data_03014 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H92 F6 N4 O9 S2 Ti2' _chemical_formula_weight 1335.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ti' 'Ti' 0.2776 0.4457 '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' 'F' 'F' 0.0171 0.0103 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1bar' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9302(14) _cell_length_b 13.0118(15) _cell_length_c 13.3215(18) _cell_angle_alpha 95.210(4) _cell_angle_beta 110.847(3) _cell_angle_gamma 106.869(4) _cell_volume 1654.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 898 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.37 _exptl_crystal_description 'needle fragment' _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 706 _exptl_absorpt_coefficient_mu 0.378 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9282 _exptl_absorpt_correction_T_max 0.9350 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details ' 0.30 degree frames measured for 5.17 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 17481 _diffrn_reflns_av_R_equivalents 0.0806 _diffrn_reflns_av_sigmaI/netI 0.0819 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7525 _reflns_number_gt 5660 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local package)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1374P)^2^+3.7348P] 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 7525 _refine_ls_number_parameters 479 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1018 _refine_ls_R_factor_gt 0.0822 _refine_ls_wR_factor_ref 0.2609 _refine_ls_wR_factor_gt 0.2484 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.12446(7) 0.07252(6) 0.08059(5) 0.0196(2) Uani 1 1 d . . . O2 O -0.0051(3) -0.0543(2) 0.0705(2) 0.0268(6) Uani 1 1 d . . . N3 N 0.2686(3) 0.0814(3) 0.2364(2) 0.0181(6) Uani 1 1 d . . . C4 C 0.4079(4) 0.1198(3) 0.2630(3) 0.0222(8) Uani 1 1 d . . . C5 C 0.4694(4) 0.1878(3) 0.2085(3) 0.0241(8) Uani 1 1 d . . . H42 H 0.5639 0.1959 0.2240 0.029 Uiso 1 1 calc R . . C6 C 0.4126(4) 0.2472(3) 0.1332(3) 0.0240(8) Uani 1 1 d . . . N7 N 0.2768(3) 0.2275(3) 0.0816(2) 0.0200(6) Uani 1 1 d . . . C8 C 0.2281(4) 0.0327(3) 0.3193(3) 0.0229(8) Uani 1 1 d . . . C9 C 0.2218(4) -0.0758(3) 0.3283(3) 0.0239(8) Uani 1 1 d . . . C10 C 0.1894(5) -0.1139(4) 0.4133(3) 0.0302(9) Uani 1 1 d . . . H43 H 0.1840 -0.1869 0.4206 0.036 Uiso 1 1 calc R . . C11 C 0.1648(5) -0.0500(4) 0.4870(4) 0.0344(10) Uani 1 1 d . . . H44 H 0.1436 -0.0784 0.5445 0.041 Uiso 1 1 calc R . . C12 C 0.1713(5) 0.0544(4) 0.4764(3) 0.0348(10) Uani 1 1 d . . . H45 H 0.1536 0.0982 0.5269 0.042 Uiso 1 1 calc R . . C13 C 0.2032(4) 0.0988(4) 0.3938(3) 0.0270(8) Uani 1 1 d . . . C14 C 0.2224(5) 0.2184(4) 0.3933(3) 0.0324(10) Uani 1 1 d . . . H46 H 0.2105 0.2289 0.3174 0.039 Uiso 1 1 calc R . . C15 C 0.1149(8) 0.2535(6) 0.4211(6) 0.0589(17) Uani 1 1 d . . . H48 H 0.1280 0.2483 0.4969 0.088 Uiso 1 1 calc R . . H47 H 0.0208 0.2052 0.3706 0.088 Uiso 1 1 calc R . . H49 H 0.1267 0.3296 0.4137 0.088 Uiso 1 1 calc R . . C16 C 0.3691(7) 0.2907(5) 0.4714(6) 0.0613(17) Uani 1 1 d . . . H50 H 0.3862 0.2776 0.5457 0.092 Uiso 1 1 calc R . . H51 H 0.3793 0.3682 0.4722 0.092 Uiso 1 1 calc R . . H52 H 0.4366 0.2731 0.4469 0.092 Uiso 1 1 calc R . . C17 C 0.2476(4) -0.1522(3) 0.2515(3) 0.0264(8) Uani 1 1 d . . . H15 H 0.2789 -0.1104 0.2004 0.032 Uiso 1 1 calc R . . C18 C 0.3595(5) -0.1988(4) 0.3138(4) 0.0373(10) Uani 1 1 d . . . H26A H 0.4439 -0.1382 0.3637 0.056 Uiso 1 1 calc R . . H26B H 0.3815 -0.2397 0.2611 0.056 Uiso 1 1 calc R . . H26C H 0.3245 -0.2482 0.3564 0.056 Uiso 1 1 calc R . . C19 C 0.1129(5) -0.2482(4) 0.1836(4) 0.0343(10) Uani 1 1 d . . . H31A H 0.0803 -0.2889 0.2329 0.051 Uiso 1 1 calc R . . H31B H 0.1302 -0.2973 0.1341 0.051 Uiso 1 1 calc R . . H31C H 0.0416 -0.2200 0.1401 0.051 Uiso 1 1 calc R . . C20 C 0.5084(4) 0.0937(4) 0.3609(4) 0.0353(10) Uani 1 1 d . . . H54 H 0.4851 0.1055 0.4246 0.053 Uiso 1 1 calc R . . H55 H 0.6040 0.1420 0.3782 0.053 Uiso 1 1 calc R . . H53 H 0.5011 0.0168 0.3432 0.053 Uiso 1 1 calc R . . C21 C 0.5203(5) 0.3421(4) 0.1196(4) 0.0386(11) Uani 1 1 d . . . H57 H 0.5525 0.3148 0.0662 0.058 Uiso 1 1 calc R . . H56 H 0.5997 0.3760 0.1906 0.058 Uiso 1 1 calc R . . H58 H 0.4785 0.3968 0.0932 0.058 Uiso 1 1 calc R . . C22 C 0.2428(4) 0.3096(3) 0.0205(3) 0.0243(8) Uani 1 1 d . . . C23 C 0.2171(4) 0.3955(3) 0.0719(3) 0.0276(9) Uani 1 1 d . . . C24 C 0.1926(5) 0.4776(4) 0.0156(4) 0.0333(10) Uani 1 1 d . . . H59 H 0.1725 0.5350 0.0485 0.040 Uiso 1 1 calc R . . C25 C 0.1969(5) 0.4775(4) -0.0860(4) 0.0388(11) Uani 1 1 d . . . H60 H 0.1809 0.5347 -0.1227 0.047 Uiso 1 1 calc R . . C26 C 0.2249(4) 0.3933(4) -0.1348(4) 0.0323(10) Uani 1 1 d . . . H61 H 0.2291 0.3940 -0.2047 0.039 Uiso 1 1 calc R . . C27 C 0.2470(4) 0.3082(4) -0.0840(3) 0.0280(9) Uani 1 1 d . . . C28 C 0.2773(5) 0.2193(4) -0.1432(4) 0.0327(10) Uani 1 1 d . . . H62 H 0.2965 0.1666 -0.0947 0.039 Uiso 1 1 calc R . . C29 C 0.4034(6) 0.2668(6) -0.1720(5) 0.0525(15) Uani 1 1 d . . . H64 H 0.3803 0.3097 -0.2283 0.079 Uiso 1 1 calc R . . H65 H 0.4274 0.2065 -0.2003 0.079 Uiso 1 1 calc R . . H63 H 0.4831 0.3145 -0.1059 0.079 Uiso 1 1 calc R . . C30 C 0.1506(5) 0.1566(4) -0.2500(4) 0.0376(11) Uani 1 1 d . . . H67 H 0.0697 0.1228 -0.2332 0.056 Uiso 1 1 calc R . . H68 H 0.1706 0.0991 -0.2875 0.056 Uiso 1 1 calc R . . H66 H 0.1304 0.2077 -0.2980 0.056 Uiso 1 1 calc R . . C31 C 0.2232(5) 0.4051(4) 0.1883(4) 0.0330(10) Uani 1 1 d . . . H27 H 0.2107 0.3307 0.2061 0.040 Uiso 1 1 calc R . . C32 C 0.1101(6) 0.4416(5) 0.2015(5) 0.0453(12) Uani 1 1 d . . . H33A H 0.1300 0.5194 0.1983 0.068 Uiso 1 1 calc R . . H33B H 0.1068 0.4318 0.2727 0.068 Uiso 1 1 calc R . . H33C H 0.0200 0.3974 0.1421 0.068 Uiso 1 1 calc R . . C33 C 0.3675(6) 0.4834(5) 0.2696(4) 0.0537(15) Uani 1 1 d . . . H40A H 0.3831 0.5568 0.2531 0.080 Uiso 1 1 calc R . . H40B H 0.4394 0.4560 0.2631 0.080 Uiso 1 1 calc R . . H40C H 0.3721 0.4876 0.3448 0.080 Uiso 1 1 calc R . . O34 O 0.2210(3) -0.0156(2) 0.0137(2) 0.0261(6) Uani 1 1 d . . . S35 S 0.15159(18) -0.08740(17) -0.09695(18) 0.0179(4) Uani 0.50 1 d P . . O36 O 0.1887(12) -0.0496(9) -0.1838(9) 0.079(5) Uani 0.50 1 d P . . O37 O 0.0008(3) -0.1538(3) -0.1168(3) 0.0390(9) Uani 1 1 d . . . C38 C 0.2351(9) -0.1914(8) -0.0733(8) 0.0290(18) Uani 0.50 1 d P . . F39 F 0.3718(6) -0.1383(6) -0.0375(6) 0.0517(18) Uani 0.50 1 d P . . F40 F 0.1925(6) -0.2604(5) -0.1678(5) 0.0303(11) Uani 0.50 1 d P . . F41 F 0.204(2) -0.2454(13) -0.0038(14) 0.053(4) Uani 0.50 1 d P . . C1S C 0.2704(19) 0.5971(14) 0.5405(13) 0.062(4) Uani 0.50 1 d P . . C2S C 0.1736(14) 0.5323(12) 0.5846(9) 0.049(3) Uani 0.50 1 d P . . O3S O 0.0333(9) 0.4933(9) 0.5004(9) 0.046(2) Uani 0.50 1 d P . . C4S C -0.0671(17) 0.4262(12) 0.5342(12) 0.066(4) Uani 0.50 1 d P . . C5S C -0.2093(19) 0.3963(17) 0.4481(19) 0.080(6) Uani 0.50 1 d P . . S35A S 0.14976(19) -0.13254(19) -0.05505(17) 0.0207(4) Uani 0.50 1 d P . . O36A O 0.194(3) -0.2149(15) -0.009(2) 0.062(6) Uani 0.50 1 d P . . C38A C 0.2116(14) -0.1171(11) -0.1645(10) 0.056(4) Uani 0.50 1 d P . . F39A F 0.3421(10) -0.0631(9) -0.1270(10) 0.113(5) Uani 0.50 1 d P . . F40A F 0.1827(6) -0.2170(6) -0.2225(6) 0.0452(16) Uani 0.50 1 d P . . F41A F 0.1394(14) -0.0619(9) -0.2269(10) 0.073(3) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0103(3) 0.0213(4) 0.0193(3) -0.0100(2) 0.0029(2) 0.0023(2) O2 0.0179(13) 0.0314(16) 0.0207(13) 0.0088(12) 0.0024(11) -0.0003(11) N3 0.0137(14) 0.0180(15) 0.0156(14) -0.0037(11) 0.0017(11) 0.0032(11) C4 0.0160(17) 0.0215(18) 0.0203(17) -0.0056(14) 0.0004(14) 0.0056(14) C5 0.0130(16) 0.027(2) 0.0237(18) -0.0056(15) 0.0037(14) 0.0036(15) C6 0.0195(18) 0.026(2) 0.0191(17) -0.0046(15) 0.0071(14) 0.0012(15) N7 0.0146(14) 0.0221(16) 0.0163(14) -0.0027(12) 0.0032(11) 0.0023(12) C8 0.0194(18) 0.026(2) 0.0141(16) 0.0004(14) 0.0006(14) 0.0034(15) C9 0.0186(18) 0.027(2) 0.0188(17) 0.0011(15) 0.0019(14) 0.0056(15) C10 0.027(2) 0.035(2) 0.026(2) 0.0132(18) 0.0062(17) 0.0102(18) C11 0.031(2) 0.052(3) 0.024(2) 0.016(2) 0.0135(18) 0.016(2) C12 0.043(3) 0.044(3) 0.0200(19) 0.0079(18) 0.0125(18) 0.019(2) C13 0.028(2) 0.032(2) 0.0164(17) 0.0005(15) 0.0036(15) 0.0107(17) C14 0.044(3) 0.032(2) 0.0186(18) -0.0006(16) 0.0097(18) 0.016(2) C15 0.087(5) 0.059(4) 0.067(4) 0.023(3) 0.050(4) 0.049(4) C16 0.057(4) 0.032(3) 0.064(4) -0.014(3) 0.001(3) 0.009(3) C17 0.024(2) 0.024(2) 0.0254(19) 0.0037(16) 0.0066(16) 0.0051(16) C18 0.032(2) 0.041(3) 0.040(3) 0.012(2) 0.013(2) 0.016(2) C19 0.031(2) 0.026(2) 0.036(2) 0.0023(18) 0.0086(19) 0.0039(18) C20 0.0146(18) 0.039(3) 0.039(2) 0.012(2) -0.0013(17) 0.0045(17) C21 0.0165(19) 0.048(3) 0.037(2) 0.013(2) 0.0045(17) -0.0028(19) C22 0.0155(17) 0.0228(19) 0.0232(18) 0.0028(15) 0.0028(14) -0.0027(14) C23 0.0235(19) 0.0203(19) 0.028(2) 0.0006(16) 0.0062(16) -0.0015(15) C24 0.027(2) 0.023(2) 0.042(2) 0.0046(18) 0.0098(19) 0.0022(17) C25 0.029(2) 0.033(2) 0.046(3) 0.021(2) 0.009(2) 0.0025(19) C26 0.023(2) 0.039(2) 0.029(2) 0.0120(19) 0.0093(17) 0.0027(18) C27 0.0181(18) 0.033(2) 0.0250(19) 0.0061(17) 0.0065(15) 0.0005(16) C28 0.030(2) 0.044(3) 0.025(2) 0.0103(19) 0.0122(17) 0.011(2) C29 0.042(3) 0.071(4) 0.050(3) 0.013(3) 0.028(3) 0.015(3) C30 0.039(3) 0.049(3) 0.024(2) 0.008(2) 0.0113(19) 0.015(2) C31 0.043(3) 0.021(2) 0.031(2) 0.0002(17) 0.0136(19) 0.0070(18) C32 0.057(3) 0.035(3) 0.048(3) 0.004(2) 0.029(3) 0.013(2) C33 0.048(3) 0.056(4) 0.035(3) -0.015(2) 0.005(2) 0.008(3) O34 0.0110(12) 0.0306(16) 0.0260(14) -0.0134(12) 0.0026(10) 0.0042(11) S35 0.0109(8) 0.0168(9) 0.0203(9) -0.0087(8) 0.0035(7) 0.0038(7) O36 0.057(6) 0.024(5) 0.061(7) 0.013(4) -0.053(5) -0.022(4) O37 0.0134(14) 0.0403(18) 0.0434(18) -0.0289(15) 0.0009(12) 0.0058(13) C38 0.026(4) 0.027(4) 0.028(4) -0.004(4) 0.005(3) 0.010(3) F39 0.021(3) 0.049(4) 0.067(4) -0.024(3) 0.002(3) 0.015(3) F40 0.035(3) 0.030(3) 0.027(3) -0.008(2) 0.013(2) 0.015(2) F41 0.092(7) 0.038(8) 0.032(4) 0.006(4) 0.028(5) 0.021(6) C1S 0.051(9) 0.057(9) 0.055(8) -0.010(6) 0.022(7) -0.007(8) C2S 0.063(8) 0.055(7) 0.030(5) 0.000(5) 0.016(5) 0.026(6) O3S 0.050(7) 0.032(4) 0.038(3) -0.006(3) 0.008(5) 0.004(5) C4S 0.075(9) 0.057(8) 0.068(8) -0.003(7) 0.040(8) 0.018(7) C5S 0.044(9) 0.062(11) 0.094(14) -0.013(9) 0.010(9) -0.006(8) S35A 0.0153(9) 0.0229(10) 0.0192(9) -0.0058(8) 0.0044(7) 0.0064(8) O36A 0.065(8) 0.040(11) 0.041(6) -0.006(7) -0.004(6) -0.004(8) C38A 0.058(7) 0.042(7) 0.049(6) -0.028(5) 0.036(6) -0.019(6) F39A 0.077(6) 0.101(7) 0.132(8) -0.072(7) 0.085(6) -0.034(5) F40A 0.041(3) 0.048(4) 0.042(4) -0.025(3) 0.022(3) 0.013(3) F41A 0.110(9) 0.065(7) 0.095(8) 0.045(6) 0.072(7) 0.053(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O2 1.793(3) . ? Ti1 O2 1.917(3) 2 ? Ti1 N3 2.080(3) . ? Ti1 O34 2.099(3) . ? Ti1 O37 2.108(3) 2 ? Ti1 N7 2.207(3) . ? Ti1 Ti1 2.7751(13) 2 ? O2 Ti1 1.917(3) 2 ? N3 C4 1.355(5) . ? N3 C8 1.459(5) . ? C4 C5 1.372(6) . ? C4 C20 1.517(6) . ? C5 C6 1.401(6) . ? C6 N7 1.328(5) . ? C6 C21 1.514(6) . ? N7 C22 1.454(5) . ? C8 C13 1.404(6) . ? C8 C9 1.412(6) . ? C9 C10 1.392(6) . ? C9 C17 1.516(6) . ? C10 C11 1.378(7) . ? C11 C12 1.363(7) . ? C12 C13 1.393(6) . ? C13 C14 1.510(6) . ? C14 C16 1.516(8) . ? C14 C15 1.522(7) . ? C17 C19 1.525(6) . ? C17 C18 1.533(6) . ? C22 C23 1.406(6) . ? C22 C27 1.407(6) . ? C23 C24 1.394(6) . ? C23 C31 1.520(6) . ? C24 C25 1.372(7) . ? C25 C26 1.387(8) . ? C26 C27 1.384(6) . ? C27 C28 1.522(7) . ? C28 C30 1.529(7) . ? C28 C29 1.535(7) . ? C31 C32 1.505(7) . ? C31 C33 1.533(7) . ? O34 S35 1.471(3) . ? O34 S35A 1.521(3) . ? S35 O36 1.437(15) . ? S35 O37 1.534(4) . ? S35 C38 1.831(9) . ? O37 S35A 1.466(3) . ? O37 Ti1 2.108(3) 2 ? C38 F41 1.29(2) . ? C38 F40 1.320(10) . ? C38 F39 1.331(11) . ? C1S C5S 0.76(2) 2_566 ? C1S C2S 1.48(2) . ? C1S C4S 2.00(3) 2_566 ? C2S C5S 1.09(2) 2_566 ? C2S O3S 1.445(15) . ? C2S C4S 1.83(2) 2_566 ? O3S O3S 0.793(15) 2_566 ? O3S C4S 1.196(18) 2_566 ? O3S C4S 1.428(19) . ? O3S C5S 1.87(2) 2_566 ? C4S O3S 1.196(18) 2_566 ? C4S C5S 1.48(2) . ? C4S C2S 1.83(2) 2_566 ? C4S C1S 2.00(3) 2_566 ? C5S C1S 0.76(2) 2_566 ? C5S C2S 1.09(2) 2_566 ? C5S O3S 1.87(2) 2_566 ? S35A O36A 1.40(2) . ? S35A C38A 1.816(11) . ? C38A F39A 1.275(14) . ? C38A F40A 1.339(13) . ? C38A F41A 1.341(19) . ? 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 O2 83.22(12) . 2 ? O2 Ti1 N3 97.17(12) . . ? O2 Ti1 N3 172.23(13) 2 . ? O2 Ti1 O34 89.89(13) . . ? O2 Ti1 O34 83.73(12) 2 . ? N3 Ti1 O34 88.50(12) . . ? O2 Ti1 O37 87.42(14) . 2 ? O2 Ti1 O37 85.48(13) 2 2 ? N3 Ti1 O37 102.29(13) . 2 ? O34 Ti1 O37 169.12(12) . 2 ? O2 Ti1 N7 176.32(12) . . ? O2 Ti1 N7 93.13(12) 2 . ? N3 Ti1 N7 86.40(12) . . ? O34 Ti1 N7 89.30(12) . . ? O37 Ti1 N7 92.71(13) 2 . ? O2 Ti1 Ti1 43.30(9) . 2 ? O2 Ti1 Ti1 39.91(8) 2 2 ? N3 Ti1 Ti1 139.90(10) . 2 ? O34 Ti1 Ti1 85.60(8) . 2 ? O37 Ti1 Ti1 85.21(8) 2 2 ? N7 Ti1 Ti1 133.04(9) . 2 ? Ti1 O2 Ti1 96.78(12) . 2 ? C4 N3 C8 114.7(3) . . ? C4 N3 Ti1 121.9(3) . . ? C8 N3 Ti1 122.8(2) . . ? N3 C4 C5 123.7(4) . . ? N3 C4 C20 121.1(4) . . ? C5 C4 C20 115.1(4) . . ? C4 C5 C6 129.3(4) . . ? N7 C6 C5 124.1(4) . . ? N7 C6 C21 121.6(4) . . ? C5 C6 C21 114.2(4) . . ? C6 N7 C22 114.4(3) . . ? C6 N7 Ti1 120.0(3) . . ? C22 N7 Ti1 125.4(2) . . ? C13 C8 C9 120.9(4) . . ? C13 C8 N3 118.1(4) . . ? C9 C8 N3 120.9(3) . . ? C10 C9 C8 117.2(4) . . ? C10 C9 C17 118.7(4) . . ? C8 C9 C17 124.1(4) . . ? C11 C10 C9 122.6(4) . . ? C12 C11 C10 119.0(4) . . ? C11 C12 C13 122.0(4) . . ? C12 C13 C8 118.3(4) . . ? C12 C13 C14 119.2(4) . . ? C8 C13 C14 122.3(4) . . ? C13 C14 C16 110.2(4) . . ? C13 C14 C15 112.6(4) . . ? C16 C14 C15 110.6(5) . . ? C9 C17 C19 109.8(4) . . ? C9 C17 C18 112.3(4) . . ? C19 C17 C18 108.4(4) . . ? C23 C22 C27 120.7(4) . . ? C23 C22 N7 118.4(3) . . ? C27 C22 N7 120.7(4) . . ? C24 C23 C22 118.3(4) . . ? C24 C23 C31 119.2(4) . . ? C22 C23 C31 122.4(4) . . ? C25 C24 C23 121.6(5) . . ? C24 C25 C26 119.4(4) . . ? C27 C26 C25 121.6(4) . . ? C26 C27 C22 118.4(4) . . ? C26 C27 C28 118.2(4) . . ? C22 C27 C28 123.4(4) . . ? C27 C28 C30 109.9(4) . . ? C27 C28 C29 112.2(4) . . ? C30 C28 C29 108.1(4) . . ? C32 C31 C23 113.0(4) . . ? C32 C31 C33 110.5(4) . . ? C23 C31 C33 109.7(4) . . ? S35 O34 S35A 32.83(11) . . ? S35 O34 Ti1 123.47(17) . . ? S35A O34 Ti1 124.89(17) . . ? O36 S35 O34 119.0(4) . . ? O36 S35 O37 122.0(4) . . ? O34 S35 O37 109.0(2) . . ? O36 S35 C38 100.0(7) . . ? O34 S35 C38 100.0(3) . . ? O37 S35 C38 101.8(3) . . ? S35A O37 S35 32.70(12) . . ? S35A O37 Ti1 127.93(19) . 2 ? S35 O37 Ti1 119.6(2) . 2 ? F41 C38 F40 109.3(10) . . ? F41 C38 F39 111.8(12) . . ? F40 C38 F39 108.8(7) . . ? F41 C38 S35 111.2(10) . . ? F40 C38 S35 108.9(6) . . ? F39 C38 S35 106.7(6) . . ? C5S C1S C2S 45(2) 2_566 . ? C5S C1S C4S 38(2) 2_566 2_566 ? C2S C1S C4S 61.4(9) . 2_566 ? C5S C2S O3S 94.2(14) 2_566 . ? C5S C2S C1S 29.9(14) 2_566 . ? O3S C2S C1S 109.0(11) . . ? C5S C2S C4S 53.7(12) 2_566 2_566 ? O3S C2S C4S 40.6(7) . 2_566 ? C1S C2S C4S 73.4(11) . 2_566 ? O3S O3S C4S 89.4(18) 2_566 2_566 ? O3S O3S C4S 56.9(15) 2_566 . ? C4S O3S C4S 146.3(8) 2_566 . ? O3S O3S C2S 129.6(18) 2_566 . ? C4S O3S C2S 87.4(11) 2_566 . ? C4S O3S C2S 113.1(11) . . ? O3S O3S C5S 121.5(19) 2_566 2_566 ? C4S O3S C5S 52.0(12) 2_566 2_566 ? C4S O3S C5S 143.7(12) . 2_566 ? C2S O3S C5S 35.5(9) . 2_566 ? O3S C4S O3S 33.7(8) 2_566 . ? O3S C4S C5S 88.4(15) 2_566 . ? O3S C4S C5S 110.4(15) . . ? O3S C4S C2S 51.9(9) 2_566 2_566 ? O3S C4S C2S 76.5(9) . 2_566 ? C5S C4S C2S 36.5(10) . 2_566 ? O3S C4S C1S 93.0(12) 2_566 2_566 ? O3S C4S C1S 121.6(12) . 2_566 ? C5S C4S C1S 18.6(11) . 2_566 ? C2S C4S C1S 45.2(8) 2_566 2_566 ? C1S C5S C2S 105(3) 2_566 2_566 ? C1S C5S C4S 123(3) 2_566 . ? C2S C5S C4S 89.8(15) 2_566 . ? C1S C5S O3S 124(3) 2_566 2_566 ? C2S C5S O3S 50.3(10) 2_566 2_566 ? C4S C5S O3S 39.6(8) . 2_566 ? O36A S35A O37 120.0(10) . . ? O36A S35A O34 117.6(9) . . ? O37 S35A O34 110.1(2) . . ? O36A S35A C38A 104.8(14) . . ? O37 S35A C38A 100.3(5) . . ? O34 S35A C38A 100.0(4) . . ? F39A C38A F40A 110.2(11) . . ? F39A C38A F41A 110.2(14) . . ? F40A C38A F41A 110.6(11) . . ? F39A C38A S35A 111.8(9) . . ? F40A C38A S35A 108.9(9) . . ? F41A C38A S35A 105.0(9) . . ? 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 O2 Ti1 0.0 2 . . 2 ? N3 Ti1 O2 Ti1 -172.18(13) . . . 2 ? O34 Ti1 O2 Ti1 -83.70(14) . . . 2 ? O37 Ti1 O2 Ti1 85.75(15) 2 . . 2 ? N7 Ti1 O2 Ti1 -6(2) . . . 2 ? O2 Ti1 N3 C4 142.5(3) . . . . ? O2 Ti1 N3 C4 50.1(11) 2 . . . ? O34 Ti1 N3 C4 52.8(3) . . . . ? O37 Ti1 N3 C4 -128.6(3) 2 . . . ? N7 Ti1 N3 C4 -36.6(3) . . . . ? Ti1 Ti1 N3 C4 134.1(3) 2 . . . ? O2 Ti1 N3 C8 -28.4(3) . . . . ? O2 Ti1 N3 C8 -120.7(9) 2 . . . ? O34 Ti1 N3 C8 -118.1(3) . . . . ? O37 Ti1 N3 C8 60.5(3) 2 . . . ? N7 Ti1 N3 C8 152.5(3) . . . . ? Ti1 Ti1 N3 C8 -36.7(4) 2 . . . ? C8 N3 C4 C5 -166.0(4) . . . . ? Ti1 N3 C4 C5 22.5(5) . . . . ? C8 N3 C4 C20 10.9(5) . . . . ? Ti1 N3 C4 C20 -160.6(3) . . . . ? N3 C4 C5 C6 13.2(7) . . . . ? C20 C4 C5 C6 -163.8(4) . . . . ? C4 C5 C6 N7 -16.6(7) . . . . ? C4 C5 C6 C21 159.9(4) . . . . ? C5 C6 N7 C22 171.0(4) . . . . ? C21 C6 N7 C22 -5.2(5) . . . . ? C5 C6 N7 Ti1 -14.6(5) . . . . ? C21 C6 N7 Ti1 169.2(3) . . . . ? O2 Ti1 N7 C6 -133(2) . . . . ? O2 Ti1 N7 C6 -139.3(3) 2 . . . ? N3 Ti1 N7 C6 32.9(3) . . . . ? O34 Ti1 N7 C6 -55.6(3) . . . . ? O37 Ti1 N7 C6 135.1(3) 2 . . . ? Ti1 Ti1 N7 C6 -138.9(2) 2 . . . ? O2 Ti1 N7 C22 41(2) . . . . ? O2 Ti1 N7 C22 34.5(3) 2 . . . ? N3 Ti1 N7 C22 -153.3(3) . . . . ? O34 Ti1 N7 C22 118.2(3) . . . . ? O37 Ti1 N7 C22 -51.1(3) 2 . . . ? Ti1 Ti1 N7 C22 34.8(4) 2 . . . ? C4 N3 C8 C13 96.6(4) . . . . ? Ti1 N3 C8 C13 -91.9(4) . . . . ? C4 N3 C8 C9 -79.9(4) . . . . ? Ti1 N3 C8 C9 91.5(4) . . . . ? C13 C8 C9 C10 0.3(6) . . . . ? N3 C8 C9 C10 176.7(3) . . . . ? C13 C8 C9 C17 -179.9(4) . . . . ? N3 C8 C9 C17 -3.4(6) . . . . ? C8 C9 C10 C11 -0.4(6) . . . . ? C17 C9 C10 C11 179.8(4) . . . . ? C9 C10 C11 C12 0.5(7) . . . . ? C10 C11 C12 C13 -0.6(7) . . . . ? C11 C12 C13 C8 0.5(7) . . . . ? C11 C12 C13 C14 -174.1(4) . . . . ? C9 C8 C13 C12 -0.3(6) . . . . ? N3 C8 C13 C12 -176.9(4) . . . . ? C9 C8 C13 C14 174.1(4) . . . . ? N3 C8 C13 C14 -2.4(6) . . . . ? C12 C13 C14 C16 82.5(6) . . . . ? C8 C13 C14 C16 -91.9(5) . . . . ? C12 C13 C14 C15 -41.5(6) . . . . ? C8 C13 C14 C15 144.1(5) . . . . ? C10 C9 C17 C19 66.8(5) . . . . ? C8 C9 C17 C19 -113.1(4) . . . . ? C10 C9 C17 C18 -53.9(5) . . . . ? C8 C9 C17 C18 126.3(4) . . . . ? C6 N7 C22 C23 -95.1(4) . . . . ? Ti1 N7 C22 C23 90.9(4) . . . . ? C6 N7 C22 C27 79.7(5) . . . . ? Ti1 N7 C22 C27 -94.4(4) . . . . ? C27 C22 C23 C24 1.6(6) . . . . ? N7 C22 C23 C24 176.3(3) . . . . ? C27 C22 C23 C31 -175.0(4) . . . . ? N7 C22 C23 C31 -0.3(6) . . . . ? C22 C23 C24 C25 -1.8(6) . . . . ? C31 C23 C24 C25 174.8(4) . . . . ? C23 C24 C25 C26 0.7(7) . . . . ? C24 C25 C26 C27 0.8(7) . . . . ? C25 C26 C27 C22 -1.1(6) . . . . ? C25 C26 C27 C28 -179.9(4) . . . . ? C23 C22 C27 C26 -0.1(6) . . . . ? N7 C22 C27 C26 -174.8(3) . . . . ? C23 C22 C27 C28 178.6(4) . . . . ? N7 C22 C27 C28 4.0(6) . . . . ? C26 C27 C28 C30 -64.3(5) . . . . ? C22 C27 C28 C30 116.9(4) . . . . ? C26 C27 C28 C29 56.1(5) . . . . ? C22 C27 C28 C29 -122.7(5) . . . . ? C24 C23 C31 C32 43.1(6) . . . . ? C22 C23 C31 C32 -140.4(4) . . . . ? C24 C23 C31 C33 -80.7(6) . . . . ? C22 C23 C31 C33 95.8(5) . . . . ? O2 Ti1 O34 S35 61.4(3) . . . . ? O2 Ti1 O34 S35 -21.8(2) 2 . . . ? N3 Ti1 O34 S35 158.6(3) . . . . ? O37 Ti1 O34 S35 -14.2(9) 2 . . . ? N7 Ti1 O34 S35 -115.0(3) . . . . ? Ti1 Ti1 O34 S35 18.3(2) 2 . . . ? O2 Ti1 O34 S35A 21.5(3) . . . . ? O2 Ti1 O34 S35A -61.7(2) 2 . . . ? N3 Ti1 O34 S35A 118.6(3) . . . . ? O37 Ti1 O34 S35A -54.2(8) 2 . . . ? N7 Ti1 O34 S35A -154.9(2) . . . . ? Ti1 Ti1 O34 S35A -21.7(2) 2 . . . ? S35A O34 S35 O36 -151.5(7) . . . . ? Ti1 O34 S35 O36 104.6(7) . . . . ? S35A O34 S35 O37 62.2(2) . . . . ? Ti1 O34 S35 O37 -41.7(3) . . . . ? S35A O34 S35 C38 -44.1(4) . . . . ? Ti1 O34 S35 C38 -148.0(4) . . . . ? O36 S35 O37 S35A 147.8(7) . . . . ? O34 S35 O37 S35A -67.1(3) . . . . ? C38 S35 O37 S35A 38.0(3) . . . . ? O36 S35 O37 Ti1 -97.0(7) . . . 2 ? O34 S35 O37 Ti1 48.0(3) . . . 2 ? C38 S35 O37 Ti1 153.1(3) . . . 2 ? O36 S35 C38 F41 -173.8(11) . . . . ? O34 S35 C38 F41 64.2(11) . . . . ? O37 S35 C38 F41 -47.9(11) . . . . ? O36 S35 C38 F40 -53.3(7) . . . . ? O34 S35 C38 F40 -175.4(6) . . . . ? O37 S35 C38 F40 72.6(7) . . . . ? O36 S35 C38 F39 64.0(7) . . . . ? O34 S35 C38 F39 -58.1(7) . . . . ? O37 S35 C38 F39 -170.1(6) . . . . ? C4S C1S C2S C5S -44(3) 2_566 . . 2_566 ? C5S C1S C2S O3S 64(3) 2_566 . . . ? C4S C1S C2S O3S 19.8(9) 2_566 . . . ? C5S C1S C2S C4S 44(3) 2_566 . . 2_566 ? C5S C2S O3S O3S -90(3) 2_566 . . 2_566 ? C1S C2S O3S O3S -117(3) . . . 2_566 ? C4S C2S O3S O3S -87(3) 2_566 . . 2_566 ? C5S C2S O3S C4S -3.3(16) 2_566 . . 2_566 ? C1S C2S O3S C4S -29.9(13) . . . 2_566 ? C5S C2S O3S C4S -155.7(16) 2_566 . . . ? C1S C2S O3S C4S 177.8(12) . . . . ? C4S C2S O3S C4S -152.3(10) 2_566 . . . ? C1S C2S O3S C5S -26.6(14) . . . 2_566 ? C4S C2S O3S C5S 3.3(16) 2_566 . . 2_566 ? C4S O3S C4S O3S 0.000(4) 2_566 . . 2_566 ? C2S O3S C4S O3S 123(2) . . . 2_566 ? C5S O3S C4S O3S 99(2) 2_566 . . 2_566 ? O3S O3S C4S C5S 52(2) 2_566 . . . ? C4S O3S C4S C5S 52(2) 2_566 . . . ? C2S O3S C4S C5S 175.6(13) . . . . ? C5S O3S C4S C5S 151.8(11) 2_566 . . . ? O3S O3S C4S C2S 38.5(15) 2_566 . . 2_566 ? C4S O3S C4S C2S 38.5(15) 2_566 . . 2_566 ? C2S O3S C4S C2S 161.9(7) . . . 2_566 ? C5S O3S C4S C2S 138.0(17) 2_566 . . 2_566 ? O3S O3S C4S C1S 35.7(19) 2_566 . . 2_566 ? C4S O3S C4S C1S 35.7(19) 2_566 . . 2_566 ? C2S O3S C4S C1S 159.0(10) . . . 2_566 ? C5S O3S C4S C1S 135.2(17) 2_566 . . 2_566 ? O3S C4S C5S C1S -104(4) 2_566 . . 2_566 ? O3S C4S C5S C1S -130(4) . . . 2_566 ? C2S C4S C5S C1S -108(4) 2_566 . . 2_566 ? O3S C4S C5S C2S 3.3(16) 2_566 . . 2_566 ? O3S C4S C5S C2S -22.8(19) . . . 2_566 ? C1S C4S C5S C2S 108(4) 2_566 . . 2_566 ? O3S C4S C5S O3S -26.1(10) . . . 2_566 ? C2S C4S C5S O3S -3.3(16) 2_566 . . 2_566 ? C1S C4S C5S O3S 104(4) 2_566 . . 2_566 ? S35 O37 S35A O36A -154.9(13) . . . . ? Ti1 O37 S35A O36A 118.4(13) 2 . . . ? S35 O37 S35A O34 63.7(2) . . . . ? Ti1 O37 S35A O34 -23.1(4) 2 . . . ? S35 O37 S35A C38A -41.0(5) . . . . ? Ti1 O37 S35A C38A -127.8(5) 2 . . . ? S35 O34 S35A O36A 148.9(14) . . . . ? Ti1 O34 S35A O36A -112.0(14) . . . . ? S35 O34 S35A O37 -68.7(3) . . . . ? Ti1 O34 S35A O37 30.5(3) . . . . ? S35 O34 S35A C38A 36.2(6) . . . . ? Ti1 O34 S35A C38A 135.4(6) . . . . ? O36A S35A C38A F39A -76.7(15) . . . . ? O37 S35A C38A F39A 158.2(12) . . . . ? O34 S35A C38A F39A 45.5(13) . . . . ? O36A S35A C38A F40A 45.3(14) . . . . ? O37 S35A C38A F40A -79.7(10) . . . . ? O34 S35A C38A F40A 167.6(9) . . . . ? O36A S35A C38A F41A 163.8(12) . . . . ? O37 S35A C38A F41A 38.8(9) . . . . ? O34 S35A C38A F41A -73.9(8) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.508 _refine_diff_density_min -0.758 _refine_diff_density_rms 0.132