# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Masanobu Hidai' _publ_contact_author_address ; Department of Materials Science & Technology Tokyo University of Science Fac. Industrial Sci & Technol. Noda Chiba 278-8510 JAPAN ; _publ_contact_author_email HIDAI@RS.NODA.TUS.AC.JP _publ_section_title ; Ti-Mo heterobimetallic thiacalix[4]arene complex containing an unusual a-agostic m2-h5:h5-cyclopentadienyl ligand ; loop_ _publ_author_name 'Masanobu Hidai' 'Yasushi Mizobe' 'Shin Takemoto' 'Shinpei Tanaka' data_[TC4A-(OH)(O)3TiCp](3) _database_code_depnum_ccdc_archive 'CCDC 228239' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H100 O8 S8 Ti2' _chemical_formula_weight 1662.07 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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.483(3) _cell_length_b 16.930(8) _cell_length_c 20.649(6) _cell_angle_alpha 109.90(3) _cell_angle_beta 95.721(19) _cell_angle_gamma 93.84(3) _cell_volume 4384(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 0.426 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7271 _exptl_absorpt_correction_T_max 0.9197 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -3.95 _diffrn_reflns_number 16123 _diffrn_reflns_av_R_equivalents 0.1122 _diffrn_reflns_av_sigmaI/netI 0.0960 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15406 _reflns_number_gt 8595 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. The asymmetric unit consists of two crystallographically independent molecules, whose structures are essentially identical. All non hydrogen atoms were refined anisotropically. All C-H hydrogen atoms were placed at the calculated positions, and were treated as riding models. The O-H hydrogen atom for one of the two molecules was found in the difference Fourier map, and its position was refined, while that for another molecule was not found and therefore was not included in the calculation. The largest residual peak of 2.985 eA^3 is close to a Ti atom. The peak may be due to a disorder in the site of the Ti atom. However, we did not include the minor contributor in the calculation because peaks ascribed to the corresponding cyclopentadienyl carbon atoms were not found and the minor component of the disorder is very small. ; _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^)+(0.1227P)^2^+3.2119P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15406 _refine_ls_number_parameters 977 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1496 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.2249 _refine_ls_wR_factor_gt 0.1818 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 1.42975(7) 0.87698(6) 0.14206(5) 0.0399(3) Uani 1 1 d . . . Ti2 Ti 0.81070(6) 0.57238(6) 0.37938(5) 0.0316(2) Uani 1 1 d . . . S1 S 1.21314(10) 0.78920(9) 0.20220(8) 0.0431(4) Uani 1 1 d . . . S2 S 1.19833(11) 1.01298(11) 0.05723(8) 0.0497(4) Uani 1 1 d . . . S3 S 1.59518(10) 1.11340(10) 0.14192(8) 0.0432(4) Uani 1 1 d . . . S4 S 1.59529(10) 0.92352(9) 0.31609(8) 0.0467(4) Uani 1 1 d . . . S5 S 1.04907(11) 0.46170(9) 0.37529(8) 0.0464(4) Uani 1 1 d . . . S6 S 1.00895(10) 0.78864(8) 0.37808(8) 0.0424(3) Uani 1 1 d . . . S7 S 0.62582(10) 0.69280(9) 0.25085(9) 0.0456(4) Uani 1 1 d . . . S8 S 0.65707(11) 0.37013(9) 0.26460(10) 0.0546(4) Uani 1 1 d . . . O1 O 1.4318(3) 0.8212(2) 0.2078(2) 0.0452(9) Uani 1 1 d . . . O2 O 1.3034(2) 0.9103(2) 0.13716(19) 0.0382(8) Uani 1 1 d . . . O3 O 1.4135(3) 1.0215(3) 0.0436(2) 0.0634(12) Uani 1 1 d . . . O4 O 1.5129(3) 0.9742(2) 0.19175(18) 0.0381(8) Uani 1 1 d . . . O5 O 0.8276(3) 0.4612(2) 0.3706(2) 0.0411(9) Uani 1 1 d . . . O6 O 0.9331(2) 0.6083(2) 0.36349(18) 0.0352(8) Uani 1 1 d . . . O7 O 0.7916(3) 0.7979(3) 0.3604(2) 0.0550(11) Uani 1 1 d . . . O8 O 0.7251(2) 0.5595(2) 0.30074(18) 0.0362(8) Uani 1 1 d . . . C1 C 1.3600(6) 1.1021(5) 0.4971(4) 0.080(2) Uani 1 1 d . . . H1A H 1.3308 1.1351 0.5368 0.120 Uiso 1 1 calc R . . H1B H 1.3811 1.1375 0.4722 0.120 Uiso 1 1 calc R . . H1C H 1.4168 1.0785 0.5121 0.120 Uiso 1 1 calc R . . C2 C 1.2503(7) 0.9755(5) 0.4910(4) 0.089(3) Uani 1 1 d . . . H2A H 1.2014 0.9302 0.4620 0.133 Uiso 1 1 calc R . . H2B H 1.2218 1.0091 0.5308 0.133 Uiso 1 1 calc R . . H2C H 1.3078 0.9525 0.5060 0.133 Uiso 1 1 calc R . . C3 C 1.1906(6) 1.0684(6) 0.4289(5) 0.095(3) Uani 1 1 d . . . H3A H 1.1416 1.0237 0.3991 0.142 Uiso 1 1 calc R . . H3B H 1.2094 1.1053 0.4047 0.142 Uiso 1 1 calc R . . H3C H 1.1627 1.0998 0.4698 0.142 Uiso 1 1 calc R . . C4 C 0.8454(7) 0.8827(9) 0.1963(7) 0.170(7) Uani 1 1 d . . . H4A H 0.8698 0.8313 0.1978 0.256 Uiso 1 1 calc R . . H4B H 0.7736 0.8770 0.1925 0.256 Uiso 1 1 calc R . . H4C H 0.8724 0.9286 0.2380 0.256 Uiso 1 1 calc R . . C5 C 0.8291(6) 0.8307(7) 0.0676(7) 0.180(7) Uani 1 1 d . . . H5A H 0.8510 0.8436 0.0291 0.270 Uiso 1 1 calc R . . H5B H 0.7574 0.8285 0.0645 0.270 Uiso 1 1 calc R . . H5C H 0.8493 0.7771 0.0665 0.270 Uiso 1 1 calc R . . C6 C 0.8375(6) 0.9793(6) 0.1338(5) 0.091(3) Uani 1 1 d . . . H6A H 0.8562 0.9901 0.0937 0.137 Uiso 1 1 calc R . . H6B H 0.8652 1.0256 0.1751 0.137 Uiso 1 1 calc R . . H6C H 0.7657 0.9733 0.1311 0.137 Uiso 1 1 calc R . . C7 C 1.3864(11) 1.2344(10) 0.3601(5) 0.189(7) Uani 1 1 d . . . H7A H 1.3687 1.1767 0.3557 0.284 Uiso 1 1 calc R . . H7B H 1.3719 1.2713 0.4041 0.284 Uiso 1 1 calc R . . H7C H 1.4566 1.2430 0.3570 0.284 Uiso 1 1 calc R . . C8 C 1.2165(7) 1.2432(8) 0.3118(5) 0.142(5) Uani 1 1 d . . . H8A H 1.1982 1.1861 0.3087 0.213 Uiso 1 1 calc R . . H8B H 1.1753 1.2555 0.2765 0.213 Uiso 1 1 calc R . . H8C H 1.2069 1.2813 0.3567 0.213 Uiso 1 1 calc R . . C9 C 1.3506(14) 1.3406(7) 0.3064(8) 0.231(10) Uani 1 1 d . . . H9A H 1.4200 1.3490 0.3010 0.346 Uiso 1 1 calc R . . H9B H 1.3388 1.3782 0.3509 0.346 Uiso 1 1 calc R . . H9C H 1.3096 1.3519 0.2704 0.346 Uiso 1 1 calc R . . C10 C 1.9327(5) 1.2037(5) 0.3229(4) 0.081(2) Uani 1 1 d . . . H10A H 1.9028 1.2265 0.2899 0.122 Uiso 1 1 calc R . . H10B H 1.9573 1.1512 0.2988 0.122 Uiso 1 1 calc R . . H10C H 1.9872 1.2429 0.3524 0.122 Uiso 1 1 calc R . . C11 C 1.9011(6) 1.1535(6) 0.4197(5) 0.101(3) Uani 1 1 d . . . H11A H 1.8519 1.1445 0.4477 0.151 Uiso 1 1 calc R . . H11B H 1.9558 1.1927 0.4489 0.151 Uiso 1 1 calc R . . H11C H 1.9256 1.1007 0.3958 0.151 Uiso 1 1 calc R . . C12 C 1.8204(7) 1.2746(5) 0.4067(5) 0.097(3) Uani 1 1 d . . . H12A H 1.7908 1.2982 0.3741 0.145 Uiso 1 1 calc R . . H12B H 1.8773 1.3120 0.4348 0.145 Uiso 1 1 calc R . . H12C H 1.7720 1.2676 0.4360 0.145 Uiso 1 1 calc R . . C13 C 1.2824(5) 1.0309(4) 0.4496(3) 0.0557(16) Uani 1 1 d . . . C14 C 0.8766(4) 0.9000(4) 0.1363(4) 0.0537(16) Uani 1 1 d . . . C15 C 1.3254(6) 1.2536(5) 0.3015(4) 0.072(2) Uani 1 1 d . . . C16 C 1.8541(5) 1.1888(4) 0.3673(3) 0.0540(16) Uani 1 1 d . . . C17 C 1.3980(4) 0.8693(3) 0.2660(3) 0.0379(12) Uani 1 1 d . . . C18 C 1.4650(4) 0.9264(3) 0.3211(3) 0.0392(13) Uani 1 1 d . . . C19 C 1.4277(4) 0.9787(3) 0.3792(3) 0.0426(13) Uani 1 1 d . . . H19 H 1.4722 1.0166 0.4154 0.051 Uiso 1 1 calc R . . C20 C 1.3251(4) 0.9758(3) 0.3846(3) 0.0424(13) Uani 1 1 d . . . C21 C 1.2608(4) 0.9159(3) 0.3301(3) 0.0418(13) Uani 1 1 d . . . H21 H 1.1926 0.9108 0.3335 0.050 Uiso 1 1 calc R . . C22 C 1.2957(4) 0.8641(3) 0.2716(3) 0.0367(12) Uani 1 1 d . . . C23 C 1.2034(4) 0.9077(3) 0.1357(3) 0.0327(11) Uani 1 1 d . . . C24 C 1.1514(4) 0.8570(3) 0.1665(3) 0.0344(11) Uani 1 1 d . . . C25 C 1.0480(4) 0.8565(3) 0.1665(3) 0.0376(12) Uani 1 1 d . . . H25 H 1.0158 0.8232 0.1875 0.045 Uiso 1 1 calc R . . C26 C 0.9914(4) 0.9031(3) 0.1369(3) 0.0392(12) Uani 1 1 d . . . C27 C 1.0424(4) 0.9518(3) 0.1054(3) 0.0399(13) Uani 1 1 d . . . H27 H 1.0065 0.9834 0.0842 0.048 Uiso 1 1 calc R . . C28 C 1.1461(4) 0.9540(3) 0.1050(3) 0.0348(11) Uani 1 1 d . . . C29 C 1.3922(4) 1.0779(4) 0.1051(3) 0.0423(13) Uani 1 1 d . . . C30 C 1.2933(4) 1.0835(4) 0.1194(3) 0.0414(13) Uani 1 1 d . . . C31 C 1.2719(4) 1.1402(4) 0.1815(3) 0.0453(14) Uani 1 1 d . . . H31 H 1.2056 1.1428 0.1900 0.054 Uiso 1 1 calc R . . C32 C 1.3473(4) 1.1933(4) 0.2315(3) 0.0468(14) Uani 1 1 d . . . C33 C 1.4459(4) 1.1862(4) 0.2162(3) 0.0422(13) Uani 1 1 d . . . H33 H 1.4978 1.2209 0.2485 0.051 Uiso 1 1 calc R . . C34 C 1.4688(4) 1.1298(3) 0.1550(3) 0.0352(12) Uani 1 1 d . . . C35 C 1.5928(3) 1.0246(3) 0.2337(3) 0.0330(11) Uani 1 1 d . . . C36 C 1.6375(4) 1.0934(3) 0.2187(3) 0.0347(11) Uani 1 1 d . . . C37 C 1.7203(4) 1.1441(3) 0.2617(3) 0.0389(12) Uani 1 1 d . . . H37 H 1.7476 1.1893 0.2510 0.047 Uiso 1 1 calc R . . C38 C 1.7638(4) 1.1300(3) 0.3197(3) 0.0414(13) Uani 1 1 d . . . C39 C 1.7175(4) 1.0635(3) 0.3356(3) 0.0400(13) Uani 1 1 d . . . H39 H 1.7430 1.0537 0.3754 0.048 Uiso 1 1 calc R . . C40 C 1.6346(4) 1.0116(3) 0.2935(3) 0.0352(12) Uani 1 1 d . . . C41 C 1.4253(8) 0.8222(6) 0.0203(4) 0.083(3) Uani 1 1 d . . . H41 H 1.3887 0.8460 -0.0075 0.100 Uiso 1 1 calc R . . C42 C 1.5266(8) 0.8469(6) 0.0508(5) 0.096(3) Uani 1 1 d . . . H42 H 1.5693 0.8898 0.0466 0.116 Uiso 1 1 calc R . . C43 C 1.5497(7) 0.7954(7) 0.0880(5) 0.090(3) Uani 1 1 d . . . H43 H 1.6109 0.7978 0.1141 0.108 Uiso 1 1 calc R . . C44 C 1.4683(9) 0.7411(5) 0.0799(5) 0.089(3) Uani 1 1 d . . . H44 H 1.4644 0.6986 0.0989 0.107 Uiso 1 1 calc R . . C45 C 1.3923(7) 0.7576(5) 0.0395(4) 0.083(2) Uani 1 1 d . . . H45 H 1.3281 0.7290 0.0272 0.100 Uiso 1 1 calc R . . C46 C 1.0537(8) 0.2919(9) 0.1029(6) 0.173(7) Uani 1 1 d . . . H46A H 1.0541 0.3474 0.1002 0.259 Uiso 1 1 calc R . . H46B H 1.0720 0.2536 0.0607 0.259 Uiso 1 1 calc R . . H46C H 1.1008 0.2934 0.1414 0.259 Uiso 1 1 calc R . . C47 C 0.9496(12) 0.1763(6) 0.1170(6) 0.180(7) Uani 1 1 d . . . H47A H 0.8837 0.1574 0.1233 0.270 Uiso 1 1 calc R . . H47B H 0.9968 0.1779 0.1555 0.270 Uiso 1 1 calc R . . H47C H 0.9680 0.1380 0.0748 0.270 Uiso 1 1 calc R . . C48 C 0.8816(9) 0.2595(7) 0.0494(5) 0.129(4) Uani 1 1 d . . . H48A H 0.8827 0.3151 0.0469 0.194 Uiso 1 1 calc R . . H48B H 0.8145 0.2395 0.0523 0.194 Uiso 1 1 calc R . . H48C H 0.9043 0.2219 0.0085 0.194 Uiso 1 1 calc R . . C49 C 0.3426(7) 0.3359(6) 0.0850(6) 0.120(4) Uani 1 1 d . . . H49A H 0.3965 0.3045 0.0669 0.179 Uiso 1 1 calc R . . H49B H 0.2838 0.3175 0.0512 0.179 Uiso 1 1 calc R . . H49C H 0.3287 0.3267 0.1267 0.179 Uiso 1 1 calc R . . C50 C 0.3957(8) 0.4382(8) 0.0328(5) 0.131(4) Uani 1 1 d . . . H50A H 0.4514 0.4072 0.0180 0.197 Uiso 1 1 calc R . . H50B H 0.4120 0.4964 0.0385 0.197 Uiso 1 1 calc R . . H50C H 0.3380 0.4149 -0.0015 0.197 Uiso 1 1 calc R . . C51 C 0.2879(6) 0.4775(8) 0.1285(6) 0.144(5) Uani 1 1 d . . . H51A H 0.2293 0.4565 0.0947 0.216 Uiso 1 1 calc R . . H51B H 0.3038 0.5367 0.1377 0.216 Uiso 1 1 calc R . . H51C H 0.2754 0.4690 0.1708 0.216 Uiso 1 1 calc R . . C52 C 0.8570(7) 0.4991(5) 0.0825(5) 0.113(4) Uani 1 1 d . . . H52A H 0.7947 0.5164 0.0682 0.170 Uiso 1 1 calc R . . H52B H 0.8462 0.4694 0.1139 0.170 Uiso 1 1 calc R . . H52C H 0.8826 0.4625 0.0426 0.170 Uiso 1 1 calc R . . C53 C 0.9445(12) 0.6204(6) 0.0673(5) 0.173(7) Uani 1 1 d . . . H53A H 0.8820 0.6394 0.0555 0.260 Uiso 1 1 calc R . . H53B H 0.9654 0.5820 0.0261 0.260 Uiso 1 1 calc R . . H53C H 0.9944 0.6681 0.0877 0.260 Uiso 1 1 calc R . . C54 C 1.0268(8) 0.5461(8) 0.1380(5) 0.158(6) Uani 1 1 d . . . H54A H 1.0489 0.5081 0.0971 0.237 Uiso 1 1 calc R . . H54B H 1.0168 0.5173 0.1700 0.237 Uiso 1 1 calc R . . H54C H 1.0767 0.5937 0.1595 0.237 Uiso 1 1 calc R . . C58 C 1.4030(7) 0.6804(17) 0.4655(7) 0.303(16) Uani 1 1 d . . . H58A H 1.4748 0.6888 0.4692 0.455 Uiso 1 1 calc R . . H58B H 1.3834 0.6294 0.4736 0.455 Uiso 1 1 calc R . . H58C H 1.3796 0.7275 0.4993 0.455 Uiso 1 1 calc R . . C59 C 1.4053(8) 0.6055(10) 0.3520(9) 0.252(12) Uani 1 1 d . . . H59A H 1.3688 0.5875 0.3062 0.377 Uiso 1 1 calc R . . H59B H 1.4036 0.5591 0.3689 0.377 Uiso 1 1 calc R . . H59C H 1.4736 0.6240 0.3505 0.377 Uiso 1 1 calc R . . C60 C 1.3960(7) 0.7421(12) 0.3799(16) 0.37(2) Uani 1 1 d . . . H60A H 1.3777 0.7298 0.3311 0.554 Uiso 1 1 calc R . . H60B H 1.4677 0.7517 0.3908 0.554 Uiso 1 1 calc R . . H60C H 1.3670 0.7917 0.4058 0.554 Uiso 1 1 calc R . . C61 C 0.9498(5) 0.2623(4) 0.1129(4) 0.0582(17) Uani 1 1 d . . . C62 C 0.9314(5) 0.5759(4) 0.1187(3) 0.0462(14) Uani 1 1 d . . . C63 C 0.3731(5) 0.4317(5) 0.1016(4) 0.069(2) Uani 1 1 d . . . C64 C 1.3604(5) 0.6739(5) 0.3976(4) 0.069(2) Uani 1 1 d . . . C65 C 0.8565(4) 0.4179(3) 0.3086(3) 0.0374(12) Uani 1 1 d . . . C66 C 0.9583(4) 0.4150(3) 0.3007(3) 0.0370(12) Uani 1 1 d . . . C67 C 0.9872(4) 0.3674(3) 0.2375(3) 0.0407(13) Uani 1 1 d . . . H67 H 1.0550 0.3664 0.2329 0.049 Uiso 1 1 calc R . . C68 C 0.9162(4) 0.3208(3) 0.1804(3) 0.0429(13) Uani 1 1 d . . . C69 C 0.8158(4) 0.3257(3) 0.1893(3) 0.0446(14) Uani 1 1 d . . . H69 H 0.7673 0.2963 0.1520 0.054 Uiso 1 1 calc R . . C70 C 0.7850(4) 0.3730(3) 0.2519(3) 0.0387(13) Uani 1 1 d . . . C71 C 1.0342(4) 0.6248(3) 0.3716(3) 0.0347(11) Uani 1 1 d . . . C72 C 1.0951(4) 0.5617(3) 0.3733(3) 0.0374(12) Uani 1 1 d . . . C73 C 1.1984(4) 0.5786(4) 0.3813(3) 0.0439(13) Uani 1 1 d . . . H73 H 1.2378 0.5358 0.3820 0.053 Uiso 1 1 calc R . . C74 C 1.2454(4) 0.6578(4) 0.3883(3) 0.0429(13) Uani 1 1 d . . . C75 C 1.1850(4) 0.7184(3) 0.3849(3) 0.0412(13) Uani 1 1 d . . . H75 H 1.2144 0.7710 0.3880 0.049 Uiso 1 1 calc R . . C76 C 1.0799(4) 0.7036(3) 0.3768(3) 0.0354(12) Uani 1 1 d . . . C77 C 0.8231(4) 0.7456(3) 0.3016(3) 0.0354(12) Uani 1 1 d . . . C78 C 0.9252(4) 0.7384(3) 0.3003(3) 0.0331(11) Uani 1 1 d . . . C79 C 0.9590(4) 0.6857(3) 0.2407(3) 0.0335(11) Uani 1 1 d . . . H79 H 1.0276 0.6831 0.2399 0.040 Uiso 1 1 calc R . . C80 C 0.8935(4) 0.6371(3) 0.1827(3) 0.0346(11) Uani 1 1 d . . . C81 C 0.7913(4) 0.6434(3) 0.1855(3) 0.0372(12) Uani 1 1 d . . . H81 H 0.7459 0.6113 0.1470 0.045 Uiso 1 1 calc R . . C82 C 0.7560(4) 0.6956(3) 0.2433(3) 0.0356(12) Uani 1 1 d . . . C83 C 0.6429(4) 0.5298(3) 0.2537(3) 0.0352(12) Uani 1 1 d . . . C84 C 0.5912(4) 0.5824(3) 0.2255(3) 0.0368(12) Uani 1 1 d . . . C85 C 0.5056(4) 0.5494(4) 0.1773(3) 0.0475(14) Uani 1 1 d . . . H85 H 0.4724 0.5854 0.1595 0.057 Uiso 1 1 calc R . . C86 C 0.4676(4) 0.4643(4) 0.1548(3) 0.0522(16) Uani 1 1 d . . . C87 C 0.5201(4) 0.4138(4) 0.1814(3) 0.0498(15) Uani 1 1 d . . . H87 H 0.4973 0.3566 0.1665 0.060 Uiso 1 1 calc R . . C88 C 0.6058(4) 0.4430(3) 0.2296(3) 0.0409(13) Uani 1 1 d . . . C89 C 0.8487(6) 0.6354(5) 0.5012(3) 0.068(2) Uani 1 1 d . . . H89 H 0.9135 0.6398 0.5232 0.082 Uiso 1 1 calc R . . C90 C 0.8083(6) 0.6942(4) 0.4750(4) 0.069(2) Uani 1 1 d . . . H90 H 0.8418 0.7446 0.4762 0.083 Uiso 1 1 calc R . . C91 C 0.7083(6) 0.6637(5) 0.4464(4) 0.069(2) Uani 1 1 d . . . H91 H 0.6637 0.6901 0.4255 0.083 Uiso 1 1 calc R . . C92 C 0.6885(6) 0.5871(5) 0.4552(4) 0.071(2) Uani 1 1 d . . . H92 H 0.6277 0.5530 0.4411 0.085 Uiso 1 1 calc R . . C93 C 0.7738(6) 0.5691(5) 0.4885(3) 0.067(2) Uani 1 1 d . . . H93 H 0.7801 0.5212 0.5003 0.080 Uiso 1 1 calc R . . H100 H 0.732(10) 0.801(9) 0.363(7) 0.21(6) Uiso 1 1 d . . . 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 0.0318(5) 0.0415(6) 0.0430(6) 0.0114(5) 0.0038(4) 0.0005(4) Ti2 0.0270(5) 0.0347(5) 0.0334(5) 0.0131(4) 0.0039(4) -0.0004(4) S1 0.0363(7) 0.0396(8) 0.0534(9) 0.0226(7) -0.0077(6) -0.0099(6) S2 0.0344(7) 0.0692(10) 0.0549(9) 0.0389(8) -0.0025(6) -0.0088(7) S3 0.0282(7) 0.0582(9) 0.0527(9) 0.0315(7) 0.0099(6) -0.0003(6) S4 0.0317(7) 0.0519(9) 0.0638(10) 0.0357(8) -0.0072(6) -0.0086(6) S5 0.0400(8) 0.0412(8) 0.0575(9) 0.0236(7) -0.0139(7) -0.0025(6) S6 0.0394(7) 0.0300(7) 0.0487(8) 0.0053(6) -0.0030(6) -0.0010(6) S7 0.0286(7) 0.0432(8) 0.0673(10) 0.0214(7) 0.0071(6) 0.0079(6) S8 0.0300(7) 0.0417(8) 0.0954(13) 0.0315(9) 0.0029(8) -0.0066(6) O1 0.039(2) 0.046(2) 0.049(2) 0.0162(19) 0.0042(18) -0.0042(17) O2 0.0270(18) 0.045(2) 0.048(2) 0.0213(18) 0.0097(16) 0.0036(15) O3 0.048(3) 0.065(3) 0.063(3) 0.001(2) 0.020(2) -0.001(2) O4 0.0326(19) 0.038(2) 0.042(2) 0.0136(17) 0.0010(16) -0.0032(15) O5 0.044(2) 0.035(2) 0.049(2) 0.0187(18) 0.0085(18) 0.0033(16) O6 0.0226(17) 0.0358(19) 0.049(2) 0.0184(17) 0.0015(15) -0.0020(14) O7 0.046(3) 0.058(3) 0.053(3) 0.006(2) 0.013(2) 0.014(2) O8 0.0288(18) 0.037(2) 0.042(2) 0.0166(17) -0.0053(15) -0.0043(15) C1 0.104(6) 0.059(5) 0.063(5) 0.003(4) 0.024(4) -0.011(4) C2 0.128(8) 0.068(5) 0.065(5) 0.014(4) 0.039(5) -0.013(5) C3 0.088(6) 0.086(6) 0.103(7) 0.015(5) 0.024(5) 0.033(5) C4 0.069(6) 0.316(17) 0.277(16) 0.259(15) 0.107(8) 0.100(8) C5 0.039(5) 0.133(9) 0.248(15) -0.081(10) 0.008(7) -0.010(5) C6 0.060(5) 0.107(7) 0.137(8) 0.070(6) 0.036(5) 0.038(5) C7 0.214(16) 0.29(2) 0.063(7) 0.041(10) 0.037(8) 0.112(14) C8 0.085(7) 0.209(13) 0.103(8) 0.003(8) 0.053(6) 0.032(8) C9 0.41(3) 0.060(7) 0.213(16) -0.009(8) 0.214(17) 0.002(11) C10 0.045(4) 0.111(6) 0.075(5) 0.029(5) -0.004(4) -0.039(4) C11 0.080(6) 0.118(7) 0.108(7) 0.075(6) -0.051(5) -0.052(5) C12 0.102(7) 0.071(5) 0.083(6) -0.007(5) 0.007(5) -0.033(5) C13 0.070(4) 0.044(3) 0.050(4) 0.011(3) 0.016(3) 0.003(3) C14 0.029(3) 0.049(4) 0.086(5) 0.024(3) 0.021(3) 0.006(3) C15 0.065(5) 0.083(5) 0.056(4) 0.003(4) 0.025(4) 0.014(4) C16 0.049(4) 0.060(4) 0.050(4) 0.022(3) -0.005(3) -0.021(3) C17 0.037(3) 0.044(3) 0.035(3) 0.019(3) 0.003(2) -0.006(2) C18 0.031(3) 0.048(3) 0.045(3) 0.028(3) 0.000(2) -0.008(2) C19 0.049(3) 0.039(3) 0.040(3) 0.019(3) -0.003(3) -0.010(3) C20 0.048(3) 0.042(3) 0.041(3) 0.020(3) 0.006(3) 0.001(3) C21 0.039(3) 0.046(3) 0.044(3) 0.024(3) 0.003(3) -0.004(3) C22 0.032(3) 0.039(3) 0.042(3) 0.022(3) -0.001(2) -0.008(2) C23 0.027(3) 0.034(3) 0.033(3) 0.009(2) 0.003(2) -0.002(2) C24 0.033(3) 0.033(3) 0.034(3) 0.010(2) 0.001(2) -0.002(2) C25 0.033(3) 0.035(3) 0.045(3) 0.014(2) 0.010(2) -0.008(2) C26 0.029(3) 0.040(3) 0.048(3) 0.013(3) 0.010(2) 0.001(2) C27 0.027(3) 0.035(3) 0.059(4) 0.019(3) 0.005(2) 0.005(2) C28 0.029(3) 0.035(3) 0.038(3) 0.012(2) 0.004(2) -0.004(2) C29 0.035(3) 0.045(3) 0.049(3) 0.021(3) 0.008(3) 0.001(2) C30 0.028(3) 0.048(3) 0.057(4) 0.031(3) 0.001(2) -0.002(2) C31 0.036(3) 0.057(4) 0.054(4) 0.030(3) 0.014(3) 0.012(3) C32 0.043(3) 0.052(4) 0.052(4) 0.023(3) 0.018(3) 0.009(3) C33 0.033(3) 0.045(3) 0.051(4) 0.021(3) 0.002(2) -0.002(2) C34 0.025(3) 0.041(3) 0.047(3) 0.024(3) 0.010(2) 0.000(2) C35 0.025(2) 0.035(3) 0.036(3) 0.009(2) 0.004(2) -0.001(2) C36 0.023(2) 0.037(3) 0.046(3) 0.017(2) 0.006(2) 0.002(2) C37 0.037(3) 0.037(3) 0.045(3) 0.019(3) 0.005(2) -0.004(2) C38 0.034(3) 0.041(3) 0.044(3) 0.010(3) 0.007(2) -0.009(2) C39 0.031(3) 0.048(3) 0.040(3) 0.016(3) 0.003(2) -0.008(2) C40 0.029(3) 0.039(3) 0.040(3) 0.018(2) 0.007(2) 0.000(2) C41 0.125(8) 0.085(6) 0.038(4) 0.013(4) 0.022(4) 0.043(6) C42 0.123(8) 0.069(6) 0.086(6) 0.000(5) 0.072(6) -0.008(5) C43 0.063(5) 0.119(8) 0.076(6) 0.010(6) 0.025(4) 0.031(5) C44 0.141(9) 0.067(5) 0.071(6) 0.024(4) 0.044(6) 0.039(6) C45 0.094(6) 0.074(6) 0.060(5) -0.002(4) 0.008(5) -0.007(5) C46 0.117(9) 0.203(13) 0.122(9) -0.048(9) 0.080(8) -0.042(9) C47 0.38(2) 0.063(6) 0.131(10) 0.038(6) 0.126(12) 0.104(10) C48 0.172(11) 0.128(9) 0.063(6) 0.000(6) -0.002(6) 0.052(8) C49 0.079(6) 0.117(8) 0.121(8) 0.010(6) -0.042(6) -0.031(6) C50 0.099(8) 0.194(12) 0.075(7) 0.031(7) -0.029(6) -0.011(8) C51 0.043(5) 0.174(11) 0.146(10) -0.021(8) -0.032(6) 0.020(6) C52 0.099(7) 0.080(6) 0.113(8) -0.033(5) 0.034(6) 0.009(5) C53 0.37(2) 0.090(7) 0.095(8) 0.036(6) 0.148(11) 0.054(10) C54 0.113(8) 0.210(13) 0.083(7) -0.045(7) -0.010(6) 0.112(9) C58 0.033(5) 0.73(5) 0.128(11) 0.145(19) -0.025(6) -0.036(12) C59 0.053(6) 0.244(18) 0.31(2) -0.103(16) 0.084(10) -0.047(8) C60 0.033(5) 0.35(3) 0.93(6) 0.50(4) 0.028(14) 0.004(9) C61 0.065(4) 0.042(3) 0.058(4) 0.006(3) 0.010(3) 0.007(3) C62 0.056(4) 0.043(3) 0.038(3) 0.010(3) 0.016(3) 0.007(3) C63 0.039(4) 0.086(5) 0.069(5) 0.017(4) -0.014(3) -0.003(3) C64 0.030(3) 0.070(5) 0.106(6) 0.034(4) 0.002(4) -0.001(3) C65 0.035(3) 0.028(3) 0.052(3) 0.018(3) 0.000(2) 0.000(2) C66 0.030(3) 0.028(3) 0.051(3) 0.014(2) -0.004(2) -0.004(2) C67 0.032(3) 0.033(3) 0.056(4) 0.016(3) 0.001(3) 0.000(2) C68 0.047(3) 0.029(3) 0.051(4) 0.014(3) 0.002(3) -0.002(2) C69 0.038(3) 0.033(3) 0.058(4) 0.016(3) -0.011(3) -0.009(2) C70 0.027(3) 0.031(3) 0.059(4) 0.019(3) 0.001(2) -0.002(2) C71 0.026(3) 0.036(3) 0.037(3) 0.009(2) -0.002(2) -0.004(2) C72 0.028(3) 0.034(3) 0.046(3) 0.012(2) -0.003(2) -0.002(2) C73 0.034(3) 0.045(3) 0.054(4) 0.018(3) 0.002(3) 0.009(2) C74 0.028(3) 0.049(3) 0.050(3) 0.016(3) 0.001(2) -0.002(2) C75 0.032(3) 0.039(3) 0.047(3) 0.012(3) -0.002(2) -0.010(2) C76 0.029(3) 0.033(3) 0.038(3) 0.008(2) -0.002(2) -0.005(2) C77 0.038(3) 0.031(3) 0.038(3) 0.011(2) 0.012(2) 0.009(2) C78 0.031(3) 0.026(3) 0.043(3) 0.015(2) 0.001(2) -0.003(2) C79 0.029(3) 0.034(3) 0.041(3) 0.015(2) 0.010(2) 0.002(2) C80 0.037(3) 0.032(3) 0.038(3) 0.016(2) 0.010(2) 0.007(2) C81 0.034(3) 0.044(3) 0.035(3) 0.017(2) 0.002(2) 0.003(2) C82 0.027(3) 0.036(3) 0.051(3) 0.022(3) 0.006(2) 0.006(2) C83 0.025(3) 0.041(3) 0.035(3) 0.008(2) 0.004(2) -0.002(2) C84 0.028(3) 0.046(3) 0.037(3) 0.015(2) 0.007(2) 0.003(2) C85 0.026(3) 0.069(4) 0.050(4) 0.026(3) 0.000(2) 0.004(3) C86 0.024(3) 0.072(4) 0.052(4) 0.015(3) -0.001(3) -0.001(3) C87 0.032(3) 0.048(3) 0.058(4) 0.007(3) 0.001(3) -0.010(3) C88 0.026(3) 0.043(3) 0.049(3) 0.012(3) 0.001(2) -0.001(2) C89 0.075(5) 0.083(5) 0.037(4) 0.010(4) 0.000(3) 0.007(4) C90 0.097(6) 0.048(4) 0.054(4) 0.005(3) 0.025(4) 0.003(4) C91 0.074(5) 0.080(5) 0.068(5) 0.031(4) 0.035(4) 0.040(4) C92 0.062(5) 0.090(6) 0.064(5) 0.023(4) 0.036(4) 0.005(4) C93 0.090(6) 0.076(5) 0.050(4) 0.036(4) 0.026(4) 0.018(4) _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 O2 1.835(3) . ? Ti1 O4 1.842(4) . ? Ti1 O1 1.898(4) . ? Ti1 C43 2.320(8) . ? Ti1 C42 2.332(7) . ? Ti1 C44 2.344(8) . ? Ti1 C41 2.357(7) . ? Ti1 C45 2.358(8) . ? Ti1 C17 2.682(5) . ? Ti2 O6 1.820(3) . ? Ti2 O8 1.835(3) . ? Ti2 O5 1.861(4) . ? Ti2 C90 2.324(7) . ? Ti2 C91 2.329(6) . ? Ti2 C92 2.352(6) . ? Ti2 C89 2.361(7) . ? Ti2 C93 2.373(6) . ? Ti2 C65 2.675(5) . ? S1 C24 1.771(5) . ? S1 C22 1.777(5) . ? S2 C30 1.771(6) . ? S2 C28 1.783(5) . ? S3 C36 1.779(5) . ? S3 C34 1.777(5) . ? S4 C40 1.773(5) . ? S4 C18 1.772(5) . ? S5 C66 1.778(5) . ? S5 C72 1.779(5) . ? S6 C78 1.777(5) . ? S6 C76 1.776(5) . ? S7 C82 1.776(5) . ? S7 C84 1.776(6) . ? S8 C70 1.771(5) . ? S8 C88 1.773(6) . ? O1 C17 1.346(6) . ? O2 C23 1.342(6) . ? O3 C29 1.375(7) . ? O4 C35 1.351(6) . ? O5 C65 1.353(7) . ? O6 C71 1.355(6) . ? O7 C77 1.364(6) . ? O7 H100 0.81(13) . ? O8 C83 1.343(6) . ? C1 C13 1.527(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C13 1.537(9) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C13 1.517(10) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C14 1.459(11) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C14 1.544(12) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C14 1.490(9) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C15 1.532(13) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C15 1.512(11) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C15 1.456(13) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C16 1.530(9) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C16 1.512(9) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C16 1.528(11) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C20 1.542(8) . ? C14 C26 1.543(7) . ? C15 C32 1.529(9) . ? C16 C38 1.540(8) . ? C17 C22 1.394(7) . ? C17 C18 1.405(7) . ? C18 C19 1.391(8) . ? C19 C20 1.397(8) . ? C19 H19 0.9300 . ? C20 C21 1.400(8) . ? C21 C22 1.377(8) . ? C21 H21 0.9300 . ? C23 C28 1.391(7) . ? C23 C24 1.419(7) . ? C24 C25 1.393(7) . ? C25 C26 1.377(7) . ? C25 H25 0.9300 . ? C26 C27 1.397(7) . ? C27 C28 1.397(7) . ? C27 H27 0.9300 . ? C29 C34 1.397(8) . ? C29 C30 1.397(7) . ? C30 C31 1.386(8) . ? C31 C32 1.395(8) . ? C31 H31 0.9300 . ? C32 C33 1.400(8) . ? C33 C34 1.378(8) . ? C33 H33 0.9300 . ? C35 C40 1.398(7) . ? C35 C36 1.415(7) . ? C36 C37 1.387(7) . ? C37 C38 1.383(8) . ? C37 H37 0.9300 . ? C38 C39 1.401(7) . ? C39 C40 1.389(7) . ? C39 H39 0.9300 . ? C41 C45 1.348(11) . ? C41 C42 1.417(12) . ? C41 H41 0.9300 . ? C42 C43 1.375(13) . ? C42 H42 0.9300 . ? C43 C44 1.343(12) . ? C43 H43 0.9300 . ? C44 C45 1.359(12) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C61 1.512(11) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C61 1.488(10) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 C61 1.508(11) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C63 1.556(12) . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 C63 1.519(12) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C63 1.477(11) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 C62 1.507(10) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C62 1.513(10) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 C62 1.479(10) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C58 C64 1.425(14) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 C64 1.435(14) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 C64 1.395(14) . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 C68 1.541(9) . ? C62 C80 1.535(7) . ? C63 C86 1.532(8) . ? C64 C74 1.537(8) . ? C65 C70 1.395(7) . ? C65 C66 1.400(7) . ? C66 C67 1.389(8) . ? C67 C68 1.403(7) . ? C67 H67 0.9300 . ? C68 C69 1.389(8) . ? C69 C70 1.390(8) . ? C69 H69 0.9300 . ? C71 C76 1.397(7) . ? C71 C72 1.397(7) . ? C72 C73 1.384(7) . ? C73 C74 1.398(8) . ? C73 H73 0.9300 . ? C74 C75 1.368(8) . ? C75 C76 1.406(7) . ? C75 H75 0.9300 . ? C77 C78 1.391(7) . ? C77 C82 1.404(7) . ? C78 C79 1.392(7) . ? C79 C80 1.382(7) . ? C79 H79 0.9300 . ? C80 C81 1.394(7) . ? C81 C82 1.374(7) . ? C81 H81 0.9300 . ? C83 C84 1.404(7) . ? C83 C88 1.417(7) . ? C84 C85 1.393(7) . ? C85 C86 1.396(9) . ? C85 H85 0.9300 . ? C86 C87 1.363(9) . ? C87 C88 1.390(8) . ? C87 H87 0.9300 . ? C89 C93 1.393(10) . ? C89 C90 1.400(10) . ? C89 H89 0.9300 . ? C90 C91 1.404(10) . ? C90 H90 0.9300 . ? C91 C92 1.382(10) . ? C91 H91 0.9300 . ? C92 C93 1.385(10) . ? C92 H92 0.9300 . ? C93 H93 0.9300 . ? 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 O2 Ti1 O4 105.34(17) . . ? O2 Ti1 O1 104.77(16) . . ? O4 Ti1 O1 100.72(17) . . ? O2 Ti1 C43 149.0(3) . . ? O4 Ti1 C43 98.3(3) . . ? O1 Ti1 C43 90.0(3) . . ? O2 Ti1 C42 124.0(4) . . ? O4 Ti1 C42 91.4(3) . . ? O1 Ti1 C42 124.3(3) . . ? C43 Ti1 C42 34.4(3) . . ? O2 Ti1 C44 123.6(3) . . ? O4 Ti1 C44 130.3(3) . . ? O1 Ti1 C44 76.1(2) . . ? C43 Ti1 C44 33.5(3) . . ? C42 Ti1 C44 56.0(3) . . ? O2 Ti1 C41 93.3(3) . . ? O4 Ti1 C41 118.6(3) . . ? O1 Ti1 C41 130.4(3) . . ? C43 Ti1 C41 57.3(3) . . ? C42 Ti1 C41 35.2(3) . . ? C44 Ti1 C41 55.8(3) . . ? O2 Ti1 C45 94.0(3) . . ? O4 Ti1 C45 147.9(3) . . ? O1 Ti1 C45 98.7(3) . . ? C43 Ti1 C45 56.3(3) . . ? C42 Ti1 C45 56.5(3) . . ? C44 Ti1 C45 33.6(3) . . ? C41 Ti1 C45 33.2(3) . . ? O2 Ti1 C17 86.12(16) . . ? O4 Ti1 C17 85.87(16) . . ? O1 Ti1 C17 28.05(16) . . ? C43 Ti1 C17 115.8(3) . . ? C42 Ti1 C17 149.2(4) . . ? C44 Ti1 C17 103.9(2) . . ? C41 Ti1 C17 154.6(3) . . ? C45 Ti1 C17 121.4(3) . . ? O6 Ti2 O8 105.50(16) . . ? O6 Ti2 O5 101.04(16) . . ? O8 Ti2 O5 102.46(17) . . ? O6 Ti2 C90 92.4(2) . . ? O8 Ti2 C90 117.2(2) . . ? O5 Ti2 C90 132.7(2) . . ? O6 Ti2 C91 122.8(2) . . ? O8 Ti2 C91 90.0(2) . . ? O5 Ti2 C91 129.3(2) . . ? C90 Ti2 C91 35.1(3) . . ? O6 Ti2 C92 148.5(2) . . ? O8 Ti2 C92 97.1(2) . . ? O5 Ti2 C92 95.0(2) . . ? C90 Ti2 C92 57.3(3) . . ? C91 Ti2 C92 34.3(3) . . ? O6 Ti2 C89 93.6(2) . . ? O8 Ti2 C89 147.9(2) . . ? O5 Ti2 C89 98.8(2) . . ? C90 Ti2 C89 34.8(2) . . ? C91 Ti2 C89 57.9(3) . . ? C92 Ti2 C89 57.0(3) . . ? O6 Ti2 C93 124.2(2) . . ? O8 Ti2 C93 129.5(2) . . ? O5 Ti2 C93 78.2(2) . . ? C90 Ti2 C93 57.3(3) . . ? C91 Ti2 C93 57.3(3) . . ? C92 Ti2 C93 34.1(2) . . ? C89 Ti2 C93 34.2(3) . . ? O6 Ti2 C65 84.78(16) . . ? O8 Ti2 C65 85.13(16) . . ? O5 Ti2 C65 28.02(16) . . ? C90 Ti2 C65 157.3(2) . . ? C91 Ti2 C65 152.2(2) . . ? C92 Ti2 C65 119.3(2) . . ? C89 Ti2 C65 122.8(2) . . ? C93 Ti2 C65 106.2(2) . . ? C24 S1 C22 100.7(2) . . ? C30 S2 C28 102.6(2) . . ? C36 S3 C34 100.0(2) . . ? C40 S4 C18 106.0(2) . . ? C66 S5 C72 106.5(2) . . ? C78 S6 C76 99.4(2) . . ? C82 S7 C84 101.1(2) . . ? C70 S8 C88 105.8(3) . . ? C17 O1 Ti1 110.4(3) . . ? C23 O2 Ti1 159.5(3) . . ? C35 O4 Ti1 159.2(3) . . ? C65 O5 Ti2 111.7(3) . . ? C71 O6 Ti2 158.3(3) . . ? C77 O7 H100 121(10) . . ? C83 O8 Ti2 157.1(3) . . ? C13 C1 H1A 109.5 . . ? C13 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C13 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C13 C2 H2A 109.5 . . ? C13 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C13 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C13 C3 H3A 109.5 . . ? C13 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C13 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C14 C4 H4A 109.5 . . ? C14 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C14 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C14 C5 H5A 109.5 . . ? C14 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C14 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C14 C6 H6A 109.5 . . ? C14 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C14 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C15 C7 H7A 109.5 . . ? C15 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C15 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C15 C8 H8A 109.5 . . ? C15 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C15 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C15 C9 H9A 109.5 . . ? C15 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C15 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C16 C10 H10A 109.5 . . ? C16 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C16 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 H11A 109.5 . . ? C16 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C16 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C16 C12 H12A 109.5 . . ? C16 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C16 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 C13 C20 111.8(6) . . ? C1 C13 C3 109.3(6) . . ? C20 C13 C3 110.5(6) . . ? C1 C13 C2 108.1(6) . . ? C20 C13 C2 109.1(5) . . ? C3 C13 C2 108.0(7) . . ? C4 C14 C6 109.2(7) . . ? C4 C14 C26 111.7(6) . . ? C6 C14 C26 112.5(5) . . ? C4 C14 C5 111.2(9) . . ? C6 C14 C5 105.0(8) . . ? C26 C14 C5 107.0(5) . . ? C9 C15 C8 108.0(10) . . ? C9 C15 C32 109.6(7) . . ? C8 C15 C32 112.6(7) . . ? C9 C15 C7 110.9(11) . . ? C8 C15 C7 106.5(9) . . ? C32 C15 C7 109.1(7) . . ? C11 C16 C10 109.6(6) . . ? C11 C16 C38 112.4(5) . . ? C10 C16 C38 109.5(5) . . ? C11 C16 C12 108.4(7) . . ? C10 C16 C12 107.4(6) . . ? C38 C16 C12 109.6(6) . . ? O1 C17 C22 120.2(5) . . ? O1 C17 C18 120.3(5) . . ? C22 C17 C18 119.5(5) . . ? O1 C17 Ti1 41.6(2) . . ? C22 C17 Ti1 110.7(3) . . ? C18 C17 Ti1 112.7(3) . . ? C19 C18 C17 119.2(5) . . ? C19 C18 S4 122.4(4) . . ? C17 C18 S4 118.2(4) . . ? C18 C19 C20 121.9(5) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C19 C20 C21 117.4(5) . . ? C19 C20 C13 122.7(5) . . ? C21 C20 C13 119.7(5) . . ? C22 C21 C20 121.9(5) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C21 C22 C17 120.1(5) . . ? C21 C22 S1 121.5(4) . . ? C17 C22 S1 118.4(4) . . ? O2 C23 C28 122.6(4) . . ? O2 C23 C24 120.6(4) . . ? C28 C23 C24 116.9(4) . . ? C25 C24 C23 120.2(5) . . ? C25 C24 S1 117.8(4) . . ? C23 C24 S1 121.8(4) . . ? C26 C25 C24 122.9(5) . . ? C26 C25 H25 118.5 . . ? C24 C25 H25 118.5 . . ? C25 C26 C27 116.8(5) . . ? C25 C26 C14 121.9(5) . . ? C27 C26 C14 121.3(5) . . ? C28 C27 C26 121.6(5) . . ? C28 C27 H27 119.2 . . ? C26 C27 H27 119.2 . . ? C23 C28 C27 121.6(5) . . ? C23 C28 S2 122.3(4) . . ? C27 C28 S2 115.9(4) . . ? C34 C29 O3 120.9(5) . . ? C34 C29 C30 118.6(5) . . ? O3 C29 C30 120.5(5) . . ? C31 C30 C29 120.5(5) . . ? C31 C30 S2 121.8(4) . . ? C29 C30 S2 117.6(5) . . ? C30 C31 C32 121.7(5) . . ? C30 C31 H31 119.1 . . ? C32 C31 H31 119.1 . . ? C33 C32 C31 116.7(5) . . ? C33 C32 C15 120.8(6) . . ? C31 C32 C15 122.4(5) . . ? C34 C33 C32 122.5(5) . . ? C34 C33 H33 118.8 . . ? C32 C33 H33 118.8 . . ? C29 C34 C33 120.0(5) . . ? C29 C34 S3 118.5(4) . . ? C33 C34 S3 121.1(4) . . ? O4 C35 C40 121.9(4) . . ? O4 C35 C36 120.9(4) . . ? C40 C35 C36 117.1(4) . . ? C37 C36 C35 120.5(5) . . ? C37 C36 S3 117.9(4) . . ? C35 C36 S3 121.5(4) . . ? C36 C37 C38 122.6(5) . . ? C36 C37 H37 118.7 . . ? C38 C37 H37 118.7 . . ? C37 C38 C39 116.7(5) . . ? C37 C38 C16 121.3(5) . . ? C39 C38 C16 121.9(5) . . ? C40 C39 C38 121.9(5) . . ? C40 C39 H39 119.1 . . ? C38 C39 H39 119.1 . . ? C35 C40 C39 121.1(5) . . ? C35 C40 S4 123.1(4) . . ? C39 C40 S4 115.4(4) . . ? C45 C41 C42 106.8(8) . . ? C45 C41 Ti1 73.4(5) . . ? C42 C41 Ti1 71.4(4) . . ? C45 C41 H41 126.6 . . ? C42 C41 H41 126.6 . . ? Ti1 C41 H41 120.4 . . ? C43 C42 C41 107.0(8) . . ? C43 C42 Ti1 72.3(5) . . ? C41 C42 Ti1 73.4(4) . . ? C43 C42 H42 126.5 . . ? C41 C42 H42 126.5 . . ? Ti1 C42 H42 119.7 . . ? C44 C43 C42 107.8(9) . . ? C44 C43 Ti1 74.3(5) . . ? C42 C43 Ti1 73.3(5) . . ? C44 C43 H43 126.1 . . ? C42 C43 H43 126.1 . . ? Ti1 C43 H43 118.3 . . ? C43 C44 C45 109.6(9) . . ? C43 C44 Ti1 72.3(5) . . ? C45 C44 Ti1 73.8(5) . . ? C43 C44 H44 125.2 . . ? C45 C44 H44 125.2 . . ? Ti1 C44 H44 120.5 . . ? C41 C45 C44 108.8(9) . . ? C41 C45 Ti1 73.4(5) . . ? C44 C45 Ti1 72.6(5) . . ? C41 C45 H45 125.6 . . ? C44 C45 H45 125.6 . . ? Ti1 C45 H45 120.1 . . ? C61 C46 H46A 109.5 . . ? C61 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C61 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C61 C47 H47A 109.5 . . ? C61 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C61 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C61 C48 H48A 109.5 . . ? C61 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C61 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C63 C49 H49A 109.5 . . ? C63 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C63 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C63 C50 H50A 109.5 . . ? C63 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C63 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C63 C51 H51A 109.5 . . ? C63 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C63 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C62 C52 H52A 109.5 . . ? C62 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C62 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C62 C53 H53A 109.5 . . ? C62 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C62 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C62 C54 H54A 109.5 . . ? C62 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C62 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C64 C58 H58A 109.5 . . ? C64 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C64 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C64 C59 H59A 109.5 . . ? C64 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C64 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C64 C60 H60A 109.5 . . ? C64 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C64 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C47 C61 C46 109.3(10) . . ? C47 C61 C48 110.0(8) . . ? C46 C61 C48 105.9(9) . . ? C47 C61 C68 107.7(6) . . ? C46 C61 C68 112.1(6) . . ? C48 C61 C68 111.9(6) . . ? C54 C62 C80 111.2(5) . . ? C54 C62 C53 110.7(9) . . ? C80 C62 C53 108.6(5) . . ? C54 C62 C52 107.6(7) . . ? C80 C62 C52 111.6(5) . . ? C53 C62 C52 107.1(8) . . ? C51 C63 C86 110.4(6) . . ? C51 C63 C50 113.3(8) . . ? C86 C63 C50 109.0(6) . . ? C51 C63 C49 107.6(8) . . ? C86 C63 C49 111.7(6) . . ? C50 C63 C49 104.7(8) . . ? C58 C64 C74 111.5(7) . . ? C58 C64 C60 111.8(14) . . ? C74 C64 C60 113.8(7) . . ? C58 C64 C59 104.2(12) . . ? C74 C64 C59 112.6(7) . . ? C60 C64 C59 102.1(13) . . ? O5 C65 C70 120.2(5) . . ? O5 C65 C66 120.8(5) . . ? C70 C65 C66 119.0(5) . . ? O5 C65 Ti2 40.2(2) . . ? C70 C65 Ti2 113.3(3) . . ? C66 C65 Ti2 113.5(3) . . ? C65 C66 C67 120.2(5) . . ? C65 C66 S5 118.8(4) . . ? C67 C66 S5 120.5(4) . . ? C66 C67 C68 121.5(5) . . ? C66 C67 H67 119.3 . . ? C68 C67 H67 119.3 . . ? C69 C68 C67 117.1(5) . . ? C69 C68 C61 122.2(5) . . ? C67 C68 C61 120.6(5) . . ? C68 C69 C70 122.5(5) . . ? C68 C69 H69 118.8 . . ? C70 C69 H69 118.8 . . ? C65 C70 C69 119.7(5) . . ? C65 C70 S8 118.4(4) . . ? C69 C70 S8 121.6(4) . . ? O6 C71 C76 121.3(5) . . ? O6 C71 C72 120.1(4) . . ? C76 C71 C72 118.5(5) . . ? C73 C72 C71 119.9(5) . . ? C73 C72 S5 116.0(4) . . ? C71 C72 S5 123.7(4) . . ? C72 C73 C74 122.3(5) . . ? C72 C73 H73 118.8 . . ? C74 C73 H73 118.8 . . ? C75 C74 C73 117.2(5) . . ? C75 C74 C64 122.3(5) . . ? C73 C74 C64 120.5(5) . . ? C74 C75 C76 122.1(5) . . ? C74 C75 H75 118.9 . . ? C76 C75 H75 118.9 . . ? C71 C76 C75 119.9(5) . . ? C71 C76 S6 121.8(4) . . ? C75 C76 S6 118.3(4) . . ? O7 C77 C78 119.0(5) . . ? O7 C77 C82 122.3(5) . . ? C78 C77 C82 118.6(5) . . ? C79 C78 C77 119.9(5) . . ? C79 C78 S6 120.8(4) . . ? C77 C78 S6 118.9(4) . . ? C80 C79 C78 121.8(5) . . ? C80 C79 H79 119.1 . . ? C78 C79 H79 119.1 . . ? C79 C80 C81 117.6(5) . . ? C79 C80 C62 121.3(5) . . ? C81 C80 C62 121.1(5) . . ? C82 C81 C80 121.8(5) . . ? C82 C81 H81 119.1 . . ? C80 C81 H81 119.1 . . ? C81 C82 C77 120.2(5) . . ? C81 C82 S7 121.4(4) . . ? C77 C82 S7 118.0(4) . . ? O8 C83 C84 121.9(5) . . ? O8 C83 C88 120.8(5) . . ? C84 C83 C88 117.3(5) . . ? C85 C84 C83 120.2(5) . . ? C85 C84 S7 116.5(4) . . ? C83 C84 S7 123.3(4) . . ? C86 C85 C84 122.6(5) . . ? C86 C85 H85 118.7 . . ? C84 C85 H85 118.7 . . ? C87 C86 C85 116.4(5) . . ? C87 C86 C63 123.4(6) . . ? C85 C86 C63 120.2(6) . . ? C86 C87 C88 123.6(6) . . ? C86 C87 H87 118.2 . . ? C88 C87 H87 118.2 . . ? C87 C88 C83 119.8(5) . . ? C87 C88 S8 117.2(4) . . ? C83 C88 S8 122.7(4) . . ? C93 C89 C90 107.4(7) . . ? C93 C89 Ti2 73.4(4) . . ? C90 C89 Ti2 71.2(4) . . ? C93 C89 H89 126.3 . . ? C90 C89 H89 126.3 . . ? Ti2 C89 H89 121.0 . . ? C89 C90 C91 108.1(7) . . ? C89 C90 Ti2 74.1(4) . . ? C91 C90 Ti2 72.6(4) . . ? C89 C90 H90 125.9 . . ? C91 C90 H90 125.9 . . ? Ti2 C90 H90 119.2 . . ? C92 C91 C90 107.2(7) . . ? C92 C91 Ti2 73.8(4) . . ? C90 C91 Ti2 72.2(4) . . ? C92 C91 H91 126.4 . . ? C90 C91 H91 126.4 . . ? Ti2 C91 H91 119.5 . . ? C93 C92 C91 109.1(7) . . ? C93 C92 Ti2 73.8(4) . . ? C91 C92 Ti2 71.9(4) . . ? C93 C92 H92 125.5 . . ? C91 C92 H92 125.5 . . ? Ti2 C92 H92 120.6 . . ? C92 C93 C89 108.1(7) . . ? C92 C93 Ti2 72.1(4) . . ? C89 C93 Ti2 72.4(4) . . ? C92 C93 H93 125.9 . . ? C89 C93 H93 125.9 . . ? Ti2 C93 H93 121.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Ti1 O1 C17 -49.9(4) . . . . ? O4 Ti1 O1 C17 59.2(3) . . . . ? C43 Ti1 O1 C17 157.6(4) . . . . ? C42 Ti1 O1 C17 158.4(4) . . . . ? C44 Ti1 O1 C17 -171.6(5) . . . . ? C41 Ti1 O1 C17 -157.5(4) . . . . ? C45 Ti1 O1 C17 -146.5(4) . . . . ? O4 Ti1 O2 C23 -143.9(9) . . . . ? O1 Ti1 O2 C23 -38.1(10) . . . . ? C43 Ti1 O2 C23 77.9(12) . . . . ? C42 Ti1 O2 C23 113.7(10) . . . . ? C44 Ti1 O2 C23 44.9(10) . . . . ? C41 Ti1 O2 C23 95.3(10) . . . . ? C45 Ti1 O2 C23 62.0(10) . . . . ? C17 Ti1 O2 C23 -59.2(10) . . . . ? O2 Ti1 O4 C35 152.4(9) . . . . ? O1 Ti1 O4 C35 43.6(10) . . . . ? C43 Ti1 O4 C35 -47.9(10) . . . . ? C42 Ti1 O4 C35 -81.7(10) . . . . ? C44 Ti1 O4 C35 -37.2(11) . . . . ? C41 Ti1 O4 C35 -105.1(10) . . . . ? C45 Ti1 O4 C35 -82.6(11) . . . . ? C17 Ti1 O4 C35 67.5(10) . . . . ? O6 Ti2 O5 C65 -55.7(3) . . . . ? O8 Ti2 O5 C65 53.1(3) . . . . ? C90 Ti2 O5 C65 -159.5(4) . . . . ? C91 Ti2 O5 C65 153.5(4) . . . . ? C92 Ti2 O5 C65 151.5(4) . . . . ? C89 Ti2 O5 C65 -151.1(4) . . . . ? C93 Ti2 O5 C65 -178.7(4) . . . . ? O8 Ti2 O6 C71 -161.9(9) . . . . ? O5 Ti2 O6 C71 -55.5(9) . . . . ? C90 Ti2 O6 C71 79.0(9) . . . . ? C91 Ti2 O6 C71 97.8(9) . . . . ? C92 Ti2 O6 C71 63.8(10) . . . . ? C89 Ti2 O6 C71 44.2(9) . . . . ? C93 Ti2 O6 C71 27.7(10) . . . . ? C65 Ti2 O6 C71 -78.4(9) . . . . ? O6 Ti2 O8 C83 157.4(9) . . . . ? O5 Ti2 O8 C83 52.1(9) . . . . ? C90 Ti2 O8 C83 -101.5(9) . . . . ? C91 Ti2 O8 C83 -78.4(9) . . . . ? C92 Ti2 O8 C83 -44.7(9) . . . . ? C89 Ti2 O8 C83 -78.2(10) . . . . ? C93 Ti2 O8 C83 -32.8(10) . . . . ? C65 Ti2 O8 C83 74.2(9) . . . . ? Ti1 O1 C17 C22 87.7(5) . . . . ? Ti1 O1 C17 C18 -90.8(5) . . . . ? O2 Ti1 C17 O1 132.1(3) . . . . ? O4 Ti1 C17 O1 -122.2(3) . . . . ? C43 Ti1 C17 O1 -25.0(5) . . . . ? C42 Ti1 C17 O1 -36.4(6) . . . . ? C44 Ti1 C17 O1 8.4(5) . . . . ? C41 Ti1 C17 O1 42.6(7) . . . . ? C45 Ti1 C17 O1 39.8(4) . . . . ? O2 Ti1 C17 C22 19.6(4) . . . . ? O4 Ti1 C17 C22 125.3(4) . . . . ? O1 Ti1 C17 C22 -112.6(5) . . . . ? C43 Ti1 C17 C22 -137.5(4) . . . . ? C42 Ti1 C17 C22 -149.0(5) . . . . ? C44 Ti1 C17 C22 -104.1(5) . . . . ? C41 Ti1 C17 C22 -69.9(7) . . . . ? C45 Ti1 C17 C22 -72.8(5) . . . . ? O2 Ti1 C17 C18 -117.2(4) . . . . ? O4 Ti1 C17 C18 -11.5(4) . . . . ? O1 Ti1 C17 C18 110.7(5) . . . . ? C43 Ti1 C17 C18 85.7(5) . . . . ? C42 Ti1 C17 C18 74.2(6) . . . . ? C44 Ti1 C17 C18 119.1(5) . . . . ? C41 Ti1 C17 C18 153.3(6) . . . . ? C45 Ti1 C17 C18 150.4(4) . . . . ? O1 C17 C18 C19 176.5(5) . . . . ? C22 C17 C18 C19 -2.0(7) . . . . ? Ti1 C17 C18 C19 130.6(4) . . . . ? O1 C17 C18 S4 -7.9(7) . . . . ? C22 C17 C18 S4 173.5(4) . . . . ? Ti1 C17 C18 S4 -53.9(5) . . . . ? C40 S4 C18 C19 -80.8(5) . . . . ? C40 S4 C18 C17 103.8(4) . . . . ? C17 C18 C19 C20 0.3(8) . . . . ? S4 C18 C19 C20 -175.1(4) . . . . ? C18 C19 C20 C21 2.2(8) . . . . ? C18 C19 C20 C13 177.8(5) . . . . ? C1 C13 C20 C19 14.5(8) . . . . ? C3 C13 C20 C19 136.4(6) . . . . ? C2 C13 C20 C19 -105.1(7) . . . . ? C1 C13 C20 C21 -170.1(6) . . . . ? C3 C13 C20 C21 -48.2(8) . . . . ? C2 C13 C20 C21 70.4(8) . . . . ? C19 C20 C21 C22 -3.0(8) . . . . ? C13 C20 C21 C22 -178.7(5) . . . . ? C20 C21 C22 C17 1.3(8) . . . . ? C20 C21 C22 S1 -179.1(4) . . . . ? O1 C17 C22 C21 -177.3(5) . . . . ? C18 C17 C22 C21 1.3(8) . . . . ? Ti1 C17 C22 C21 -132.2(4) . . . . ? O1 C17 C22 S1 3.1(7) . . . . ? C18 C17 C22 S1 -178.3(4) . . . . ? Ti1 C17 C22 S1 48.2(5) . . . . ? C24 S1 C22 C21 71.7(5) . . . . ? C24 S1 C22 C17 -108.8(4) . . . . ? Ti1 O2 C23 C28 -155.8(7) . . . . ? Ti1 O2 C23 C24 24.6(12) . . . . ? O2 C23 C24 C25 178.2(5) . . . . ? C28 C23 C24 C25 -1.4(7) . . . . ? O2 C23 C24 S1 -4.8(7) . . . . ? C28 C23 C24 S1 175.6(4) . . . . ? C22 S1 C24 C25 -118.5(4) . . . . ? C22 S1 C24 C23 64.5(5) . . . . ? C23 C24 C25 C26 0.7(8) . . . . ? S1 C24 C25 C26 -176.4(4) . . . . ? C24 C25 C26 C27 0.5(8) . . . . ? C24 C25 C26 C14 178.7(5) . . . . ? C4 C14 C26 C25 29.7(10) . . . . ? C6 C14 C26 C25 152.9(6) . . . . ? C5 C14 C26 C25 -92.2(9) . . . . ? C4 C14 C26 C27 -152.2(8) . . . . ? C6 C14 C26 C27 -29.0(9) . . . . ? C5 C14 C26 C27 85.9(9) . . . . ? C25 C26 C27 C28 -1.0(8) . . . . ? C14 C26 C27 C28 -179.2(5) . . . . ? O2 C23 C28 C27 -178.6(5) . . . . ? C24 C23 C28 C27 1.0(8) . . . . ? O2 C23 C28 S2 6.3(7) . . . . ? C24 C23 C28 S2 -174.1(4) . . . . ? C26 C27 C28 C23 0.2(8) . . . . ? C26 C27 C28 S2 175.6(4) . . . . ? C30 S2 C28 C23 -58.5(5) . . . . ? C30 S2 C28 C27 126.2(4) . . . . ? C34 C29 C30 C31 0.6(8) . . . . ? O3 C29 C30 C31 179.8(5) . . . . ? C34 C29 C30 S2 -176.7(4) . . . . ? O3 C29 C30 S2 2.5(7) . . . . ? C28 S2 C30 C31 -59.1(5) . . . . ? C28 S2 C30 C29 118.1(4) . . . . ? C29 C30 C31 C32 0.3(8) . . . . ? S2 C30 C31 C32 177.4(4) . . . . ? C30 C31 C32 C33 -0.5(8) . . . . ? C30 C31 C32 C15 -177.5(6) . . . . ? C9 C15 C32 C33 67.7(12) . . . . ? C8 C15 C32 C33 -172.0(8) . . . . ? C7 C15 C32 C33 -54.0(10) . . . . ? C9 C15 C32 C31 -115.4(11) . . . . ? C8 C15 C32 C31 4.9(11) . . . . ? C7 C15 C32 C31 122.9(9) . . . . ? C31 C32 C33 C34 -0.1(8) . . . . ? C15 C32 C33 C34 176.9(6) . . . . ? O3 C29 C34 C33 179.6(5) . . . . ? C30 C29 C34 C33 -1.2(8) . . . . ? O3 C29 C34 S3 -7.0(7) . . . . ? C30 C29 C34 S3 172.1(4) . . . . ? C32 C33 C34 C29 1.0(8) . . . . ? C32 C33 C34 S3 -172.2(4) . . . . ? C36 S3 C34 C29 -121.7(4) . . . . ? C36 S3 C34 C33 51.5(5) . . . . ? Ti1 O4 C35 C40 -40.3(12) . . . . ? Ti1 O4 C35 C36 140.0(8) . . . . ? O4 C35 C36 C37 -179.2(5) . . . . ? C40 C35 C36 C37 1.1(7) . . . . ? O4 C35 C36 S3 -3.5(7) . . . . ? C40 C35 C36 S3 176.8(4) . . . . ? C34 S3 C36 C37 -123.6(4) . . . . ? C34 S3 C36 C35 60.5(5) . . . . ? C35 C36 C37 C38 0.8(8) . . . . ? S3 C36 C37 C38 -175.1(4) . . . . ? C36 C37 C38 C39 -2.7(8) . . . . ? C36 C37 C38 C16 -178.5(5) . . . . ? C11 C16 C38 C37 -169.7(7) . . . . ? C10 C16 C38 C37 -47.7(8) . . . . ? C12 C16 C38 C37 69.8(8) . . . . ? C11 C16 C38 C39 14.7(9) . . . . ? C10 C16 C38 C39 136.7(6) . . . . ? C12 C16 C38 C39 -105.8(7) . . . . ? C37 C38 C39 C40 2.7(8) . . . . ? C16 C38 C39 C40 178.5(5) . . . . ? O4 C35 C40 C39 179.3(5) . . . . ? C36 C35 C40 C39 -1.0(8) . . . . ? O4 C35 C40 S4 5.9(7) . . . . ? C36 C35 C40 S4 -174.4(4) . . . . ? C38 C39 C40 C35 -0.9(8) . . . . ? C38 C39 C40 S4 172.9(4) . . . . ? C18 S4 C40 C35 -57.3(5) . . . . ? C18 S4 C40 C39 129.0(4) . . . . ? O2 Ti1 C41 C45 -92.4(6) . . . . ? O4 Ti1 C41 C45 158.2(5) . . . . ? O1 Ti1 C41 C45 20.3(8) . . . . ? C43 Ti1 C41 C45 77.1(6) . . . . ? C42 Ti1 C41 C45 114.7(8) . . . . ? C44 Ti1 C41 C45 36.8(6) . . . . ? C17 Ti1 C41 C45 -4.5(10) . . . . ? O2 Ti1 C41 C42 152.9(6) . . . . ? O4 Ti1 C41 C42 43.5(6) . . . . ? O1 Ti1 C41 C42 -94.4(7) . . . . ? C43 Ti1 C41 C42 -37.6(5) . . . . ? C44 Ti1 C41 C42 -77.9(6) . . . . ? C45 Ti1 C41 C42 -114.7(8) . . . . ? C17 Ti1 C41 C42 -119.2(8) . . . . ? C45 C41 C42 C43 -0.4(9) . . . . ? Ti1 C41 C42 C43 65.0(6) . . . . ? C45 C41 C42 Ti1 -65.4(6) . . . . ? O2 Ti1 C42 C43 -147.7(6) . . . . ? O4 Ti1 C42 C43 102.7(6) . . . . ? O1 Ti1 C42 C43 -1.3(8) . . . . ? C44 Ti1 C42 C43 -37.2(5) . . . . ? C41 Ti1 C42 C43 -114.5(8) . . . . ? C45 Ti1 C42 C43 -77.9(6) . . . . ? C17 Ti1 C42 C43 18.5(9) . . . . ? O2 Ti1 C42 C41 -33.2(7) . . . . ? O4 Ti1 C42 C41 -142.8(6) . . . . ? O1 Ti1 C42 C41 113.2(6) . . . . ? C43 Ti1 C42 C41 114.5(8) . . . . ? C44 Ti1 C42 C41 77.3(6) . . . . ? C45 Ti1 C42 C41 36.7(5) . . . . ? C17 Ti1 C42 C41 133.0(6) . . . . ? C41 C42 C43 C44 1.1(9) . . . . ? Ti1 C42 C43 C44 66.8(6) . . . . ? C41 C42 C43 Ti1 -65.7(5) . . . . ? O2 Ti1 C43 C44 -55.3(10) . . . . ? O4 Ti1 C43 C44 165.1(6) . . . . ? O1 Ti1 C43 C44 64.3(6) . . . . ? C42 Ti1 C43 C44 -114.6(8) . . . . ? C41 Ti1 C43 C44 -76.1(6) . . . . ? C45 Ti1 C43 C44 -36.2(5) . . . . ? C17 Ti1 C43 C44 75.8(6) . . . . ? O2 Ti1 C43 C42 59.3(10) . . . . ? O4 Ti1 C43 C42 -80.2(6) . . . . ? O1 Ti1 C43 C42 178.9(6) . . . . ? C44 Ti1 C43 C42 114.6(8) . . . . ? C41 Ti1 C43 C42 38.5(5) . . . . ? C45 Ti1 C43 C42 78.4(6) . . . . ? C17 Ti1 C43 C42 -169.6(6) . . . . ? C42 C43 C44 C45 -1.3(10) . . . . ? Ti1 C43 C44 C45 64.8(6) . . . . ? C42 C43 C44 Ti1 -66.2(6) . . . . ? O2 Ti1 C44 C43 149.4(6) . . . . ? O4 Ti1 C44 C43 -19.5(7) . . . . ? O1 Ti1 C44 C43 -111.9(7) . . . . ? C42 Ti1 C44 C43 38.2(6) . . . . ? C41 Ti1 C44 C43 81.0(6) . . . . ? C45 Ti1 C44 C43 117.4(8) . . . . ? C17 Ti1 C44 C43 -115.9(6) . . . . ? O2 Ti1 C44 C45 32.1(7) . . . . ? O4 Ti1 C44 C45 -136.8(6) . . . . ? O1 Ti1 C44 C45 130.8(6) . . . . ? C43 Ti1 C44 C45 -117.4(8) . . . . ? C42 Ti1 C44 C45 -79.1(6) . . . . ? C41 Ti1 C44 C45 -36.4(5) . . . . ? C17 Ti1 C44 C45 126.7(6) . . . . ? C42 C41 C45 C44 -0.4(9) . . . . ? Ti1 C41 C45 C44 -64.5(6) . . . . ? C42 C41 C45 Ti1 64.1(5) . . . . ? C43 C44 C45 C41 1.1(10) . . . . ? Ti1 C44 C45 C41 65.0(6) . . . . ? C43 C44 C45 Ti1 -63.9(6) . . . . ? O2 Ti1 C45 C41 89.8(6) . . . . ? O4 Ti1 C45 C41 -37.8(9) . . . . ? O1 Ti1 C45 C41 -164.5(6) . . . . ? C43 Ti1 C45 C41 -80.4(6) . . . . ? C42 Ti1 C45 C41 -38.9(6) . . . . ? C44 Ti1 C45 C41 -116.5(9) . . . . ? C17 Ti1 C45 C41 177.7(5) . . . . ? O2 Ti1 C45 C44 -153.7(6) . . . . ? O4 Ti1 C45 C44 78.6(8) . . . . ? O1 Ti1 C45 C44 -48.1(6) . . . . ? C43 Ti1 C45 C44 36.0(6) . . . . ? C42 Ti1 C45 C44 77.6(6) . . . . ? C41 Ti1 C45 C44 116.5(9) . . . . ? C17 Ti1 C45 C44 -65.8(6) . . . . ? Ti2 O5 C65 C70 -91.1(5) . . . . ? Ti2 O5 C65 C66 90.9(5) . . . . ? O6 Ti2 C65 O5 125.5(3) . . . . ? O8 Ti2 C65 O5 -128.4(3) . . . . ? C90 Ti2 C65 O5 41.7(7) . . . . ? C91 Ti2 C65 O5 -47.7(6) . . . . ? C92 Ti2 C65 O5 -33.0(4) . . . . ? C89 Ti2 C65 O5 34.6(4) . . . . ? C93 Ti2 C65 O5 1.4(4) . . . . ? O6 Ti2 C65 C70 -124.6(4) . . . . ? O8 Ti2 C65 C70 -18.5(4) . . . . ? O5 Ti2 C65 C70 109.9(5) . . . . ? C90 Ti2 C65 C70 151.6(6) . . . . ? C91 Ti2 C65 C70 62.2(7) . . . . ? C92 Ti2 C65 C70 76.9(5) . . . . ? C89 Ti2 C65 C70 144.5(4) . . . . ? C93 Ti2 C65 C70 111.2(4) . . . . ? O6 Ti2 C65 C66 15.1(4) . . . . ? O8 Ti2 C65 C66 121.2(4) . . . . ? O5 Ti2 C65 C66 -110.4(5) . . . . ? C90 Ti2 C65 C66 -68.7(7) . . . . ? C91 Ti2 C65 C66 -158.2(5) . . . . ? C92 Ti2 C65 C66 -143.4(4) . . . . ? C89 Ti2 C65 C66 -75.9(5) . . . . ? C93 Ti2 C65 C66 -109.1(4) . . . . ? O5 C65 C66 C67 177.3(4) . . . . ? C70 C65 C66 C67 -0.7(7) . . . . ? Ti2 C65 C66 C67 -137.9(4) . . . . ? O5 C65 C66 S5 5.4(6) . . . . ? C70 C65 C66 S5 -172.6(4) . . . . ? Ti2 C65 C66 S5 50.2(5) . . . . ? C72 S5 C66 C65 -100.8(4) . . . . ? C72 S5 C66 C67 87.2(5) . . . . ? C65 C66 C67 C68 -0.4(8) . . . . ? S5 C66 C67 C68 171.4(4) . . . . ? C66 C67 C68 C69 1.3(8) . . . . ? C66 C67 C68 C61 -174.6(5) . . . . ? C47 C61 C68 C69 -83.0(9) . . . . ? C46 C61 C68 C69 156.7(8) . . . . ? C48 C61 C68 C69 38.0(9) . . . . ? C47 C61 C68 C67 92.7(9) . . . . ? C46 C61 C68 C67 -27.5(10) . . . . ? C48 C61 C68 C67 -146.2(7) . . . . ? C67 C68 C69 C70 -1.2(8) . . . . ? C61 C68 C69 C70 174.7(5) . . . . ? O5 C65 C70 C69 -177.2(4) . . . . ? C66 C65 C70 C69 0.8(7) . . . . ? Ti2 C65 C70 C69 138.1(4) . . . . ? O5 C65 C70 S8 -3.1(7) . . . . ? C66 C65 C70 S8 174.9(4) . . . . ? Ti2 C65 C70 S8 -47.8(5) . . . . ? C68 C69 C70 C65 0.2(8) . . . . ? C68 C69 C70 S8 -173.7(4) . . . . ? C88 S8 C70 C65 102.5(5) . . . . ? C88 S8 C70 C69 -83.5(5) . . . . ? Ti2 O6 C71 C76 -130.7(8) . . . . ? Ti2 O6 C71 C72 50.9(11) . . . . ? O6 C71 C72 C73 179.6(5) . . . . ? C76 C71 C72 C73 1.2(8) . . . . ? O6 C71 C72 S5 -7.5(7) . . . . ? C76 C71 C72 S5 174.0(4) . . . . ? C66 S5 C72 C73 -129.6(5) . . . . ? C66 S5 C72 C71 57.3(5) . . . . ? C71 C72 C73 C74 0.5(9) . . . . ? S5 C72 C73 C74 -173.0(5) . . . . ? C72 C73 C74 C75 -2.0(9) . . . . ? C72 C73 C74 C64 179.5(6) . . . . ? C58 C64 C74 C75 108.0(13) . . . . ? C60 C64 C74 C75 -19.7(17) . . . . ? C59 C64 C74 C75 -135.3(11) . . . . ? C58 C64 C74 C73 -73.5(14) . . . . ? C60 C64 C74 C73 158.8(15) . . . . ? C59 C64 C74 C73 43.2(13) . . . . ? C73 C74 C75 C76 1.9(9) . . . . ? C64 C74 C75 C76 -179.6(6) . . . . ? O6 C71 C76 C75 -179.7(5) . . . . ? C72 C71 C76 C75 -1.2(8) . . . . ? O6 C71 C76 S6 3.7(7) . . . . ? C72 C71 C76 S6 -177.8(4) . . . . ? C74 C75 C76 C71 -0.3(8) . . . . ? C74 C75 C76 S6 176.4(4) . . . . ? C78 S6 C76 C71 -54.6(5) . . . . ? C78 S6 C76 C75 128.7(4) . . . . ? O7 C77 C78 C79 -179.7(5) . . . . ? C82 C77 C78 C79 3.3(7) . . . . ? O7 C77 C78 S6 6.7(7) . . . . ? C82 C77 C78 S6 -170.3(4) . . . . ? C76 S6 C78 C79 -41.4(4) . . . . ? C76 S6 C78 C77 132.1(4) . . . . ? C77 C78 C79 C80 -2.4(7) . . . . ? S6 C78 C79 C80 171.0(4) . . . . ? C78 C79 C80 C81 0.8(7) . . . . ? C78 C79 C80 C62 -176.9(5) . . . . ? C54 C62 C80 C79 27.3(9) . . . . ? C53 C62 C80 C79 -94.7(8) . . . . ? C52 C62 C80 C79 147.4(7) . . . . ? C54 C62 C80 C81 -150.3(8) . . . . ? C53 C62 C80 C81 87.6(9) . . . . ? C52 C62 C80 C81 -30.2(8) . . . . ? C79 C80 C81 C82 -0.1(7) . . . . ? C62 C80 C81 C82 177.6(5) . . . . ? C80 C81 C82 C77 1.1(8) . . . . ? C80 C81 C82 S7 -171.5(4) . . . . ? O7 C77 C82 C81 -179.5(5) . . . . ? C78 C77 C82 C81 -2.7(7) . . . . ? O7 C77 C82 S7 -6.7(7) . . . . ? C78 C77 C82 S7 170.2(4) . . . . ? C84 S7 C82 C81 47.3(5) . . . . ? C84 S7 C82 C77 -125.4(4) . . . . ? Ti2 O8 C83 C84 137.6(7) . . . . ? Ti2 O8 C83 C88 -43.5(11) . . . . ? O8 C83 C84 C85 -179.3(5) . . . . ? C88 C83 C84 C85 1.8(8) . . . . ? O8 C83 C84 S7 -2.3(7) . . . . ? C88 C83 C84 S7 178.8(4) . . . . ? C82 S7 C84 C85 -132.7(4) . . . . ? C82 S7 C84 C83 50.2(5) . . . . ? C83 C84 C85 C86 -0.3(9) . . . . ? S7 C84 C85 C86 -177.5(5) . . . . ? C84 C85 C86 C87 -1.3(9) . . . . ? C84 C85 C86 C63 -179.9(6) . . . . ? C51 C63 C86 C87 122.4(9) . . . . ? C50 C63 C86 C87 -112.5(9) . . . . ? C49 C63 C86 C87 2.7(10) . . . . ? C51 C63 C86 C85 -59.0(10) . . . . ? C50 C63 C86 C85 66.1(9) . . . . ? C49 C63 C86 C85 -178.7(7) . . . . ? C85 C86 C87 C88 1.4(9) . . . . ? C63 C86 C87 C88 -180.0(6) . . . . ? C86 C87 C88 C83 0.0(9) . . . . ? C86 C87 C88 S8 174.1(5) . . . . ? O8 C83 C88 C87 179.4(5) . . . . ? C84 C83 C88 C87 -1.6(8) . . . . ? O8 C83 C88 S8 5.7(7) . . . . ? C84 C83 C88 S8 -175.3(4) . . . . ? C70 S8 C88 C87 127.3(5) . . . . ? C70 S8 C88 C83 -58.8(5) . . . . ? O6 Ti2 C89 C93 -155.3(5) . . . . ? O8 Ti2 C89 C93 77.5(6) . . . . ? O5 Ti2 C89 C93 -53.6(5) . . . . ? C90 Ti2 C89 C93 115.6(7) . . . . ? C91 Ti2 C89 C93 77.8(5) . . . . ? C92 Ti2 C89 C93 36.8(4) . . . . ? C65 Ti2 C89 C93 -69.2(5) . . . . ? O6 Ti2 C89 C90 89.0(5) . . . . ? O8 Ti2 C89 C90 -38.1(7) . . . . ? O5 Ti2 C89 C90 -169.2(5) . . . . ? C91 Ti2 C89 C90 -37.9(4) . . . . ? C92 Ti2 C89 C90 -78.9(5) . . . . ? C93 Ti2 C89 C90 -115.6(7) . . . . ? C65 Ti2 C89 C90 175.1(4) . . . . ? C93 C89 C90 C91 0.3(8) . . . . ? Ti2 C89 C90 C91 65.2(5) . . . . ? C93 C89 C90 Ti2 -64.9(5) . . . . ? O6 Ti2 C90 C89 -92.8(5) . . . . ? O8 Ti2 C90 C89 158.3(4) . . . . ? O5 Ti2 C90 C89 14.6(6) . . . . ? C91 Ti2 C90 C89 115.3(7) . . . . ? C92 Ti2 C90 C89 77.8(5) . . . . ? C93 Ti2 C90 C89 37.1(4) . . . . ? C65 Ti2 C90 C89 -10.6(9) . . . . ? O6 Ti2 C90 C91 151.8(4) . . . . ? O8 Ti2 C90 C91 43.0(5) . . . . ? O5 Ti2 C90 C91 -100.7(5) . . . . ? C92 Ti2 C90 C91 -37.5(4) . . . . ? C89 Ti2 C90 C91 -115.3(7) . . . . ? C93 Ti2 C90 C91 -78.3(5) . . . . ? C65 Ti2 C90 C91 -125.9(6) . . . . ? C89 C90 C91 C92 -0.1(8) . . . . ? Ti2 C90 C91 C92 66.0(5) . . . . ? C89 C90 C91 Ti2 -66.1(5) . . . . ? O6 Ti2 C91 C92 -148.8(4) . . . . ? O8 Ti2 C91 C92 102.7(5) . . . . ? O5 Ti2 C91 C92 -3.5(6) . . . . ? C90 Ti2 C91 C92 -114.7(7) . . . . ? C89 Ti2 C91 C92 -77.2(5) . . . . ? C93 Ti2 C91 C92 -36.4(5) . . . . ? C65 Ti2 C91 C92 23.2(8) . . . . ? O6 Ti2 C91 C90 -34.1(5) . . . . ? O8 Ti2 C91 C90 -142.7(4) . . . . ? O5 Ti2 C91 C90 111.1(5) . . . . ? C92 Ti2 C91 C90 114.7(7) . . . . ? C89 Ti2 C91 C90 37.5(4) . . . . ? C93 Ti2 C91 C90 78.3(5) . . . . ? C65 Ti2 C91 C90 137.8(5) . . . . ? C90 C91 C92 C93 -0.1(8) . . . . ? Ti2 C91 C92 C93 64.9(5) . . . . ? C90 C91 C92 Ti2 -65.0(5) . . . . ? O6 Ti2 C92 C93 -60.5(7) . . . . ? O8 Ti2 C92 C93 163.5(5) . . . . ? O5 Ti2 C92 C93 60.3(5) . . . . ? C90 Ti2 C92 C93 -78.6(5) . . . . ? C91 Ti2 C92 C93 -117.0(7) . . . . ? C89 Ti2 C92 C93 -36.9(5) . . . . ? C65 Ti2 C92 C93 75.2(5) . . . . ? O6 Ti2 C92 C91 56.5(7) . . . . ? O8 Ti2 C92 C91 -79.5(5) . . . . ? O5 Ti2 C92 C91 177.3(5) . . . . ? C90 Ti2 C92 C91 38.4(5) . . . . ? C89 Ti2 C92 C91 80.1(5) . . . . ? C93 Ti2 C92 C91 117.0(7) . . . . ? C65 Ti2 C92 C91 -167.9(4) . . . . ? C91 C92 C93 C89 0.2(8) . . . . ? Ti2 C92 C93 C89 63.9(5) . . . . ? C91 C92 C93 Ti2 -63.7(5) . . . . ? C90 C89 C93 C92 -0.3(8) . . . . ? Ti2 C89 C93 C92 -63.8(5) . . . . ? C90 C89 C93 Ti2 63.4(5) . . . . ? O6 Ti2 C93 C92 146.7(4) . . . . ? O8 Ti2 C93 C92 -21.4(6) . . . . ? O5 Ti2 C93 C92 -117.9(5) . . . . ? C90 Ti2 C93 C92 78.7(5) . . . . ? C91 Ti2 C93 C92 36.7(5) . . . . ? C89 Ti2 C93 C92 116.4(7) . . . . ? C65 Ti2 C93 C92 -118.6(5) . . . . ? O6 Ti2 C93 C89 30.2(5) . . . . ? O8 Ti2 C93 C89 -137.8(4) . . . . ? O5 Ti2 C93 C89 125.7(5) . . . . ? C90 Ti2 C93 C89 -37.7(5) . . . . ? C91 Ti2 C93 C89 -79.7(5) . . . . ? C92 Ti2 C93 C89 -116.4(7) . . . . ? C65 Ti2 C93 C89 125.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.985 _refine_diff_density_min -0.930 _refine_diff_density_rms 0.097 #===END data_[TC4A-(O)4Ti(mu2-eta5:eta1-C5H5)MoH(PMe2Ph)2](4) _database_code_depnum_ccdc_archive 'CCDC 228240' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H75 Mo O4 P2 S4 Ti' _chemical_formula_weight 1242.33 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' Mo Mo -1.6832 0.6857 '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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P bca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 23.430(10) _cell_length_b 23.594(11) _cell_length_c 22.051(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12190(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5192 _exptl_absorpt_coefficient_mu 0.572 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8945 _exptl_absorpt_correction_T_max 0.9721 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 70858 _diffrn_reflns_av_R_equivalents 0.2589 _diffrn_reflns_av_sigmaI/netI 0.1572 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 4.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10290 _reflns_number_gt 6753 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. The crystal contains 0.5 equiv of solvated benzene molecule per molecule of the complex. The carbon atoms of this solvent molecule were refined with isotropic thermal parameters. All hydrogen atoms except for H1, H2, and those on the solvated benzene molecule were located at calculated position and were treated as riding models. The H1 and H2 atoms were found in the difference Fourier map and its positions were refined. Hydrogen atoms on the benzene carbon atoms were not included in the calculation. ; _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^)+(0.0267P)^2^+195.0306P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10290 _refine_ls_number_parameters 676 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2346 _refine_ls_R_factor_gt 0.1726 _refine_ls_wR_factor_ref 0.2878 _refine_ls_wR_factor_gt 0.2641 _refine_ls_goodness_of_fit_ref 1.280 _refine_ls_restrained_S_all 1.280 _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 Mo1 Mo 0.07072(5) 0.65800(5) 0.95375(5) 0.0301(3) Uani 1 1 d . . . Ti1 Ti 0.12404(11) 0.68201(11) 1.06077(10) 0.0306(6) Uani 1 1 d . . . S1 S 0.12930(16) 0.70495(17) 0.88179(15) 0.0339(9) Uani 1 1 d . . . S2 S 0.08081(16) 0.85419(16) 1.05380(16) 0.0383(10) Uani 1 1 d . . . S3 S 0.2076(2) 0.71971(18) 1.20521(17) 0.0478(12) Uani 1 1 d . . . S4 S 0.27613(19) 0.58376(17) 1.02548(17) 0.0431(10) Uani 1 1 d . . . P1 P -0.02281(18) 0.70937(17) 0.92919(17) 0.0367(10) Uani 1 1 d . . . P2 P 0.08340(18) 0.56834(17) 0.90390(17) 0.0363(10) Uani 1 1 d . . . O1 O 0.0981(4) 0.7353(4) 0.9969(4) 0.030(2) Uani 1 1 d . . . O2 O 0.1126(4) 0.7465(4) 1.1128(4) 0.035(2) Uani 1 1 d . . . O3 O 0.2071(4) 0.6806(4) 1.0807(4) 0.035(2) Uani 1 1 d . . . O4 O 0.1581(4) 0.6419(4) 0.9847(4) 0.029(2) Uani 1 1 d . . . C1 C -0.0249(7) 0.7856(6) 0.9422(7) 0.051(4) Uani 1 1 d . . . H1A H -0.0279 0.8049 0.9041 0.076 Uiso 1 1 calc R . . H1B H 0.0094 0.7972 0.9625 0.076 Uiso 1 1 calc R . . H1C H -0.0573 0.7947 0.9670 0.076 Uiso 1 1 calc R . . C2 C -0.0396(8) 0.7079(7) 0.8523(6) 0.053(5) Uani 1 1 d . . . H2A H -0.0527 0.7446 0.8399 0.079 Uiso 1 1 calc R . . H2B H -0.0691 0.6804 0.8453 0.079 Uiso 1 1 calc R . . H2C H -0.0063 0.6978 0.8294 0.079 Uiso 1 1 calc R . . C3 C 0.0417(9) 0.5071(7) 0.9308(8) 0.068(6) Uani 1 1 d . . . H3A H 0.0029 0.5185 0.9375 0.103 Uiso 1 1 calc R . . H3B H 0.0577 0.4934 0.9681 0.103 Uiso 1 1 calc R . . H3C H 0.0428 0.4776 0.9009 0.103 Uiso 1 1 calc R . . C4 C 0.1609(7) 0.5388(7) 0.9000(7) 0.051(5) Uani 1 1 d . . . H4A H 0.1608 0.5034 0.8786 0.076 Uiso 1 1 calc R . . H4B H 0.1751 0.5330 0.9404 0.076 Uiso 1 1 calc R . . H4C H 0.1849 0.5654 0.8792 0.076 Uiso 1 1 calc R . . C5 C 0.2323(10) 0.9124(10) 0.8356(11) 0.107(9) Uani 1 1 d . . . H5A H 0.2460 0.9434 0.8114 0.161 Uiso 1 1 calc R . . H5B H 0.2340 0.8780 0.8123 0.161 Uiso 1 1 calc R . . H5C H 0.2557 0.9085 0.8710 0.161 Uiso 1 1 calc R . . C6 C 0.1268(13) 0.9289(12) 0.8044(12) 0.158(15) Uani 1 1 d . . . H6A H 0.1371 0.9605 0.7791 0.237 Uiso 1 1 calc R . . H6B H 0.0890 0.9346 0.8201 0.237 Uiso 1 1 calc R . . H6C H 0.1276 0.8947 0.7809 0.237 Uiso 1 1 calc R . . C7 C 0.1715(15) 0.9801(9) 0.8861(11) 0.167(16) Uani 1 1 d . . . H7A H 0.1836 1.0083 0.8575 0.251 Uiso 1 1 calc R . . H7B H 0.1985 0.9780 0.9187 0.251 Uiso 1 1 calc R . . H7C H 0.1347 0.9901 0.9019 0.251 Uiso 1 1 calc R . . C8 C 0.2555(15) 0.9809(10) 1.1375(19) 0.26(3) Uani 1 1 d . . . H8A H 0.2600 0.9764 1.0945 0.393 Uiso 1 1 calc R . . H8B H 0.2797 1.0110 1.1514 0.393 Uiso 1 1 calc R . . H8C H 0.2165 0.9900 1.1464 0.393 Uiso 1 1 calc R . . C9 C 0.2615(16) 0.9433(14) 1.2320(11) 0.186(17) Uani 1 1 d . . . H9A H 0.2703 0.9106 1.2561 0.280 Uiso 1 1 calc R . . H9B H 0.2223 0.9538 1.2383 0.280 Uiso 1 1 calc R . . H9C H 0.2858 0.9742 1.2436 0.280 Uiso 1 1 calc R . . C10 C 0.3329(11) 0.9144(10) 1.1643(12) 0.119(10) Uani 1 1 d . . . H10A H 0.3394 0.8805 1.1873 0.179 Uiso 1 1 calc R . . H10B H 0.3553 0.9448 1.1809 0.179 Uiso 1 1 calc R . . H10C H 0.3438 0.9082 1.1228 0.179 Uiso 1 1 calc R . . C11 C 0.4507(8) 0.6493(9) 1.2222(8) 0.071(6) Uani 1 1 d . . . H11A H 0.4640 0.6642 1.1842 0.107 Uiso 1 1 calc R . . H11B H 0.4825 0.6357 1.2454 0.107 Uiso 1 1 calc R . . H11C H 0.4316 0.6788 1.2444 0.107 Uiso 1 1 calc R . . C12 C 0.3886(10) 0.5757(12) 1.2680(9) 0.125(11) Uani 1 1 d . . . H12A H 0.3652 0.6027 1.2889 0.187 Uiso 1 1 calc R . . H12B H 0.4206 0.5658 1.2930 0.187 Uiso 1 1 calc R . . H12C H 0.3666 0.5423 1.2595 0.187 Uiso 1 1 calc R . . C13 C 0.4456(11) 0.5551(13) 1.1806(11) 0.147(14) Uani 1 1 d . . . H13A H 0.4599 0.5689 1.1426 0.221 Uiso 1 1 calc R . . H13B H 0.4229 0.5218 1.1738 0.221 Uiso 1 1 calc R . . H13C H 0.4771 0.5458 1.2067 0.221 Uiso 1 1 calc R . . C14 C 0.3654(10) 0.6960(11) 0.7981(7) 0.108(10) Uani 1 1 d . . . H14A H 0.3280 0.7063 0.7843 0.162 Uiso 1 1 calc R . . H14B H 0.3714 0.6563 0.7915 0.162 Uiso 1 1 calc R . . H14C H 0.3935 0.7173 0.7760 0.162 Uiso 1 1 calc R . . C15 C 0.3664(11) 0.7740(10) 0.8612(10) 0.114(10) Uani 1 1 d . . . H15A H 0.3702 0.7870 0.9023 0.171 Uiso 1 1 calc R . . H15B H 0.3302 0.7858 0.8453 0.171 Uiso 1 1 calc R . . H15C H 0.3965 0.7898 0.8370 0.171 Uiso 1 1 calc R . . C16 C 0.4260(8) 0.6942(11) 0.8892(8) 0.097(9) Uani 1 1 d . . . H16A H 0.4241 0.7032 0.9316 0.145 Uiso 1 1 calc R . . H16B H 0.4558 0.7160 0.8705 0.145 Uiso 1 1 calc R . . H16C H 0.4340 0.6545 0.8843 0.145 Uiso 1 1 calc R . . C17 C 0.1679(8) 0.9243(7) 0.8554(7) 0.049(4) Uani 1 1 d . . . C18 C 0.2706(8) 0.9300(9) 1.1671(9) 0.063(5) Uani 1 1 d . . . C19 C 0.4092(8) 0.6006(8) 1.2104(8) 0.055(5) Uani 1 1 d . . . C20 C 0.3703(7) 0.7079(10) 0.8598(7) 0.060(6) Uani 1 1 d . . . C21 C 0.0519(6) 0.6180(7) 1.0480(8) 0.043(4) Uani 1 1 d . . . C22 C 0.0296(8) 0.6531(8) 1.0910(7) 0.052(5) Uani 1 1 d . . . H22 H -0.0013 0.6776 1.0870 0.062 Uiso 1 1 calc R . . C23 C 0.0615(9) 0.6448(7) 1.1400(7) 0.061(6) Uani 1 1 d . . . H23 H 0.0558 0.6630 1.1769 0.073 Uiso 1 1 calc R . . C24 C 0.1067(8) 0.6032(8) 1.1284(7) 0.057(5) Uani 1 1 d . . . H24 H 0.1346 0.5907 1.1553 0.068 Uiso 1 1 calc R . . C25 C 0.0993(7) 0.5874(7) 1.0721(6) 0.041(4) Uani 1 1 d . . . H25 H 0.1212 0.5609 1.0513 0.049 Uiso 1 1 calc R . . C26 C -0.0953(6) 0.6876(7) 0.9585(7) 0.044(4) Uani 1 1 d . . . C27 C -0.1477(7) 0.7202(7) 0.9503(8) 0.054(5) Uani 1 1 d . . . H27 H -0.1441 0.7538 0.9285 0.065 Uiso 1 1 calc R . . C28 C -0.2060(8) 0.7066(8) 0.9723(9) 0.062(5) Uani 1 1 d . . . H28 H -0.2376 0.7295 0.9649 0.074 Uiso 1 1 calc R . . C29 C -0.2085(8) 0.6589(11) 1.0035(9) 0.078(6) Uani 1 1 d . . . H29 H -0.2436 0.6469 1.0185 0.093 Uiso 1 1 calc R . . C30 C -0.1577(8) 0.6242(9) 1.0151(9) 0.071(6) Uani 1 1 d . . . H30 H -0.1609 0.5917 1.0388 0.085 Uiso 1 1 calc R . . C31 C -0.1042(7) 0.6390(8) 0.9912(7) 0.052(5) Uani 1 1 d . . . H31 H -0.0735 0.6148 0.9978 0.063 Uiso 1 1 calc R . . C32 C 0.0609(7) 0.5728(7) 0.8298(6) 0.040(4) Uani 1 1 d . . . C33 C 0.1012(10) 0.5977(8) 0.7900(7) 0.071(6) Uani 1 1 d . . . H33 H 0.1380 0.6071 0.8023 0.085 Uiso 1 1 calc R . . C34 C 0.0828(13) 0.6066(11) 0.7348(8) 0.097(9) Uani 1 1 d . . . H34 H 0.1074 0.6230 0.7067 0.116 Uiso 1 1 calc R . . C35 C 0.0287(14) 0.5927(12) 0.7170(9) 0.108(10) Uani 1 1 d . . . H35 H 0.0180 0.6004 0.6773 0.130 Uiso 1 1 calc R . . C36 C -0.0112(11) 0.5675(9) 0.7555(10) 0.084(7) Uani 1 1 d . . . H36 H -0.0474 0.5580 0.7416 0.101 Uiso 1 1 calc R . . C37 C 0.0039(8) 0.5574(8) 0.8125(7) 0.057(5) Uani 1 1 d . . . H37 H -0.0213 0.5411 0.8400 0.068 Uiso 1 1 calc R . . C38 C 0.1145(6) 0.7820(6) 0.9666(6) 0.034(4) Uani 1 1 d . . . C39 C 0.1122(6) 0.8373(6) 0.9859(5) 0.025(3) Uani 1 1 d . . . C40 C 0.1294(6) 0.8826(6) 0.9505(7) 0.039(4) Uani 1 1 d . . . H40 H 0.1273 0.9191 0.9663 0.046 Uiso 1 1 calc R . . C41 C 0.1491(7) 0.8749(7) 0.8935(6) 0.038(4) Uani 1 1 d . . . C42 C 0.1467(6) 0.8207(6) 0.8745(6) 0.033(4) Uani 1 1 d . . . H42 H 0.1567 0.8134 0.8344 0.040 Uiso 1 1 calc R . . C43 C 0.1308(6) 0.7763(6) 0.9091(6) 0.028(3) Uani 1 1 d . . . C44 C 0.1519(7) 0.7866(7) 1.1245(6) 0.037(4) Uani 1 1 d . . . C45 C 0.1998(7) 0.7833(6) 1.1647(6) 0.033(4) Uani 1 1 d . . . C46 C 0.2357(6) 0.8287(6) 1.1764(6) 0.039(4) Uani 1 1 d . . . H46 H 0.2653 0.8230 1.2039 0.047 Uiso 1 1 calc R . . C47 C 0.2309(7) 0.8812(7) 1.1507(7) 0.045(4) Uani 1 1 d . . . C48 C 0.1830(6) 0.8874(6) 1.1122(6) 0.037(4) Uani 1 1 d . . . H48 H 0.1765 0.9225 1.0941 0.044 Uiso 1 1 calc R . . C49 C 0.1441(7) 0.8419(7) 1.0999(6) 0.039(4) Uani 1 1 d . . . C50 C 0.2532(6) 0.6601(6) 1.1116(6) 0.033(3) Uani 1 1 d . . . C51 C 0.2949(8) 0.6201(7) 1.0904(6) 0.045(4) Uani 1 1 d . . . C52 C 0.3433(7) 0.6033(7) 1.1224(6) 0.040(4) Uani 1 1 d . . . H52 H 0.3690 0.5785 1.1043 0.048 Uiso 1 1 calc R . . C53 C 0.3533(7) 0.6220(7) 1.1782(7) 0.047(4) Uani 1 1 d . . . C54 C 0.3119(7) 0.6606(7) 1.1982(6) 0.044(4) Uani 1 1 d . . . H54 H 0.3174 0.6757 1.2368 0.053 Uiso 1 1 calc R . . C55 C 0.2634(6) 0.6792(6) 1.1674(6) 0.038(4) Uani 1 1 d . . . C56 C 0.2096(5) 0.6545(6) 0.9545(7) 0.033(3) Uani 1 1 d . . . C57 C 0.2050(6) 0.6865(6) 0.9035(6) 0.033(4) Uani 1 1 d . . . C58 C 0.2546(6) 0.7017(6) 0.8739(6) 0.036(4) Uani 1 1 d . . . H58 H 0.2502 0.7231 0.8388 0.043 Uiso 1 1 calc R . . C59 C 0.3114(8) 0.6888(7) 0.8907(6) 0.045(4) Uani 1 1 d . . . C60 C 0.3177(7) 0.6543(7) 0.9404(6) 0.047(4) Uani 1 1 d . . . H60 H 0.3537 0.6431 0.9534 0.056 Uiso 1 1 calc R . . C61 C 0.2669(7) 0.6360(7) 0.9720(6) 0.041(4) Uani 1 1 d . . . C62 C -0.003(3) 0.498(2) 0.5547(19) 0.181(15) Uiso 1 1 d . . . C63 C -0.039(3) 0.532(3) 0.532(4) 0.25(2) Uiso 1 1 d . . . C64 C 0.033(2) 0.467(2) 0.524(3) 0.207(19) Uiso 1 1 d . . . H1 H 0.011(5) 0.619(4) 0.926(5) 0.016 Uiso 1 1 d . . . H2 H 0.034(5) 0.600(5) 1.016(5) 0.016 Uiso 1 1 d . . . 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 Mo1 0.0311(7) 0.0317(6) 0.0274(6) 0.0013(6) 0.0012(6) -0.0017(6) Ti1 0.0350(16) 0.0340(14) 0.0228(13) 0.0022(11) 0.0023(12) 0.0018(12) S1 0.033(2) 0.043(2) 0.0255(18) 0.0011(17) -0.0018(17) 0.0014(18) S2 0.036(2) 0.045(2) 0.034(2) -0.0019(18) -0.0047(18) 0.0107(18) S3 0.072(3) 0.046(3) 0.026(2) 0.0031(18) -0.001(2) 0.015(2) S4 0.058(3) 0.034(2) 0.037(2) 0.0007(18) -0.003(2) 0.009(2) P1 0.041(3) 0.037(2) 0.032(2) 0.0022(18) -0.0020(19) -0.005(2) P2 0.041(3) 0.036(2) 0.032(2) 0.0019(18) 0.0014(19) 0.0028(19) O1 0.046(6) 0.024(5) 0.021(5) 0.007(4) -0.006(5) -0.012(5) O2 0.053(7) 0.029(5) 0.023(5) 0.001(4) -0.002(5) 0.002(5) O3 0.030(6) 0.045(6) 0.030(5) -0.001(5) -0.001(4) 0.011(5) O4 0.038(6) 0.029(6) 0.021(5) 0.003(4) -0.014(4) -0.005(4) C1 0.059(11) 0.038(9) 0.055(10) 0.011(8) 0.006(9) 0.014(8) C2 0.077(14) 0.047(10) 0.035(9) 0.013(8) -0.004(9) 0.007(10) C3 0.114(18) 0.035(10) 0.056(11) -0.001(9) 0.024(11) -0.020(11) C4 0.052(12) 0.050(11) 0.051(10) 0.000(9) -0.010(9) 0.006(9) C5 0.09(2) 0.11(2) 0.12(2) 0.051(16) 0.051(16) 0.022(16) C6 0.18(3) 0.14(3) 0.15(3) 0.11(2) -0.09(2) -0.09(2) C7 0.34(5) 0.068(17) 0.095(18) -0.017(14) 0.10(2) -0.10(2) C8 0.27(4) 0.064(18) 0.45(6) 0.13(3) -0.31(4) -0.09(2) C9 0.27(5) 0.21(4) 0.082(19) -0.06(2) 0.00(3) -0.07(3) C10 0.11(2) 0.086(19) 0.16(3) -0.044(18) 0.00(2) -0.029(17) C11 0.059(13) 0.089(16) 0.066(12) 0.002(12) -0.031(10) -0.006(12) C12 0.088(18) 0.20(3) 0.087(17) 0.086(19) -0.013(14) 0.065(19) C13 0.11(2) 0.23(3) 0.098(19) -0.02(2) -0.035(16) 0.14(2) C14 0.105(19) 0.18(3) 0.037(11) -0.012(14) 0.020(12) -0.079(19) C15 0.14(2) 0.10(2) 0.107(19) 0.021(15) 0.076(18) -0.044(17) C16 0.031(11) 0.19(3) 0.068(13) 0.058(15) 0.003(10) -0.008(15) C17 0.062(12) 0.030(9) 0.054(10) 0.002(8) 0.002(9) 0.003(9) C18 0.034(11) 0.070(14) 0.086(15) -0.003(11) -0.015(10) 0.007(10) C19 0.049(12) 0.064(12) 0.052(11) 0.009(10) -0.003(9) 0.016(10) C20 0.030(10) 0.117(17) 0.033(9) -0.001(10) 0.004(8) -0.022(11) C21 0.030(9) 0.057(11) 0.043(9) -0.029(9) -0.005(8) -0.015(8) C22 0.059(12) 0.069(12) 0.028(8) 0.004(9) 0.018(8) -0.017(10) C23 0.094(16) 0.050(12) 0.037(9) 0.003(8) 0.014(10) -0.022(11) C24 0.059(13) 0.073(13) 0.039(10) 0.020(9) 0.003(9) 0.007(11) C25 0.037(10) 0.062(11) 0.024(8) 0.004(8) 0.011(7) 0.007(8) C26 0.032(9) 0.058(10) 0.041(9) -0.015(9) -0.008(8) -0.009(8) C27 0.038(10) 0.055(11) 0.069(12) -0.001(10) -0.005(10) 0.008(8) C28 0.041(11) 0.065(13) 0.078(14) 0.011(11) 0.012(10) -0.005(10) C29 0.033(11) 0.14(2) 0.064(13) -0.002(14) 0.001(9) -0.005(13) C30 0.051(13) 0.086(15) 0.076(14) 0.030(12) 0.012(11) -0.028(11) C31 0.040(11) 0.071(13) 0.046(10) 0.010(9) 0.009(8) -0.005(9) C32 0.041(10) 0.051(10) 0.028(8) -0.011(7) 0.018(7) 0.001(8) C33 0.108(18) 0.069(13) 0.036(10) -0.033(10) 0.020(11) -0.001(12) C34 0.14(3) 0.12(2) 0.026(11) 0.000(11) 0.023(13) -0.013(19) C35 0.15(3) 0.14(3) 0.029(12) 0.025(14) 0.011(15) 0.02(2) C36 0.100(19) 0.088(16) 0.066(14) -0.003(13) -0.024(14) 0.038(14) C37 0.064(14) 0.067(13) 0.039(10) 0.010(9) 0.006(9) 0.017(10) C38 0.039(9) 0.034(9) 0.029(8) -0.003(7) -0.009(7) -0.011(7) C39 0.034(8) 0.024(7) 0.018(6) 0.004(6) 0.003(6) -0.004(7) C40 0.037(9) 0.031(8) 0.048(9) 0.012(8) -0.005(8) -0.001(7) C41 0.049(11) 0.040(10) 0.026(8) 0.006(7) 0.005(7) -0.005(8) C42 0.036(9) 0.039(9) 0.025(7) 0.014(7) -0.001(7) -0.013(7) C43 0.025(8) 0.041(9) 0.020(7) 0.005(6) -0.014(6) 0.006(7) C44 0.040(10) 0.049(10) 0.021(7) -0.006(7) -0.005(7) 0.003(8) C45 0.043(10) 0.032(9) 0.025(7) -0.003(6) -0.001(7) 0.002(7) C46 0.035(9) 0.045(10) 0.037(8) -0.002(7) 0.001(7) 0.017(8) C47 0.047(11) 0.035(9) 0.054(10) -0.006(8) -0.014(9) 0.006(8) C48 0.045(10) 0.038(9) 0.028(8) 0.009(7) -0.001(7) -0.009(8) C49 0.052(10) 0.048(10) 0.018(7) -0.008(7) -0.001(7) 0.007(9) C50 0.036(9) 0.036(8) 0.026(7) 0.013(7) -0.003(7) 0.004(8) C51 0.068(13) 0.040(10) 0.027(8) -0.006(7) 0.001(8) -0.004(9) C52 0.042(10) 0.048(10) 0.031(8) 0.000(8) 0.004(8) -0.004(8) C53 0.051(11) 0.053(11) 0.037(9) 0.015(8) 0.003(8) 0.005(9) C54 0.062(12) 0.040(9) 0.030(8) 0.002(7) -0.001(8) 0.009(9) C55 0.035(9) 0.042(9) 0.037(8) 0.003(7) 0.007(7) 0.011(8) C56 0.010(7) 0.051(9) 0.039(8) -0.010(8) 0.006(6) -0.008(7) C57 0.034(9) 0.035(8) 0.030(8) -0.010(7) -0.006(7) 0.009(7) C58 0.039(10) 0.046(10) 0.022(7) 0.001(7) 0.007(7) -0.015(8) C59 0.066(13) 0.040(9) 0.030(8) 0.002(7) -0.009(8) -0.025(9) C60 0.047(10) 0.056(10) 0.038(9) 0.001(8) -0.018(8) 0.003(9) C61 0.050(11) 0.046(10) 0.026(8) -0.008(7) 0.015(7) -0.008(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 Mo1 O1 2.154(9) . ? Mo1 O4 2.191(9) . ? Mo1 C21 2.325(17) . ? Mo1 S1 2.373(4) . ? Mo1 P2 2.402(4) . ? Mo1 P1 2.562(5) . ? Mo1 Ti1 2.730(3) . ? Mo1 H1 1.78(11) . ? Ti1 O2 1.925(9) . ? Ti1 O1 1.983(9) . ? Ti1 O3 1.996(10) . ? Ti1 O4 2.084(9) . ? Ti1 C21 2.285(15) . ? Ti1 C25 2.319(16) . ? Ti1 C23 2.444(17) . ? Ti1 C22 2.410(16) . ? Ti1 C24 2.419(17) . ? S1 C43 1.789(14) . ? S1 C57 1.888(15) . ? S2 C39 1.715(13) . ? S2 C49 1.821(15) . ? S3 C45 1.755(14) . ? S3 C55 1.821(14) . ? S4 C61 1.720(16) . ? S4 C51 1.725(15) . ? P1 C2 1.740(14) . ? P1 C1 1.821(15) . ? P1 C26 1.890(16) . ? P2 C32 1.719(15) . ? P2 C3 1.842(16) . ? P2 C4 1.946(16) . ? O1 C38 1.346(15) . ? O2 C44 1.345(17) . ? O3 C50 1.366(15) . ? O4 C56 1.412(15) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C17 1.60(2) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C17 1.49(3) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C17 1.48(2) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C18 1.41(3) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C18 1.48(3) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C18 1.51(3) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C19 1.53(2) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C19 1.48(2) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C19 1.52(3) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C20 1.39(2) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C20 1.56(3) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C20 1.49(2) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C41 1.50(2) . ? C18 C47 1.52(2) . ? C19 C53 1.57(2) . ? C20 C59 1.60(2) . ? C21 C22 1.36(2) . ? C21 C25 1.43(2) . ? C21 H2 0.92(11) . ? C22 C23 1.33(2) . ? C22 H22 0.9300 . ? C23 C24 1.47(2) . ? C23 H23 0.9300 . ? C24 C25 1.31(2) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C31 1.37(2) . ? C26 C27 1.46(2) . ? C27 C28 1.48(2) . ? C27 H27 0.9300 . ? C28 C29 1.32(3) . ? C28 H28 0.9300 . ? C29 C30 1.47(3) . ? C29 H29 0.9300 . ? C30 C31 1.40(2) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.42(2) . ? C32 C37 1.44(2) . ? C33 C34 1.31(3) . ? C33 H33 0.9300 . ? C34 C35 1.37(3) . ? C34 H34 0.9300 . ? C35 C36 1.40(3) . ? C35 H35 0.9300 . ? C36 C37 1.33(2) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C43 1.330(18) . ? C38 C39 1.374(18) . ? C39 C40 1.382(18) . ? C40 C41 1.35(2) . ? C40 H40 0.9300 . ? C41 C42 1.348(19) . ? C42 C43 1.349(18) . ? C42 H42 0.9300 . ? C44 C49 1.42(2) . ? C44 C45 1.432(19) . ? C45 C46 1.39(2) . ? C46 C47 1.37(2) . ? C46 H46 0.9300 . ? C47 C48 1.42(2) . ? C48 C49 1.43(2) . ? C48 H48 0.9300 . ? C50 C55 1.332(19) . ? C50 C51 1.44(2) . ? C51 C52 1.39(2) . ? C52 C53 1.33(2) . ? C52 H52 0.9300 . ? C53 C54 1.40(2) . ? C54 C55 1.39(2) . ? C54 H54 0.9300 . ? C56 C57 1.359(19) . ? C56 C61 1.46(2) . ? C57 C58 1.381(19) . ? C58 C59 1.41(2) . ? C58 H58 0.9300 . ? C59 C60 1.37(2) . ? C60 C61 1.44(2) . ? C60 H60 0.9300 . ? C62 C63 1.27(6) . ? C62 C64 1.30(5) . ? C62 C63 2.27(6) 5_566 ? C62 C64 2.05(5) 5_566 ? C63 C64 1.25(6) 5_566 ? C63 C62 2.27(6) 5_566 ? C64 C63 1.25(6) 5_566 ? C64 C62 2.05(5) 5_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 O1 Mo1 O4 74.4(3) . . ? O1 Mo1 C21 90.3(4) . . ? O4 Mo1 C21 80.1(4) . . ? O1 Mo1 S1 74.2(3) . . ? O4 Mo1 S1 75.5(2) . . ? C21 Mo1 S1 153.8(4) . . ? O1 Mo1 P2 155.5(3) . . ? O4 Mo1 P2 82.8(2) . . ? C21 Mo1 P2 94.3(4) . . ? S1 Mo1 P2 91.92(14) . . ? O1 Mo1 P1 87.0(3) . . ? O4 Mo1 P1 161.3(2) . . ? C21 Mo1 P1 102.6(4) . . ? S1 Mo1 P1 97.62(14) . . ? P2 Mo1 P1 115.19(14) . . ? O1 Mo1 Ti1 46.1(2) . . ? O4 Mo1 Ti1 48.6(2) . . ? C21 Mo1 Ti1 53.0(4) . . ? S1 Mo1 Ti1 102.51(11) . . ? P2 Mo1 Ti1 121.44(12) . . ? P1 Mo1 Ti1 118.42(11) . . ? O1 Mo1 H1 145(3) . . ? O4 Mo1 H1 139(3) . . ? C21 Mo1 H1 87(3) . . ? S1 Mo1 H1 118(3) . . ? P2 Mo1 H1 59(3) . . ? P1 Mo1 H1 60(3) . . ? Ti1 Mo1 H1 140(3) . . ? O2 Ti1 O1 83.1(4) . . ? O2 Ti1 O3 91.0(4) . . ? O1 Ti1 O3 117.8(4) . . ? O2 Ti1 O4 153.1(4) . . ? O1 Ti1 O4 80.4(4) . . ? O3 Ti1 O4 78.3(4) . . ? O2 Ti1 C21 119.6(5) . . ? O1 Ti1 C21 96.0(5) . . ? O3 Ti1 C21 137.5(5) . . ? O4 Ti1 C21 83.3(5) . . ? O2 Ti1 C25 131.5(5) . . ? O1 Ti1 C25 127.6(5) . . ? O3 Ti1 C25 101.7(5) . . ? O4 Ti1 C25 75.2(4) . . ? C21 Ti1 C25 36.1(5) . . ? O2 Ti1 C23 77.0(5) . . ? O1 Ti1 C23 123.5(6) . . ? O3 Ti1 C23 114.9(6) . . ? O4 Ti1 C23 129.9(5) . . ? C21 Ti1 C23 53.6(6) . . ? C25 Ti1 C23 55.1(5) . . ? O2 Ti1 C22 86.0(5) . . ? O1 Ti1 C22 95.4(5) . . ? O3 Ti1 C22 146.1(5) . . ? O4 Ti1 C22 116.5(5) . . ? C21 Ti1 C22 33.7(5) . . ? C25 Ti1 C22 57.9(6) . . ? C23 Ti1 C22 31.7(5) . . ? O2 Ti1 C24 102.5(5) . . ? O1 Ti1 C24 150.9(6) . . ? O3 Ti1 C24 90.8(5) . . ? O4 Ti1 C24 102.2(5) . . ? C21 Ti1 C24 56.2(6) . . ? C25 Ti1 C24 32.0(5) . . ? C23 Ti1 C24 35.1(6) . . ? C22 Ti1 C24 57.1(6) . . ? O2 Ti1 Mo1 128.0(3) . . ? O1 Ti1 Mo1 51.5(3) . . ? O3 Ti1 Mo1 129.3(3) . . ? O4 Ti1 Mo1 52.1(2) . . ? C21 Ti1 Mo1 54.4(4) . . ? C25 Ti1 Mo1 77.2(4) . . ? C23 Ti1 Mo1 105.6(5) . . ? C22 Ti1 Mo1 76.1(4) . . ? C24 Ti1 Mo1 107.3(5) . . ? C43 S1 C57 96.5(6) . . ? C43 S1 Mo1 103.0(5) . . ? C57 S1 Mo1 105.4(5) . . ? C39 S2 C49 95.9(7) . . ? C45 S3 C55 106.9(7) . . ? C61 S4 C51 104.2(7) . . ? C2 P1 C1 99.6(8) . . ? C2 P1 C26 97.1(8) . . ? C1 P1 C26 101.0(8) . . ? C2 P1 Mo1 112.9(6) . . ? C1 P1 Mo1 117.2(6) . . ? C26 P1 Mo1 124.6(5) . . ? C32 P2 C3 101.1(8) . . ? C32 P2 C4 105.4(7) . . ? C3 P2 C4 103.2(8) . . ? C32 P2 Mo1 110.0(5) . . ? C3 P2 Mo1 118.5(6) . . ? C4 P2 Mo1 116.8(5) . . ? C38 O1 Ti1 141.7(9) . . ? C38 O1 Mo1 124.0(8) . . ? Ti1 O1 Mo1 82.5(3) . . ? C44 O2 Ti1 125.1(9) . . ? C50 O3 Ti1 152.6(9) . . ? C56 O4 Ti1 127.6(8) . . ? C56 O4 Mo1 128.0(8) . . ? Ti1 O4 Mo1 79.3(3) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? P1 C2 H2A 109.5 . . ? P1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P2 C3 H3A 109.5 . . ? P2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P2 C4 H4A 109.5 . . ? P2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C17 C5 H5A 109.5 . . ? C17 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C17 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C17 C6 H6A 109.5 . . ? C17 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C17 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C17 C7 H7A 109.5 . . ? C17 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C17 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C18 C8 H8A 109.5 . . ? C18 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C18 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C18 C9 H9A 109.5 . . ? C18 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C18 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C18 C10 H10A 109.5 . . ? C18 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C18 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C19 C11 H11A 109.5 . . ? C19 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C19 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C19 C12 H12A 109.5 . . ? C19 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C19 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C19 C13 H13A 109.5 . . ? C19 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C19 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C20 C14 H14A 109.5 . . ? C20 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C20 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 H15A 109.5 . . ? C20 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C20 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C20 C16 H16A 109.5 . . ? C20 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C20 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C41 C17 C7 116.8(15) . . ? C41 C17 C6 106.9(15) . . ? C7 C17 C6 108(2) . . ? C41 C17 C5 107.1(14) . . ? C7 C17 C5 103.2(19) . . ? C6 C17 C5 115(2) . . ? C8 C18 C9 103(3) . . ? C8 C18 C47 112.3(16) . . ? C9 C18 C47 107.6(19) . . ? C8 C18 C10 116(2) . . ? C9 C18 C10 103(2) . . ? C47 C18 C10 113.4(17) . . ? C12 C19 C13 105.8(18) . . ? C12 C19 C53 104.1(15) . . ? C13 C19 C53 119.9(16) . . ? C12 C19 C11 111.2(18) . . ? C13 C19 C11 104.3(18) . . ? C53 C19 C11 111.5(15) . . ? C14 C20 C16 116.8(19) . . ? C14 C20 C15 102.5(19) . . ? C16 C20 C15 105.0(19) . . ? C14 C20 C59 106.8(14) . . ? C16 C20 C59 120.4(14) . . ? C15 C20 C59 102.9(15) . . ? C22 C21 C25 110.2(15) . . ? C22 C21 Mo1 116.6(12) . . ? C25 C21 Mo1 113.0(10) . . ? C22 C21 Ti1 78.2(9) . . ? C25 C21 Ti1 73.2(9) . . ? Mo1 C21 Ti1 72.6(5) . . ? C22 C21 H2 130(8) . . ? C25 C21 H2 114(7) . . ? Mo1 C21 H2 66(7) . . ? Ti1 C21 H2 137(7) . . ? C23 C22 C21 105.2(18) . . ? C23 C22 Ti1 75.6(11) . . ? C21 C22 Ti1 68.2(9) . . ? C23 C22 H22 127.4 . . ? C21 C22 H22 127.4 . . ? Ti1 C22 H22 120.7 . . ? C22 C23 C24 111.3(16) . . ? C22 C23 Ti1 72.7(9) . . ? C24 C23 Ti1 71.5(9) . . ? C22 C23 H23 124.3 . . ? C24 C23 H23 124.3 . . ? Ti1 C23 H23 123.0 . . ? C25 C24 C23 105.1(16) . . ? C25 C24 Ti1 69.8(10) . . ? C23 C24 Ti1 73.4(9) . . ? C25 C24 H24 127.5 . . ? C23 C24 H24 127.5 . . ? Ti1 C24 H24 121.2 . . ? C24 C25 C21 108.2(15) . . ? C24 C25 Ti1 78.2(11) . . ? C21 C25 Ti1 70.6(9) . . ? C24 C25 H25 125.9 . . ? C21 C25 H25 125.9 . . ? Ti1 C25 H25 117.2 . . ? C31 C26 C27 112.2(15) . . ? C31 C26 P1 123.0(13) . . ? C27 C26 P1 124.8(13) . . ? C26 C27 C28 128.2(16) . . ? C26 C27 H27 115.9 . . ? C28 C27 H27 115.9 . . ? C29 C28 C27 113.3(18) . . ? C29 C28 H28 123.3 . . ? C27 C28 H28 123.3 . . ? C28 C29 C30 122.0(18) . . ? C28 C29 H29 119.0 . . ? C30 C29 H29 119.0 . . ? C31 C30 C29 121.3(18) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C26 C31 C30 122.8(18) . . ? C26 C31 H31 118.6 . . ? C30 C31 H31 118.6 . . ? C33 C32 C37 124.1(16) . . ? C33 C32 P2 114.2(13) . . ? C37 C32 P2 121.4(12) . . ? C34 C33 C32 115(2) . . ? C34 C33 H33 122.5 . . ? C32 C33 H33 122.5 . . ? C33 C34 C35 122(2) . . ? C33 C34 H34 118.8 . . ? C35 C34 H34 118.8 . . ? C34 C35 C36 123(2) . . ? C34 C35 H35 118.3 . . ? C36 C35 H35 118.3 . . ? C37 C36 C35 118(2) . . ? C37 C36 H36 120.9 . . ? C35 C36 H36 120.9 . . ? C36 C37 C32 117.0(19) . . ? C36 C37 H37 121.5 . . ? C32 C37 H37 121.5 . . ? O1 C38 C43 118.2(13) . . ? O1 C38 C39 127.8(12) . . ? C43 C38 C39 113.7(13) . . ? C38 C39 C40 123.2(13) . . ? C38 C39 S2 120.5(10) . . ? C40 C39 S2 116.0(11) . . ? C41 C40 C39 121.4(14) . . ? C41 C40 H40 119.3 . . ? C39 C40 H40 119.3 . . ? C42 C41 C40 113.7(14) . . ? C42 C41 C17 125.0(13) . . ? C40 C41 C17 121.1(14) . . ? C43 C42 C41 124.9(14) . . ? C43 C42 H42 117.5 . . ? C41 C42 H42 117.5 . . ? C38 C43 C42 122.7(14) . . ? C38 C43 S1 114.2(11) . . ? C42 C43 S1 123.1(11) . . ? O2 C44 C49 118.9(13) . . ? O2 C44 C45 128.0(14) . . ? C49 C44 C45 112.7(14) . . ? C46 C45 C44 123.3(14) . . ? C46 C45 S3 120.1(11) . . ? C44 C45 S3 116.4(12) . . ? C45 C46 C47 125.0(15) . . ? C45 C46 H46 117.5 . . ? C47 C46 H46 117.5 . . ? C46 C47 C48 114.1(15) . . ? C46 C47 C18 122.4(15) . . ? C48 C47 C18 123.2(14) . . ? C49 C48 C47 122.6(14) . . ? C49 C48 H48 118.7 . . ? C47 C48 H48 118.7 . . ? C44 C49 C48 122.1(14) . . ? C44 C49 S2 117.6(12) . . ? C48 C49 S2 120.2(12) . . ? C55 C50 O3 118.8(13) . . ? C55 C50 C51 113.7(13) . . ? O3 C50 C51 127.4(13) . . ? C52 C51 C50 125.1(13) . . ? C52 C51 S4 119.1(13) . . ? C50 C51 S4 115.1(12) . . ? C53 C52 C51 121.2(16) . . ? C53 C52 H52 119.4 . . ? C51 C52 H52 119.4 . . ? C52 C53 C54 112.7(15) . . ? C52 C53 C19 117.4(15) . . ? C54 C53 C19 129.9(15) . . ? C55 C54 C53 127.9(14) . . ? C55 C54 H54 116.1 . . ? C53 C54 H54 116.1 . . ? C50 C55 C54 119.3(14) . . ? C50 C55 S3 118.2(12) . . ? C54 C55 S3 121.8(11) . . ? C57 C56 O4 116.0(12) . . ? C57 C56 C61 117.2(12) . . ? O4 C56 C61 126.7(13) . . ? C56 C57 C58 117.9(13) . . ? C56 C57 S1 114.4(11) . . ? C58 C57 S1 127.7(11) . . ? C59 C58 C57 127.7(14) . . ? C59 C58 H58 116.2 . . ? C57 C58 H58 116.2 . . ? C60 C59 C58 116.0(15) . . ? C60 C59 C20 114.4(15) . . ? C58 C59 C20 129.5(14) . . ? C59 C60 C61 118.3(15) . . ? C59 C60 H60 120.9 . . ? C61 C60 H60 120.9 . . ? C60 C61 C56 122.6(13) . . ? C60 C61 S4 116.2(12) . . ? C56 C61 S4 120.7(11) . . ? C63 C62 C64 126(5) . . ? C63 C62 C63 99(4) . 5_566 ? C64 C62 C63 27(3) . 5_566 ? C63 C62 C64 35(3) . 5_566 ? C64 C62 C64 90(4) . 5_566 ? C63 C62 C64 64(2) 5_566 5_566 ? C64 C63 C62 109(6) 5_566 . ? C64 C63 C62 28(3) 5_566 5_566 ? C62 C63 C62 81(4) . 5_566 ? C63 C64 C62 126(6) 5_566 . ? C63 C64 C62 36(3) 5_566 5_566 ? C62 C64 C62 90(4) . 5_566 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Mo1 Ti1 O2 35.2(5) . . . . ? O4 Mo1 Ti1 O2 145.7(5) . . . . ? C21 Mo1 Ti1 O2 -102.1(6) . . . . ? S1 Mo1 Ti1 O2 88.3(4) . . . . ? P2 Mo1 Ti1 O2 -171.6(4) . . . . ? P1 Mo1 Ti1 O2 -17.7(4) . . . . ? O4 Mo1 Ti1 O1 110.5(5) . . . . ? C21 Mo1 Ti1 O1 -137.3(6) . . . . ? S1 Mo1 Ti1 O1 53.1(4) . . . . ? P2 Mo1 Ti1 O1 153.2(4) . . . . ? P1 Mo1 Ti1 O1 -52.9(4) . . . . ? O1 Mo1 Ti1 O3 -96.8(5) . . . . ? O4 Mo1 Ti1 O3 13.7(5) . . . . ? C21 Mo1 Ti1 O3 125.9(6) . . . . ? S1 Mo1 Ti1 O3 -43.7(4) . . . . ? P2 Mo1 Ti1 O3 56.4(4) . . . . ? P1 Mo1 Ti1 O3 -149.7(4) . . . . ? O1 Mo1 Ti1 O4 -110.5(5) . . . . ? C21 Mo1 Ti1 O4 112.1(6) . . . . ? S1 Mo1 Ti1 O4 -57.5(3) . . . . ? P2 Mo1 Ti1 O4 42.7(3) . . . . ? P1 Mo1 Ti1 O4 -163.4(3) . . . . ? O1 Mo1 Ti1 C21 137.3(6) . . . . ? O4 Mo1 Ti1 C21 -112.1(6) . . . . ? S1 Mo1 Ti1 C21 -169.6(5) . . . . ? P2 Mo1 Ti1 C21 -69.5(5) . . . . ? P1 Mo1 Ti1 C21 84.5(5) . . . . ? O1 Mo1 Ti1 C25 168.4(5) . . . . ? O4 Mo1 Ti1 C25 -81.1(5) . . . . ? C21 Mo1 Ti1 C25 31.1(6) . . . . ? S1 Mo1 Ti1 C25 -138.5(4) . . . . ? P2 Mo1 Ti1 C25 -38.4(4) . . . . ? P1 Mo1 Ti1 C25 115.5(4) . . . . ? O1 Mo1 Ti1 C23 120.7(6) . . . . ? O4 Mo1 Ti1 C23 -128.8(6) . . . . ? C21 Mo1 Ti1 C23 -16.7(7) . . . . ? S1 Mo1 Ti1 C23 173.7(5) . . . . ? P2 Mo1 Ti1 C23 -86.1(5) . . . . ? P1 Mo1 Ti1 C23 67.8(5) . . . . ? O1 Mo1 Ti1 C22 108.7(6) . . . . ? O4 Mo1 Ti1 C22 -140.7(6) . . . . ? C21 Mo1 Ti1 C22 -28.6(7) . . . . ? S1 Mo1 Ti1 C22 161.8(5) . . . . ? P2 Mo1 Ti1 C22 -98.1(5) . . . . ? P1 Mo1 Ti1 C22 55.9(5) . . . . ? O1 Mo1 Ti1 C24 157.3(6) . . . . ? O4 Mo1 Ti1 C24 -92.2(6) . . . . ? C21 Mo1 Ti1 C24 20.0(7) . . . . ? S1 Mo1 Ti1 C24 -149.6(5) . . . . ? P2 Mo1 Ti1 C24 -49.5(5) . . . . ? P1 Mo1 Ti1 C24 104.4(5) . . . . ? O1 Mo1 S1 C43 -18.3(5) . . . . ? O4 Mo1 S1 C43 -95.9(5) . . . . ? C21 Mo1 S1 C43 -74.1(10) . . . . ? P2 Mo1 S1 C43 -177.9(4) . . . . ? P1 Mo1 S1 C43 66.4(4) . . . . ? Ti1 Mo1 S1 C43 -55.1(4) . . . . ? O1 Mo1 S1 C57 82.3(5) . . . . ? O4 Mo1 S1 C57 4.8(5) . . . . ? C21 Mo1 S1 C57 26.5(10) . . . . ? P2 Mo1 S1 C57 -77.3(5) . . . . ? P1 Mo1 S1 C57 167.0(5) . . . . ? Ti1 Mo1 S1 C57 45.6(5) . . . . ? O1 Mo1 P1 C2 125.5(7) . . . . ? O4 Mo1 P1 C2 118.8(10) . . . . ? C21 Mo1 P1 C2 -144.8(7) . . . . ? S1 Mo1 P1 C2 51.9(7) . . . . ? P2 Mo1 P1 C2 -43.8(7) . . . . ? Ti1 Mo1 P1 C2 160.6(6) . . . . ? O1 Mo1 P1 C1 10.6(6) . . . . ? O4 Mo1 P1 C1 3.8(10) . . . . ? C21 Mo1 P1 C1 100.3(7) . . . . ? S1 Mo1 P1 C1 -63.0(6) . . . . ? P2 Mo1 P1 C1 -158.8(6) . . . . ? Ti1 Mo1 P1 C1 45.7(6) . . . . ? O1 Mo1 P1 C26 -117.3(6) . . . . ? O4 Mo1 P1 C26 -124.1(9) . . . . ? C21 Mo1 P1 C26 -27.6(7) . . . . ? S1 Mo1 P1 C26 169.1(6) . . . . ? P2 Mo1 P1 C26 73.3(6) . . . . ? Ti1 Mo1 P1 C26 -82.2(6) . . . . ? O1 Mo1 P2 C32 -112.2(8) . . . . ? O4 Mo1 P2 C32 -133.0(6) . . . . ? C21 Mo1 P2 C32 147.5(7) . . . . ? S1 Mo1 P2 C32 -57.9(6) . . . . ? P1 Mo1 P2 C32 41.4(6) . . . . ? Ti1 Mo1 P2 C32 -163.9(6) . . . . ? O1 Mo1 P2 C3 132.3(9) . . . . ? O4 Mo1 P2 C3 111.5(8) . . . . ? C21 Mo1 P2 C3 32.0(8) . . . . ? S1 Mo1 P2 C3 -173.4(7) . . . . ? P1 Mo1 P2 C3 -74.1(8) . . . . ? Ti1 Mo1 P2 C3 80.6(8) . . . . ? O1 Mo1 P2 C4 7.9(9) . . . . ? O4 Mo1 P2 C4 -13.0(6) . . . . ? C21 Mo1 P2 C4 -92.4(7) . . . . ? S1 Mo1 P2 C4 62.1(6) . . . . ? P1 Mo1 P2 C4 161.5(6) . . . . ? Ti1 Mo1 P2 C4 -43.8(6) . . . . ? O2 Ti1 O1 C38 69.3(14) . . . . ? O3 Ti1 O1 C38 -18.2(15) . . . . ? O4 Ti1 O1 C38 -89.5(14) . . . . ? C21 Ti1 O1 C38 -171.6(14) . . . . ? C25 Ti1 O1 C38 -152.3(13) . . . . ? C23 Ti1 O1 C38 138.6(14) . . . . ? C22 Ti1 O1 C38 154.6(14) . . . . ? C24 Ti1 O1 C38 172.7(14) . . . . ? Mo1 Ti1 O1 C38 -138.0(15) . . . . ? O2 Ti1 O1 Mo1 -152.8(4) . . . . ? O3 Ti1 O1 Mo1 119.7(4) . . . . ? O4 Ti1 O1 Mo1 48.5(3) . . . . ? C21 Ti1 O1 Mo1 -33.6(5) . . . . ? C25 Ti1 O1 Mo1 -14.3(6) . . . . ? C23 Ti1 O1 Mo1 -83.4(6) . . . . ? C22 Ti1 O1 Mo1 -67.5(5) . . . . ? C24 Ti1 O1 Mo1 -49.3(11) . . . . ? O4 Mo1 O1 C38 103.1(11) . . . . ? C21 Mo1 O1 C38 -177.3(11) . . . . ? S1 Mo1 O1 C38 24.1(10) . . . . ? P2 Mo1 O1 C38 81.6(12) . . . . ? P1 Mo1 O1 C38 -74.6(11) . . . . ? Ti1 Mo1 O1 C38 150.0(12) . . . . ? O4 Mo1 O1 Ti1 -46.9(3) . . . . ? C21 Mo1 O1 Ti1 32.8(5) . . . . ? S1 Mo1 O1 Ti1 -125.8(3) . . . . ? P2 Mo1 O1 Ti1 -68.3(7) . . . . ? P1 Mo1 O1 Ti1 135.4(3) . . . . ? O1 Ti1 O2 C44 -87.8(10) . . . . ? O3 Ti1 O2 C44 30.1(11) . . . . ? O4 Ti1 O2 C44 -35.4(15) . . . . ? C21 Ti1 O2 C44 179.2(10) . . . . ? C25 Ti1 O2 C44 136.7(11) . . . . ? C23 Ti1 O2 C44 145.4(12) . . . . ? C22 Ti1 O2 C44 176.2(11) . . . . ? C24 Ti1 O2 C44 121.2(11) . . . . ? Mo1 Ti1 O2 C44 -114.8(10) . . . . ? O2 Ti1 O3 C50 99.6(19) . . . . ? O1 Ti1 O3 C50 -177.6(18) . . . . ? O4 Ti1 O3 C50 -105(2) . . . . ? C21 Ti1 O3 C50 -39(2) . . . . ? C25 Ti1 O3 C50 -33(2) . . . . ? C23 Ti1 O3 C50 24(2) . . . . ? C22 Ti1 O3 C50 15(2) . . . . ? C24 Ti1 O3 C50 -3(2) . . . . ? Mo1 Ti1 O3 C50 -116.2(19) . . . . ? O2 Ti1 O4 C56 29.4(15) . . . . ? O1 Ti1 O4 C56 82.3(10) . . . . ? O3 Ti1 O4 C56 -38.9(10) . . . . ? C21 Ti1 O4 C56 179.5(11) . . . . ? C25 Ti1 O4 C56 -144.6(11) . . . . ? C23 Ti1 O4 C56 -151.7(11) . . . . ? C22 Ti1 O4 C56 173.6(10) . . . . ? C24 Ti1 O4 C56 -127.2(11) . . . . ? Mo1 Ti1 O4 C56 130.3(11) . . . . ? O2 Ti1 O4 Mo1 -100.9(8) . . . . ? O1 Ti1 O4 Mo1 -48.0(3) . . . . ? O3 Ti1 O4 Mo1 -169.2(4) . . . . ? C21 Ti1 O4 Mo1 49.3(5) . . . . ? C25 Ti1 O4 Mo1 85.2(4) . . . . ? C23 Ti1 O4 Mo1 78.0(7) . . . . ? C22 Ti1 O4 Mo1 43.3(6) . . . . ? C24 Ti1 O4 Mo1 102.5(5) . . . . ? O1 Mo1 O4 C56 -85.5(10) . . . . ? C21 Mo1 O4 C56 -178.6(11) . . . . ? S1 Mo1 O4 C56 -8.1(9) . . . . ? P2 Mo1 O4 C56 85.8(10) . . . . ? P1 Mo1 O4 C56 -78.4(13) . . . . ? Ti1 Mo1 O4 C56 -129.9(11) . . . . ? O1 Mo1 O4 Ti1 44.4(3) . . . . ? C21 Mo1 O4 Ti1 -48.7(4) . . . . ? S1 Mo1 O4 Ti1 121.8(3) . . . . ? P2 Mo1 O4 Ti1 -144.3(2) . . . . ? P1 Mo1 O4 Ti1 51.5(9) . . . . ? O1 Mo1 C21 C22 37.4(12) . . . . ? O4 Mo1 C21 C22 111.5(12) . . . . ? S1 Mo1 C21 C22 90.1(15) . . . . ? P2 Mo1 C21 C22 -166.6(12) . . . . ? P1 Mo1 C21 C22 -49.6(13) . . . . ? Ti1 Mo1 C21 C22 66.6(12) . . . . ? O1 Mo1 C21 C25 -91.8(11) . . . . ? O4 Mo1 C21 C25 -17.7(11) . . . . ? S1 Mo1 C21 C25 -39.0(17) . . . . ? P2 Mo1 C21 C25 64.2(11) . . . . ? P1 Mo1 C21 C25 -178.8(10) . . . . ? Ti1 Mo1 C21 C25 -62.6(10) . . . . ? O1 Mo1 C21 Ti1 -29.2(4) . . . . ? O4 Mo1 C21 Ti1 44.9(3) . . . . ? S1 Mo1 C21 Ti1 23.5(11) . . . . ? P2 Mo1 C21 Ti1 126.8(3) . . . . ? P1 Mo1 C21 Ti1 -116.2(3) . . . . ? O2 Ti1 C21 C22 -5.4(13) . . . . ? O1 Ti1 C21 C22 -90.8(11) . . . . ? O3 Ti1 C21 C22 125.2(10) . . . . ? O4 Ti1 C21 C22 -170.4(11) . . . . ? C25 Ti1 C21 C22 115.6(14) . . . . ? C23 Ti1 C21 C22 36.9(10) . . . . ? C24 Ti1 C21 C22 80.1(11) . . . . ? Mo1 Ti1 C21 C22 -123.0(12) . . . . ? O2 Ti1 C21 C25 -120.9(8) . . . . ? O1 Ti1 C21 C25 153.6(8) . . . . ? O3 Ti1 C21 C25 9.6(12) . . . . ? O4 Ti1 C21 C25 74.1(8) . . . . ? C23 Ti1 C21 C25 -78.7(10) . . . . ? C22 Ti1 C21 C25 -115.6(14) . . . . ? C24 Ti1 C21 C25 -35.5(9) . . . . ? Mo1 Ti1 C21 C25 121.4(9) . . . . ? O2 Ti1 C21 Mo1 117.7(4) . . . . ? O1 Ti1 C21 Mo1 32.2(4) . . . . ? O3 Ti1 C21 Mo1 -111.8(6) . . . . ? O4 Ti1 C21 Mo1 -47.3(3) . . . . ? C25 Ti1 C21 Mo1 -121.4(9) . . . . ? C23 Ti1 C21 Mo1 159.9(8) . . . . ? C22 Ti1 C21 Mo1 123.0(12) . . . . ? C24 Ti1 C21 Mo1 -156.9(8) . . . . ? C25 C21 C22 C23 -0.3(19) . . . . ? Mo1 C21 C22 C23 -130.7(12) . . . . ? Ti1 C21 C22 C23 -67.2(12) . . . . ? C25 C21 C22 Ti1 67.0(11) . . . . ? Mo1 C21 C22 Ti1 -63.5(8) . . . . ? O2 Ti1 C22 C23 -71.5(11) . . . . ? O1 Ti1 C22 C23 -154.1(11) . . . . ? O3 Ti1 C22 C23 14.5(17) . . . . ? O4 Ti1 C22 C23 123.9(11) . . . . ? C21 Ti1 C22 C23 113.2(17) . . . . ? C25 Ti1 C22 C23 74.3(12) . . . . ? C24 Ti1 C22 C23 36.2(11) . . . . ? Mo1 Ti1 C22 C23 157.8(12) . . . . ? O2 Ti1 C22 C21 175.3(11) . . . . ? O1 Ti1 C22 C21 92.7(11) . . . . ? O3 Ti1 C22 C21 -98.7(12) . . . . ? O4 Ti1 C22 C21 10.7(12) . . . . ? C25 Ti1 C22 C21 -38.9(10) . . . . ? C23 Ti1 C22 C21 -113.2(17) . . . . ? C24 Ti1 C22 C21 -77.0(12) . . . . ? Mo1 Ti1 C22 C21 44.6(10) . . . . ? C21 C22 C23 C24 1(2) . . . . ? Ti1 C22 C23 C24 -61.4(13) . . . . ? C21 C22 C23 Ti1 62.1(11) . . . . ? O2 Ti1 C23 C22 103.9(12) . . . . ? O1 Ti1 C23 C22 31.4(13) . . . . ? O3 Ti1 C23 C22 -171.1(10) . . . . ? O4 Ti1 C23 C22 -75.6(13) . . . . ? C21 Ti1 C23 C22 -39.2(11) . . . . ? C25 Ti1 C23 C22 -84.1(12) . . . . ? C24 Ti1 C23 C22 -120.4(16) . . . . ? Mo1 Ti1 C23 C22 -22.4(12) . . . . ? O2 Ti1 C23 C24 -135.8(11) . . . . ? O1 Ti1 C23 C24 151.8(10) . . . . ? O3 Ti1 C23 C24 -50.8(11) . . . . ? O4 Ti1 C23 C24 44.7(13) . . . . ? C21 Ti1 C23 C24 81.1(11) . . . . ? C25 Ti1 C23 C24 36.3(10) . . . . ? C22 Ti1 C23 C24 120.4(16) . . . . ? Mo1 Ti1 C23 C24 98.0(10) . . . . ? C22 C23 C24 C25 -1(2) . . . . ? Ti1 C23 C24 C25 -63.0(12) . . . . ? C22 C23 C24 Ti1 62.2(13) . . . . ? O2 Ti1 C24 C25 157.6(10) . . . . ? O1 Ti1 C24 C25 59.2(16) . . . . ? O3 Ti1 C24 C25 -111.1(11) . . . . ? O4 Ti1 C24 C25 -33.0(11) . . . . ? C21 Ti1 C24 C25 40.3(10) . . . . ? C23 Ti1 C24 C25 113.5(16) . . . . ? C22 Ti1 C24 C25 80.8(11) . . . . ? Mo1 Ti1 C24 C25 20.8(11) . . . . ? O2 Ti1 C24 C23 44.1(11) . . . . ? O1 Ti1 C24 C23 -54.3(16) . . . . ? O3 Ti1 C24 C23 135.4(10) . . . . ? O4 Ti1 C24 C23 -146.5(10) . . . . ? C21 Ti1 C24 C23 -73.2(11) . . . . ? C25 Ti1 C24 C23 -113.5(16) . . . . ? C22 Ti1 C24 C23 -32.7(10) . . . . ? Mo1 Ti1 C24 C23 -92.7(10) . . . . ? C23 C24 C25 C21 0.7(19) . . . . ? Ti1 C24 C25 C21 -64.8(11) . . . . ? C23 C24 C25 Ti1 65.5(12) . . . . ? C22 C21 C25 C24 0(2) . . . . ? Mo1 C21 C25 C24 132.1(12) . . . . ? Ti1 C21 C25 C24 69.9(13) . . . . ? C22 C21 C25 Ti1 -70.2(12) . . . . ? Mo1 C21 C25 Ti1 62.2(7) . . . . ? O2 Ti1 C25 C24 -29.7(14) . . . . ? O1 Ti1 C25 C24 -148.2(10) . . . . ? O3 Ti1 C25 C24 72.3(11) . . . . ? O4 Ti1 C25 C24 146.6(12) . . . . ? C21 Ti1 C25 C24 -114.4(14) . . . . ? C23 Ti1 C25 C24 -40.1(11) . . . . ? C22 Ti1 C25 C24 -78.2(11) . . . . ? Mo1 Ti1 C25 C24 -159.7(11) . . . . ? O2 Ti1 C25 C21 84.6(10) . . . . ? O1 Ti1 C25 C21 -33.9(11) . . . . ? O3 Ti1 C25 C21 -173.4(8) . . . . ? O4 Ti1 C25 C21 -99.0(9) . . . . ? C23 Ti1 C25 C21 74.3(10) . . . . ? C22 Ti1 C25 C21 36.2(9) . . . . ? C24 Ti1 C25 C21 114.4(14) . . . . ? Mo1 Ti1 C25 C21 -45.3(8) . . . . ? C2 P1 C26 C31 118.2(14) . . . . ? C1 P1 C26 C31 -140.5(14) . . . . ? Mo1 P1 C26 C31 -6.1(16) . . . . ? C2 P1 C26 C27 -62.9(15) . . . . ? C1 P1 C26 C27 38.4(15) . . . . ? Mo1 P1 C26 C27 172.7(11) . . . . ? C31 C26 C27 C28 0(3) . . . . ? P1 C26 C27 C28 -179.2(14) . . . . ? C26 C27 C28 C29 1(3) . . . . ? C27 C28 C29 C30 1(3) . . . . ? C28 C29 C30 C31 -3(3) . . . . ? C27 C26 C31 C30 -2(2) . . . . ? P1 C26 C31 C30 177.1(14) . . . . ? C29 C30 C31 C26 3(3) . . . . ? C3 P2 C32 C33 -153.3(13) . . . . ? C4 P2 C32 C33 -46.2(14) . . . . ? Mo1 P2 C32 C33 80.6(13) . . . . ? C3 P2 C32 C37 32.4(15) . . . . ? C4 P2 C32 C37 139.6(14) . . . . ? Mo1 P2 C32 C37 -93.7(14) . . . . ? C37 C32 C33 C34 1(3) . . . . ? P2 C32 C33 C34 -173.5(16) . . . . ? C32 C33 C34 C35 0(4) . . . . ? C33 C34 C35 C36 -1(5) . . . . ? C34 C35 C36 C37 1(4) . . . . ? C35 C36 C37 C32 -1(3) . . . . ? C33 C32 C37 C36 0(3) . . . . ? P2 C32 C37 C36 173.6(14) . . . . ? Ti1 O1 C38 C43 106.4(15) . . . . ? Mo1 O1 C38 C43 -20.4(18) . . . . ? Ti1 O1 C38 C39 -80(2) . . . . ? Mo1 O1 C38 C39 153.4(12) . . . . ? O1 C38 C39 C40 -178.9(14) . . . . ? C43 C38 C39 C40 -5(2) . . . . ? O1 C38 C39 S2 -5(2) . . . . ? C43 C38 C39 S2 168.9(11) . . . . ? C49 S2 C39 C38 85.8(13) . . . . ? C49 S2 C39 C40 -100.0(12) . . . . ? C38 C39 C40 C41 1(2) . . . . ? S2 C39 C40 C41 -173.0(12) . . . . ? C39 C40 C41 C42 4(2) . . . . ? C39 C40 C41 C17 -179.8(14) . . . . ? C7 C17 C41 C42 -176(2) . . . . ? C6 C17 C41 C42 63(3) . . . . ? C5 C17 C41 C42 -61(2) . . . . ? C7 C17 C41 C40 8(3) . . . . ? C6 C17 C41 C40 -113(2) . . . . ? C5 C17 C41 C40 123.4(18) . . . . ? C40 C41 C42 C43 -5(2) . . . . ? C17 C41 C42 C43 178.7(15) . . . . ? O1 C38 C43 C42 178.4(13) . . . . ? C39 C38 C43 C42 4(2) . . . . ? O1 C38 C43 S1 -1.2(18) . . . . ? C39 C38 C43 S1 -175.9(10) . . . . ? C41 C42 C43 C38 1(2) . . . . ? C41 C42 C43 S1 -179.1(13) . . . . ? C57 S1 C43 C38 -90.3(12) . . . . ? Mo1 S1 C43 C38 17.3(12) . . . . ? C57 S1 C43 C42 90.1(13) . . . . ? Mo1 S1 C43 C42 -162.4(11) . . . . ? Ti1 O2 C44 C49 109.4(13) . . . . ? Ti1 O2 C44 C45 -77.8(17) . . . . ? O2 C44 C45 C46 -175.6(13) . . . . ? C49 C44 C45 C46 -2(2) . . . . ? O2 C44 C45 S3 -1(2) . . . . ? C49 C44 C45 S3 171.8(10) . . . . ? C55 S3 C45 C46 -83.7(13) . . . . ? C55 S3 C45 C44 101.9(12) . . . . ? C44 C45 C46 C47 -1(2) . . . . ? S3 C45 C46 C47 -175.3(12) . . . . ? C45 C46 C47 C48 3(2) . . . . ? C45 C46 C47 C18 177.8(15) . . . . ? C8 C18 C47 C46 -177(3) . . . . ? C9 C18 C47 C46 -64(3) . . . . ? C10 C18 C47 C46 50(3) . . . . ? C8 C18 C47 C48 -3(3) . . . . ? C9 C18 C47 C48 110(2) . . . . ? C10 C18 C47 C48 -136(2) . . . . ? C46 C47 C48 C49 -2(2) . . . . ? C18 C47 C48 C49 -176.2(15) . . . . ? O2 C44 C49 C48 177.7(12) . . . . ? C45 C44 C49 C48 4(2) . . . . ? O2 C44 C49 S2 -0.3(18) . . . . ? C45 C44 C49 S2 -174.1(10) . . . . ? C47 C48 C49 C44 -2(2) . . . . ? C47 C48 C49 S2 176.1(12) . . . . ? C39 S2 C49 C44 -91.1(12) . . . . ? C39 S2 C49 C48 91.0(12) . . . . ? Ti1 O3 C50 C55 -82(2) . . . . ? Ti1 O3 C50 C51 100(2) . . . . ? C55 C50 C51 C52 -3(2) . . . . ? O3 C50 C51 C52 175.7(14) . . . . ? C55 C50 C51 S4 167.5(12) . . . . ? O3 C50 C51 S4 -14(2) . . . . ? C61 S4 C51 C52 -129.1(13) . . . . ? C61 S4 C51 C50 60.2(13) . . . . ? C50 C51 C52 C53 3(3) . . . . ? S4 C51 C52 C53 -166.5(13) . . . . ? C51 C52 C53 C54 -2(2) . . . . ? C51 C52 C53 C19 -179.9(15) . . . . ? C12 C19 C53 C52 -124.9(19) . . . . ? C13 C19 C53 C52 -7(3) . . . . ? C11 C19 C53 C52 115.2(18) . . . . ? C12 C19 C53 C54 58(3) . . . . ? C13 C19 C53 C54 176(2) . . . . ? C11 C19 C53 C54 -62(2) . . . . ? C52 C53 C54 C55 1(3) . . . . ? C19 C53 C54 C55 178.6(16) . . . . ? O3 C50 C55 C54 -177.0(13) . . . . ? C51 C50 C55 C54 1(2) . . . . ? O3 C50 C55 S3 12.7(19) . . . . ? C51 C50 C55 S3 -168.9(11) . . . . ? C53 C54 C55 C50 -1(3) . . . . ? C53 C54 C55 S3 168.9(14) . . . . ? C45 S3 C55 C50 -66.5(14) . . . . ? C45 S3 C55 C54 123.5(13) . . . . ? Ti1 O4 C56 C57 -99.4(13) . . . . ? Mo1 O4 C56 C57 8.5(17) . . . . ? Ti1 O4 C56 C61 81.9(17) . . . . ? Mo1 O4 C56 C61 -170.3(11) . . . . ? O4 C56 C57 C58 177.5(12) . . . . ? C61 C56 C57 C58 -4(2) . . . . ? O4 C56 C57 S1 -2.3(16) . . . . ? C61 C56 C57 S1 176.6(10) . . . . ? C43 S1 C57 C56 102.4(11) . . . . ? Mo1 S1 C57 C56 -3.1(12) . . . . ? C43 S1 C57 C58 -77.4(14) . . . . ? Mo1 S1 C57 C58 177.2(12) . . . . ? C56 C57 C58 C59 -1(2) . . . . ? S1 C57 C58 C59 178.8(12) . . . . ? C57 C58 C59 C60 4(2) . . . . ? C57 C58 C59 C20 -176.8(16) . . . . ? C14 C20 C59 C60 129.1(19) . . . . ? C16 C20 C59 C60 -7(3) . . . . ? C15 C20 C59 C60 -123.4(17) . . . . ? C14 C20 C59 C58 -50(3) . . . . ? C16 C20 C59 C58 173.4(19) . . . . ? C15 C20 C59 C58 57(2) . . . . ? C58 C59 C60 C61 -2(2) . . . . ? C20 C59 C60 C61 178.7(14) . . . . ? C59 C60 C61 C56 -3(2) . . . . ? C59 C60 C61 S4 169.4(12) . . . . ? C57 C56 C61 C60 6(2) . . . . ? O4 C56 C61 C60 -175.7(13) . . . . ? C57 C56 C61 S4 -166.1(11) . . . . ? O4 C56 C61 S4 13(2) . . . . ? C51 S4 C61 C60 85.6(13) . . . . ? C51 S4 C61 C56 -102.3(13) . . . . ? C64 C62 C63 C64 -1(11) . . . 5_566 ? C63 C62 C63 C64 -1(5) 5_566 . . 5_566 ? C64 C62 C63 C62 -1(6) . . . 5_566 ? C63 C62 C63 C62 0.000(5) 5_566 . . 5_566 ? C64 C62 C63 C62 1(5) 5_566 . . 5_566 ? C63 C62 C64 C63 2(13) . . . 5_566 ? C64 C62 C64 C63 1(6) 5_566 . . 5_566 ? C63 C62 C64 C62 1(6) . . . 5_566 ? C63 C62 C64 C62 -1(6) 5_566 . . 5_566 ? C64 C62 C64 C62 0.000(4) 5_566 . . 5_566 ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.699 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.125