? C32 C31 Ti1 73.5(6) . . ? C33 C32 C31 107.3(11) . . ? C33 C32 Ti1 71.2(7) . . ? C31 C32 Ti1 72.0(6) . . ? C32 C33 C34 107.6(12) . . ? C32 C33 Ti1 74.4(7) . . ? C34 C33 Ti1 73.7(7) . . ? C33 C34 C30 109.5(11) . . ? C33 C34 Ti1 71.5(6) . . ? C30 C34 Ti1 73.3(7) . . ? C39 C38 S1 175.3(11) . . ? C38 C39 C40 178.2(13) . . ? C39 C40 C41 110.4(11) . . ? C39 C40 C43 110.3(10) . . ? C41 C40 C43 107.0(12) . . ? C39 C40 C42 110.1(11) . . ? C41 C40 C42 109.0(11) . . ? C43 C40 C42 110.0(11) . . ? C45 C44 S2 179.3(11) . . ? C44 C45 C46 178.2(13) . . ? C45 C46 C48 108.7(11) . . ? C45 C46 C47 109.2(11) . . ? C48 C46 C47 109.2(13) . . ? C45 C46 C49 108.8(12) . . ? C48 C46 C49 110.0(13) . . ? C47 C46 C49 111.0(14) . . ? C51 C51 C52 119.8(26) 2 2 ? C51 C52 C50 121.1(21) 2 2 ? C55 C53 C56 65.0(32) 2_646 2_646 ? C55 C53 C57 131.3(46) 2_646 2_646 ? C56 C53 C57 67.1(28) 2_646 2_646 ? C55 C53 C54 62.0(31) 2_646 2_646 ? C56 C53 C54 127.0(35) 2_646 2_646 ? C57 C53 C54 164.1(33) 2_646 2_646 ? C55 C53 C54 167.7(35) 2_646 . ? C56 C53 C54 122.3(35) 2_646 . ? C57 C53 C54 55.3(22) 2_646 . ? C54 C53 C54 110.0(25) 2_646 . ? C55 C53 C53 118.0(49) 2_646 2_646 ? C56 C53 C53 171.0(32) 2_646 2_646 ? C57 C53 C53 108.2(37) 2_646 2_646 ? C54 C53 C53 56.7(24) 2_646 2_646 ? C54 C53 C53 53.2(20) . 2_646 ? C57 C54 C55 173.5(29) 2_646 . ? C57 C54 C53 126.5(27) 2_646 2_646 ? C55 C54 C53 47.4(21) . 2_646 ? C57 C54 C53 56.9(22) 2_646 . ? C55 C54 C53 116.8(29) . . ? C53 C54 C53 70.0(25) 2_646 . ? C53 C55 C56 64.8(35) 2_646 . ? C53 C55 C54 70.6(32) 2_646 . ? C56 C55 C54 135.4(41) . . ? C53 C56 C55 50.2(22) 2_646 . ? C53 C56 C57 57.6(22) 2_646 . ? C55 C56 C57 107.4(27) . . ? C54 C57 C53 67.9(24) 2_646 2_646 ? C54 C57 C56 123.1(31) 2_646 . ? C53 C57 C56 55.3(23) 2_646 . ? C61 C58 C59 114.5(52) 2_566 . ? C61 C58 C62 54.1(37) 2_566 2_566 ? C59 C58 C62 60.4(34) . 2_566 ? C60 C59 C58 110.3(44) . . ? C60 C59 C62 46.1(36) . 2_566 ? C58 C59 C62 64.3(42) . 2_566 ? C62 C60 C59 79.6(54) 2_566 . ? C62 C60 C61 63.8(45) 2_566 . ? C59 C60 C61 143.3(61) . . ? C62 C61 C60 49.9(32) 2_566 . ? C62 C61 C62 52.9(41) 2_566 . ? C60 C61 C62 102.9(44) . . ? C62 C61 C58 121.8(51) 2_566 2_566 ? C60 C61 C58 171.8(47) . 2_566 ? C62 C61 C58 69.0(39) . 2_566 ? C60 C62 C62 132.3(100) 2_566 2_566 ? C60 C62 C61 66.2(56) 2_566 2_566 ? C62 C62 C61 66.1(56) 2_566 2_566 ? C60 C62 C61 166.5(66) 2_566 . ? C62 C62 C61 60.9(62) 2_566 . ? C61 C62 C61 127.1(41) 2_566 . ? C60 C62 C59 54.3(41) 2_566 2_566 ? C62 C62 C59 171.9(99) 2_566 2_566 ? C61 C62 C59 120.5(64) 2_566 2_566 ? C61 C62 C59 112.3(54) . 2_566 ? C60 C62 C58 109.7(54) 2_566 2_566 ? C62 C62 C58 117.8(97) 2_566 2_566 ? C61 C62 C58 175.2(54) 2_566 2_566 ? C61 C62 C58 56.9(41) . 2_566 ? C59 C62 C58 55.4(29) 2_566 2_566 ? _refine_diff_density_max 2.599 _refine_diff_density_min -1.748 _refine_diff_density_rms 0.186