# Electronic Supplementary Material (ESI) for Catalysis Science & Technology # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Cat.Sci.Tech. _journal_coden_cambridge 1486 #TrackingRef '- CIF.CIF' #SUBMISSION DETAILS: _publ_contact_author ; Wen-Hua Sun Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; loop_ _publ_author_name _publ_author_address 'Wei Huang' Wenjuan_Zhang 'Wenjuan Zhang' Chinese_Academy_of_Sciences 'Wen-Hua Sun' China 'Lin Wang' Lin_Wang C.Redshaw Chinese_Academy_of_Sciences _publ_contact_author_name 'Wen-Hua Sun' _publ_contact_author_email whsun@iccas.ac.cn data_C2 _database_code_depnum_ccdc_archive 'CCDC 869824' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H38 Cl2 N2 O Ti' _chemical_formula_weight 777.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.529(4) _cell_length_b 18.752(4) _cell_length_c 25.656(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8433(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18306 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 0.366 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8824 _exptl_absorpt_correction_T_max 0.9819 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24720 _diffrn_reflns_av_R_equivalents 0.0828 _diffrn_reflns_av_sigmaI/netI 0.0891 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.34 _reflns_number_total 7661 _reflns_number_gt 5546 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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^)+(0.1246P)^2^+15.5343P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7661 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1428 _refine_ls_R_factor_gt 0.1065 _refine_ls_wR_factor_ref 0.2817 _refine_ls_wR_factor_gt 0.2577 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _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 0.11825(6) 0.14801(5) 0.64764(4) 0.0293(3) Uani 1 1 d . . . N1 N 0.0827(3) 0.0396(2) 0.64143(17) 0.0259(11) Uani 1 1 d . . . Cl2 Cl 0.06038(9) 0.14149(8) 0.56157(6) 0.0376(4) Uani 1 1 d . . . O1 O 0.2084(2) 0.1016(2) 0.61789(16) 0.0359(10) Uani 1 1 d . . . Cl1 Cl 0.15288(8) 0.09542(8) 0.73134(6) 0.0350(4) Uani 1 1 d . . . C16 C -0.0603(3) 0.2054(3) 0.7512(2) 0.0213(11) Uani 1 1 d . . . C9 C 0.0150(3) 0.0153(3) 0.6553(2) 0.0241(12) Uani 1 1 d . . . C17 C -0.0168(3) 0.1569(3) 0.7887(2) 0.0286(13) Uani 1 1 d . . . H17A H 0.0338 0.1478 0.7720 0.034 Uiso 1 1 calc R . . N2 N -0.0087(3) 0.1339(2) 0.67792(18) 0.0250(10) Uani 1 1 d . . . C18 C -0.1203(3) 0.1967(3) 0.6074(2) 0.0292(13) Uani 1 1 d . . . H18A H -0.0677 0.1879 0.5938 0.035 Uiso 1 1 calc R . . C11 C -0.0608(3) 0.1887(3) 0.6983(2) 0.0238(12) Uani 1 1 d . . . C15 C -0.1030(3) 0.2635(3) 0.7681(2) 0.0292(13) Uani 1 1 d . . . H15A H -0.1021 0.2759 0.8039 0.035 Uiso 1 1 calc R . . C31 C -0.1611(4) 0.1242(3) 0.6068(2) 0.0341(14) Uani 1 1 d . . . C37 C -0.1570(3) 0.2510(3) 0.5706(2) 0.0282(13) Uani 1 1 d . . . C13 C -0.1522(3) 0.2812(3) 0.6823(2) 0.0268(12) Uani 1 1 d . . . H13A H -0.1856 0.3059 0.6594 0.032 Uiso 1 1 calc R . . C28 C -0.1186(4) -0.0525(3) 0.7998(3) 0.0430(17) Uani 1 1 d . . . H28A H -0.1399 -0.0990 0.8020 0.052 Uiso 1 1 calc R . . C25 C -0.0555(3) 0.0831(3) 0.7941(2) 0.0259(13) Uani 1 1 d . . . C8 C -0.0033(4) -0.0575(3) 0.6489(2) 0.0378(15) Uani 1 1 d . . . H8A H -0.0515 -0.0752 0.6597 0.045 Uiso 1 1 calc R . . C12 C -0.1104(3) 0.2240(3) 0.6635(2) 0.0248(12) Uani 1 1 d . . . C38 C -0.1183(4) 0.3134(4) 0.5592(3) 0.0403(16) Uani 1 1 d . . . H38A H -0.0694 0.3216 0.5739 0.048 Uiso 1 1 calc R . . C19 C 0.0002(4) 0.1910(3) 0.8412(2) 0.0364(15) Uani 1 1 d . . . C5 C 0.1207(4) -0.0767(3) 0.6095(3) 0.0406(16) Uani 1 1 d . . . C14 C -0.1463(3) 0.3034(3) 0.7343(2) 0.0302(13) Uani 1 1 d . . . C30 C -0.0092(4) 0.0244(3) 0.8004(3) 0.0372(15) Uani 1 1 d . . . H30A H 0.0446 0.0297 0.8029 0.045 Uiso 1 1 calc R . . C10 C -0.0350(3) 0.0698(3) 0.6762(2) 0.0216(11) Uani 1 1 d . . . H10A H -0.0849 0.0587 0.6882 0.026 Uiso 1 1 calc R . . C7 C 0.0499(4) -0.1025(3) 0.6268(3) 0.0461(18) Uani 1 1 d . . . H7A H 0.0384 -0.1518 0.6232 0.055 Uiso 1 1 calc R . . C29 C -0.0423(4) -0.0426(3) 0.8032(3) 0.0442(17) Uani 1 1 d . . . H29A H -0.0103 -0.0830 0.8077 0.053 Uiso 1 1 calc R . . C46 C 0.1149(4) 0.2563(3) 0.6953(3) 0.0482(18) Uani 1 1 d . . . H46A H 0.0881 0.2637 0.7293 0.058 Uiso 1 1 calc R . . C6 C 0.1349(4) -0.0029(3) 0.6188(2) 0.0314(14) Uani 1 1 d . . . C32 C -0.2193(4) 0.1084(3) 0.6432(3) 0.0386(15) Uani 1 1 d . . . H32A H -0.2341 0.1429 0.6684 0.046 Uiso 1 1 calc R . . C41 C -0.2599(4) 0.2913(4) 0.5157(3) 0.0490(18) Uani 1 1 d . . . H41A H -0.3090 0.2836 0.5011 0.059 Uiso 1 1 calc R . . C26 C -0.1331(3) 0.0751(3) 0.7906(2) 0.0306(13) Uani 1 1 d . . . H26A H -0.1649 0.1158 0.7866 0.037 Uiso 1 1 calc R . . C1 C 0.2041(4) 0.0321(3) 0.6061(3) 0.0406(16) Uani 1 1 d . . . C35 C -0.1760(5) 0.0072(4) 0.5700(3) 0.059(2) Uani 1 1 d . . . H35A H -0.1607 -0.0275 0.5451 0.071 Uiso 1 1 calc R . . C27 C -0.1652(4) 0.0070(3) 0.7929(3) 0.0405(16) Uani 1 1 d . . . H27A H -0.2189 0.0012 0.7897 0.049 Uiso 1 1 calc R . . C36 C -0.1409(4) 0.0725(4) 0.5705(3) 0.0443(17) Uani 1 1 d . . . H36A H -0.1022 0.0825 0.5457 0.053 Uiso 1 1 calc R . . C45 C 0.0849(4) 0.2705(3) 0.6466(3) 0.0481(19) Uani 1 1 d . . . H45A H 0.0327 0.2899 0.6396 0.058 Uiso 1 1 calc R . . C24 C -0.0522(5) 0.1877(3) 0.8828(2) 0.0457(18) Uani 1 1 d . . . H24A H -0.0992 0.1631 0.8787 0.055 Uiso 1 1 calc R . . C2 C 0.2621(4) -0.0090(4) 0.5830(3) 0.0487(18) Uani 1 1 d . . . H2A H 0.3100 0.0117 0.5745 0.058 Uiso 1 1 calc R . . C40 C -0.2213(4) 0.3526(4) 0.5044(3) 0.0490(19) Uani 1 1 d . . . H40A H -0.2430 0.3869 0.4815 0.059 Uiso 1 1 calc R . . C20 C 0.0690(4) 0.2268(4) 0.8496(3) 0.0505(19) Uani 1 1 d . . . H20A H 0.1056 0.2286 0.8223 0.061 Uiso 1 1 calc R . . C42 C -0.2279(4) 0.2394(4) 0.5488(3) 0.0468(17) Uani 1 1 d . . . H42A H -0.2550 0.1967 0.5561 0.056 Uiso 1 1 calc R . . C39 C -0.1506(4) 0.3644(4) 0.5263(3) 0.0447(17) Uani 1 1 d . . . H39A H -0.1238 0.4073 0.5190 0.054 Uiso 1 1 calc R . . C33 C -0.2553(5) 0.0414(4) 0.6420(3) 0.059(2) Uani 1 1 d . . . H33A H -0.2944 0.0309 0.6664 0.071 Uiso 1 1 calc R . . C3 C 0.2475(5) -0.0813(4) 0.5727(3) 0.057(2) Uani 1 1 d . . . H3A H 0.2867 -0.1085 0.5566 0.069 Uiso 1 1 calc R . . C34 C -0.2342(5) -0.0094(4) 0.6055(3) 0.064(2) Uani 1 1 d . . . H34A H -0.2587 -0.0546 0.6045 0.077 Uiso 1 1 calc R . . C43 C -0.1879(4) 0.3706(3) 0.7526(3) 0.0416(16) Uani 1 1 d . . . H43A H -0.1777 0.3783 0.7898 0.062 Uiso 1 1 calc R . . H43B H -0.2429 0.3647 0.7472 0.062 Uiso 1 1 calc R . . H43C H -0.1698 0.4117 0.7326 0.062 Uiso 1 1 calc R . . C23 C -0.0345(6) 0.2210(4) 0.9300(3) 0.064(2) Uani 1 1 d . . . H23A H -0.0698 0.2189 0.9581 0.076 Uiso 1 1 calc R . . C22 C 0.0326(6) 0.2563(5) 0.9362(3) 0.069(3) Uani 1 1 d . . . H22A H 0.0431 0.2789 0.9685 0.083 Uiso 1 1 calc R . . C21 C 0.0852(6) 0.2600(5) 0.8971(4) 0.075(3) Uani 1 1 d . . . H21A H 0.1320 0.2847 0.9020 0.090 Uiso 1 1 calc R . . C47 C 0.1899(5) 0.2391(4) 0.6896(4) 0.068(3) Uani 1 1 d . . . H47A H 0.2267 0.2314 0.7188 0.081 Uiso 1 1 calc R . . C44 C 0.1416(8) 0.2635(4) 0.6105(4) 0.082(3) Uani 1 1 d . . . H44A H 0.1384 0.2763 0.5727 0.099 Uiso 1 1 calc R . . C4 C 0.1797(5) -0.1153(4) 0.5846(3) 0.055(2) Uani 1 1 d . . . H4A H 0.1729 -0.1642 0.5762 0.066 Uiso 1 1 calc R . . C48 C 0.2087(6) 0.2432(5) 0.6381(6) 0.099(4) Uani 1 1 d . . . H48A H 0.2612 0.2391 0.6232 0.118 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0298(6) 0.0248(5) 0.0334(6) 0.0033(5) 0.0038(5) 0.0020(4) N1 0.028(3) 0.026(2) 0.023(2) 0.000(2) 0.001(2) 0.005(2) Cl2 0.0404(9) 0.0406(8) 0.0317(8) 0.0072(7) 0.0032(7) 0.0054(7) O1 0.035(2) 0.034(2) 0.039(2) 0.0100(19) 0.008(2) 0.0094(18) Cl1 0.0306(8) 0.0404(8) 0.0341(8) 0.0018(7) 0.0009(7) 0.0045(6) C16 0.022(3) 0.020(2) 0.023(3) -0.002(2) 0.006(2) -0.002(2) C9 0.036(3) 0.017(2) 0.019(3) 0.004(2) -0.002(2) 0.001(2) C17 0.033(3) 0.024(3) 0.029(3) -0.002(2) -0.003(3) 0.003(2) N2 0.026(3) 0.021(2) 0.028(3) 0.0010(19) 0.000(2) 0.0025(19) C18 0.029(3) 0.028(3) 0.031(3) 0.001(3) 0.007(3) 0.006(2) C11 0.026(3) 0.018(3) 0.027(3) -0.003(2) 0.007(2) -0.005(2) C15 0.034(3) 0.024(3) 0.029(3) -0.003(2) 0.000(3) -0.003(2) C31 0.040(4) 0.030(3) 0.032(3) 0.000(3) -0.010(3) 0.007(3) C37 0.029(3) 0.030(3) 0.025(3) 0.003(2) -0.005(3) 0.009(2) C13 0.029(3) 0.027(3) 0.024(3) 0.002(2) 0.000(3) 0.001(2) C28 0.043(4) 0.027(3) 0.060(5) 0.004(3) 0.005(3) -0.004(3) C25 0.031(3) 0.024(3) 0.023(3) 0.002(2) -0.005(2) 0.004(2) C8 0.044(4) 0.027(3) 0.042(4) -0.004(3) -0.006(3) -0.001(3) C12 0.030(3) 0.019(3) 0.025(3) 0.004(2) -0.004(2) -0.003(2) C38 0.036(4) 0.048(4) 0.036(4) 0.001(3) -0.007(3) -0.005(3) C19 0.047(4) 0.031(3) 0.031(3) 0.003(3) -0.008(3) 0.007(3) C5 0.055(4) 0.033(3) 0.034(4) -0.002(3) -0.003(3) 0.013(3) C14 0.028(3) 0.026(3) 0.037(3) 0.001(3) 0.004(3) 0.007(2) C30 0.030(3) 0.034(3) 0.048(4) 0.011(3) -0.003(3) 0.002(3) C10 0.024(3) 0.023(3) 0.017(3) 0.000(2) 0.001(2) 0.003(2) C7 0.070(5) 0.015(3) 0.054(4) -0.003(3) 0.000(4) 0.006(3) C29 0.044(4) 0.032(3) 0.057(4) 0.004(3) 0.005(4) 0.013(3) C46 0.059(5) 0.029(3) 0.056(5) -0.006(3) 0.007(4) -0.014(3) C6 0.043(4) 0.026(3) 0.026(3) 0.006(2) -0.001(3) 0.011(3) C32 0.039(4) 0.034(3) 0.043(4) -0.007(3) -0.006(3) -0.001(3) C41 0.045(4) 0.060(5) 0.042(4) 0.004(4) -0.010(3) 0.004(4) C26 0.029(3) 0.026(3) 0.037(3) 0.003(3) 0.003(3) 0.003(2) C1 0.047(4) 0.036(4) 0.039(4) 0.012(3) 0.009(3) 0.008(3) C35 0.071(6) 0.048(4) 0.058(5) -0.018(4) -0.003(4) -0.005(4) C27 0.034(4) 0.033(3) 0.054(4) 0.004(3) 0.009(3) -0.003(3) C36 0.050(4) 0.047(4) 0.036(4) -0.008(3) -0.007(3) -0.003(3) C45 0.054(4) 0.018(3) 0.073(5) 0.008(3) -0.015(4) -0.001(3) C24 0.081(5) 0.025(3) 0.031(4) 0.001(3) 0.010(4) 0.004(3) C2 0.043(4) 0.054(4) 0.049(4) 0.017(4) 0.012(3) 0.012(3) C40 0.050(5) 0.061(5) 0.035(4) 0.009(3) -0.005(3) 0.016(4) C20 0.050(5) 0.058(5) 0.044(4) -0.010(4) -0.009(4) 0.007(4) C42 0.048(4) 0.052(4) 0.041(4) 0.003(3) -0.010(3) -0.005(3) C39 0.054(5) 0.039(4) 0.041(4) 0.006(3) 0.001(3) -0.002(3) C33 0.061(5) 0.063(5) 0.054(5) 0.003(4) 0.001(4) -0.017(4) C3 0.066(5) 0.051(5) 0.055(5) 0.003(4) 0.011(4) 0.037(4) C34 0.088(6) 0.042(4) 0.062(5) -0.011(4) -0.001(5) -0.024(4) C43 0.050(4) 0.031(3) 0.043(4) -0.004(3) 0.000(3) 0.011(3) C23 0.111(8) 0.046(4) 0.034(4) 0.008(3) 0.005(5) 0.014(5) C22 0.117(8) 0.060(5) 0.029(4) -0.009(4) -0.014(5) 0.009(5) C21 0.084(7) 0.075(6) 0.066(6) -0.033(5) -0.038(5) 0.013(5) C47 0.050(5) 0.039(4) 0.115(8) 0.011(5) -0.025(6) -0.016(4) C44 0.152(10) 0.043(5) 0.053(5) 0.009(4) 0.033(6) -0.020(6) C4 0.075(6) 0.031(4) 0.058(5) -0.005(3) 0.007(4) 0.021(4) C48 0.058(6) 0.040(5) 0.197(14) -0.014(7) 0.066(8) -0.012(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 O1 1.959(4) . ? Ti1 N1 2.131(5) . ? Ti1 C46 2.371(7) . ? Ti1 C45 2.371(6) . ? Ti1 N2 2.372(5) . ? Ti1 C47 2.378(8) . ? Ti1 C48 2.399(8) . ? Ti1 C44 2.401(8) . ? Ti1 Cl2 2.4331(19) . ? Ti1 Cl1 2.4398(19) . ? N1 C9 1.321(7) . ? N1 C6 1.344(7) . ? O1 C1 1.339(8) . ? C16 C15 1.390(7) . ? C16 C11 1.392(7) . ? C16 C17 1.528(8) . ? C9 C8 1.412(8) . ? C9 C10 1.449(7) . ? C17 C19 1.522(8) . ? C17 C25 1.547(8) . ? C17 H17A 1.0000 . ? N2 C10 1.289(7) . ? N2 C11 1.470(7) . ? C18 C37 1.532(8) . ? C18 C31 1.535(8) . ? C18 C12 1.537(8) . ? C18 H18A 1.0000 . ? C11 C12 1.410(8) . ? C15 C14 1.373(8) . ? C15 H15A 0.9500 . ? C31 C36 1.391(9) . ? C31 C32 1.416(9) . ? C37 C42 1.381(9) . ? C37 C38 1.383(9) . ? C13 C12 1.386(8) . ? C13 C14 1.402(8) . ? C13 H13A 0.9500 . ? C28 C29 1.353(9) . ? C28 C27 1.395(9) . ? C28 H28A 0.9500 . ? C25 C26 1.370(8) . ? C25 C30 1.378(8) . ? C8 C7 1.380(9) . ? C8 H8A 0.9500 . ? C38 C39 1.394(9) . ? C38 H38A 0.9500 . ? C19 C20 1.397(10) . ? C19 C24 1.409(9) . ? C5 C7 1.405(10) . ? C5 C4 1.415(9) . ? C5 C6 1.426(8) . ? C14 C43 1.529(8) . ? C30 C29 1.385(9) . ? C30 H30A 0.9500 . ? C10 H10A 0.9500 . ? C7 H7A 0.9500 . ? C29 H29A 0.9500 . ? C46 C47 1.360(11) . ? C46 C45 1.383(10) . ? C46 H46A 1.0000 . ? C6 C1 1.417(9) . ? C32 C33 1.405(10) . ? C32 H32A 0.9500 . ? C41 C40 1.365(10) . ? C41 C42 1.407(9) . ? C41 H41A 0.9500 . ? C26 C27 1.397(8) . ? C26 H26A 0.9500 . ? C1 C2 1.408(9) . ? C35 C36 1.370(10) . ? C35 C34 1.402(11) . ? C35 H35A 0.9500 . ? C27 H27A 0.9500 . ? C36 H36A 0.9500 . ? C45 C44 1.366(12) . ? C45 H45A 1.0000 . ? C24 C23 1.398(10) . ? C24 H24A 0.9500 . ? C2 C3 1.405(10) . ? C2 H2A 0.9500 . ? C40 C39 1.379(10) . ? C40 H40A 0.9500 . ? C20 C21 1.398(10) . ? C20 H20A 0.9500 . ? C42 H42A 0.9500 . ? C39 H39A 0.9500 . ? C33 C34 1.387(11) . ? C33 H33A 0.9500 . ? C3 C4 1.383(11) . ? C3 H3A 0.9500 . ? C34 H34A 0.9500 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C23 C22 1.359(13) . ? C23 H23A 0.9500 . ? C22 C21 1.366(13) . ? C22 H22A 0.9500 . ? C21 H21A 0.9500 . ? C47 C48 1.364(15) . ? C47 H47A 1.0000 . ? C44 C48 1.424(15) . ? C44 H44A 1.0000 . ? C4 H4A 0.9500 . ? C48 H48A 1.0000 . ? 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 Ti1 N1 77.45(18) . . ? O1 Ti1 C46 127.0(2) . . ? N1 Ti1 C46 148.0(2) . . ? O1 Ti1 C45 128.7(2) . . ? N1 Ti1 C45 148.3(2) . . ? C46 Ti1 C45 33.9(2) . . ? O1 Ti1 N2 146.62(17) . . ? N1 Ti1 N2 69.17(16) . . ? C46 Ti1 N2 84.4(2) . . ? C45 Ti1 N2 83.1(2) . . ? O1 Ti1 C47 94.0(3) . . ? N1 Ti1 C47 150.8(3) . . ? C46 Ti1 C47 33.3(3) . . ? C45 Ti1 C47 55.9(3) . . ? N2 Ti1 C47 115.3(3) . . ? O1 Ti1 C48 76.0(3) . . ? N1 Ti1 C48 153.5(3) . . ? C46 Ti1 C48 55.4(3) . . ? C45 Ti1 C48 56.0(3) . . ? N2 Ti1 C48 137.4(2) . . ? C47 Ti1 C48 33.2(4) . . ? O1 Ti1 C44 96.2(3) . . ? N1 Ti1 C44 151.6(3) . . ? C46 Ti1 C44 55.7(3) . . ? C45 Ti1 C44 33.3(3) . . ? N2 Ti1 C44 113.0(3) . . ? C47 Ti1 C44 56.1(3) . . ? C48 Ti1 C44 34.5(4) . . ? O1 Ti1 Cl2 87.74(14) . . ? N1 Ti1 Cl2 76.27(13) . . ? C46 Ti1 Cl2 120.1(2) . . ? C45 Ti1 Cl2 86.30(19) . . ? N2 Ti1 Cl2 84.28(12) . . ? C47 Ti1 Cl2 131.9(2) . . ? C48 Ti1 Cl2 102.7(4) . . ? C44 Ti1 Cl2 75.9(3) . . ? O1 Ti1 Cl1 87.85(13) . . ? N1 Ti1 Cl1 75.70(13) . . ? C46 Ti1 Cl1 84.1(2) . . ? C45 Ti1 Cl1 117.6(2) . . ? N2 Ti1 Cl1 84.28(12) . . ? C47 Ti1 Cl1 76.1(2) . . ? C48 Ti1 Cl1 103.1(4) . . ? C44 Ti1 Cl1 132.2(3) . . ? Cl2 Ti1 Cl1 151.92(7) . . ? C9 N1 C6 121.5(5) . . ? C9 N1 Ti1 124.9(4) . . ? C6 N1 Ti1 113.5(4) . . ? C1 O1 Ti1 118.3(4) . . ? C15 C16 C11 118.4(5) . . ? C15 C16 C17 122.6(5) . . ? C11 C16 C17 118.9(5) . . ? N1 C9 C8 120.4(5) . . ? N1 C9 C10 113.6(5) . . ? C8 C9 C10 125.9(5) . . ? C19 C17 C16 113.9(5) . . ? C19 C17 C25 112.5(5) . . ? C16 C17 C25 111.8(5) . . ? C19 C17 H17A 106.0 . . ? C16 C17 H17A 106.0 . . ? C25 C17 H17A 106.0 . . ? C10 N2 C11 116.2(4) . . ? C10 N2 Ti1 115.4(4) . . ? C11 N2 Ti1 128.4(3) . . ? C37 C18 C31 112.7(5) . . ? C37 C18 C12 113.8(5) . . ? C31 C18 C12 110.9(5) . . ? C37 C18 H18A 106.3 . . ? C31 C18 H18A 106.3 . . ? C12 C18 H18A 106.3 . . ? C16 C11 C12 121.0(5) . . ? C16 C11 N2 120.0(5) . . ? C12 C11 N2 119.0(5) . . ? C14 C15 C16 121.9(5) . . ? C14 C15 H15A 119.0 . . ? C16 C15 H15A 119.0 . . ? C36 C31 C32 118.6(6) . . ? C36 C31 C18 120.4(6) . . ? C32 C31 C18 121.0(5) . . ? C42 C37 C38 119.2(6) . . ? C42 C37 C18 121.6(6) . . ? C38 C37 C18 119.2(5) . . ? C12 C13 C14 121.5(5) . . ? C12 C13 H13A 119.3 . . ? C14 C13 H13A 119.3 . . ? C29 C28 C27 118.6(6) . . ? C29 C28 H28A 120.7 . . ? C27 C28 H28A 120.7 . . ? C26 C25 C30 120.4(5) . . ? C26 C25 C17 121.7(5) . . ? C30 C25 C17 117.8(5) . . ? C7 C8 C9 119.1(6) . . ? C7 C8 H8A 120.5 . . ? C9 C8 H8A 120.5 . . ? C13 C12 C11 118.0(5) . . ? C13 C12 C18 121.6(5) . . ? C11 C12 C18 120.4(5) . . ? C37 C38 C39 120.6(6) . . ? C37 C38 H38A 119.7 . . ? C39 C38 H38A 119.7 . . ? C20 C19 C24 117.9(6) . . ? C20 C19 C17 120.5(6) . . ? C24 C19 C17 121.6(6) . . ? C7 C5 C4 127.7(6) . . ? C7 C5 C6 115.8(6) . . ? C4 C5 C6 116.4(7) . . ? C15 C14 C13 118.6(5) . . ? C15 C14 C43 121.3(5) . . ? C13 C14 C43 120.1(5) . . ? C25 C30 C29 118.9(6) . . ? C25 C30 H30A 120.6 . . ? C29 C30 H30A 120.6 . . ? N2 C10 C9 117.0(5) . . ? N2 C10 H10A 121.5 . . ? C9 C10 H10A 121.5 . . ? C8 C7 C5 121.1(6) . . ? C8 C7 H7A 119.5 . . ? C5 C7 H7A 119.5 . . ? C28 C29 C30 122.3(6) . . ? C28 C29 H29A 118.8 . . ? C30 C29 H29A 118.8 . . ? C47 C46 C45 108.4(8) . . ? C47 C46 Ti1 73.6(5) . . ? C45 C46 Ti1 73.1(4) . . ? C47 C46 H46A 125.5 . . ? C45 C46 H46A 125.5 . . ? Ti1 C46 H46A 125.5 . . ? N1 C6 C1 114.0(5) . . ? N1 C6 C5 122.0(6) . . ? C1 C6 C5 124.0(6) . . ? C33 C32 C31 119.8(6) . . ? C33 C32 H32A 120.1 . . ? C31 C32 H32A 120.1 . . ? C40 C41 C42 120.9(7) . . ? C40 C41 H41A 119.6 . . ? C42 C41 H41A 119.6 . . ? C25 C26 C27 119.8(5) . . ? C25 C26 H26A 120.1 . . ? C27 C26 H26A 120.1 . . ? O1 C1 C2 125.9(6) . . ? O1 C1 C6 116.5(5) . . ? C2 C1 C6 117.5(6) . . ? C36 C35 C34 121.2(7) . . ? C36 C35 H35A 119.4 . . ? C34 C35 H35A 119.4 . . ? C28 C27 C26 120.0(6) . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C35 C36 C31 121.1(7) . . ? C35 C36 H36A 119.5 . . ? C31 C36 H36A 119.5 . . ? C44 C45 C46 108.5(8) . . ? C44 C45 Ti1 74.6(5) . . ? C46 C45 Ti1 73.0(4) . . ? C44 C45 H45A 125.5 . . ? C46 C45 H45A 125.5 . . ? Ti1 C45 H45A 125.5 . . ? C23 C24 C19 119.4(8) . . ? C23 C24 H24A 120.3 . . ? C19 C24 H24A 120.3 . . ? C3 C2 C1 118.4(7) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C41 C40 C39 119.5(6) . . ? C41 C40 H40A 120.2 . . ? C39 C40 H40A 120.2 . . ? C19 C20 C21 121.6(8) . . ? C19 C20 H20A 119.2 . . ? C21 C20 H20A 119.2 . . ? C37 C42 C41 119.6(7) . . ? C37 C42 H42A 120.2 . . ? C41 C42 H42A 120.2 . . ? C40 C39 C38 120.1(7) . . ? C40 C39 H39A 120.0 . . ? C38 C39 H39A 120.0 . . ? C34 C33 C32 120.7(7) . . ? C34 C33 H33A 119.7 . . ? C32 C33 H33A 119.7 . . ? C4 C3 C2 124.1(7) . . ? C4 C3 H3A 118.0 . . ? C2 C3 H3A 118.0 . . ? C33 C34 C35 118.7(7) . . ? C33 C34 H34A 120.6 . . ? C35 C34 H34A 120.6 . . ? C14 C43 H43A 109.5 . . ? C14 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C14 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C22 C23 C24 120.8(8) . . ? C22 C23 H23A 119.6 . . ? C24 C23 H23A 119.6 . . ? C23 C22 C21 121.6(8) . . ? C23 C22 H22A 119.2 . . ? C21 C22 H22A 119.2 . . ? C22 C21 C20 118.7(9) . . ? C22 C21 H21A 120.6 . . ? C20 C21 H21A 120.6 . . ? C46 C47 C48 108.9(9) . . ? C46 C47 Ti1 73.1(4) . . ? C48 C47 Ti1 74.3(5) . . ? C46 C47 H47A 125.3 . . ? C48 C47 H47A 125.3 . . ? Ti1 C47 H47A 125.3 . . ? C45 C44 C48 106.8(8) . . ? C45 C44 Ti1 72.2(4) . . ? C48 C44 Ti1 72.7(5) . . ? C45 C44 H44A 126.4 . . ? C48 C44 H44A 126.4 . . ? Ti1 C44 H44A 126.4 . . ? C3 C4 C5 119.5(7) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C47 C48 C44 107.3(8) . . ? C47 C48 Ti1 72.5(5) . . ? C44 C48 Ti1 72.8(5) . . ? C47 C48 H48A 126.1 . . ? C44 C48 H48A 126.1 . . ? Ti1 C48 H48A 126.1 . . ? 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 Ti1 N1 C9 -179.8(5) . . . . ? C46 Ti1 N1 C9 36.5(7) . . . . ? C45 Ti1 N1 C9 -30.6(7) . . . . ? N2 Ti1 N1 C9 0.0(4) . . . . ? C47 Ti1 N1 C9 104.8(7) . . . . ? C48 Ti1 N1 C9 179.9(10) . . . . ? C44 Ti1 N1 C9 -100.1(8) . . . . ? Cl2 Ti1 N1 C9 -89.1(4) . . . . ? Cl1 Ti1 N1 C9 89.2(4) . . . . ? O1 Ti1 N1 C6 -3.5(4) . . . . ? C46 Ti1 N1 C6 -147.2(5) . . . . ? C45 Ti1 N1 C6 145.7(5) . . . . ? N2 Ti1 N1 C6 176.3(4) . . . . ? C47 Ti1 N1 C6 -78.9(7) . . . . ? C48 Ti1 N1 C6 -3.9(11) . . . . ? C44 Ti1 N1 C6 76.2(8) . . . . ? Cl2 Ti1 N1 C6 87.2(4) . . . . ? Cl1 Ti1 N1 C6 -94.5(4) . . . . ? N1 Ti1 O1 C1 3.5(4) . . . . ? C46 Ti1 O1 C1 160.4(4) . . . . ? C45 Ti1 O1 C1 -156.3(4) . . . . ? N2 Ti1 O1 C1 3.1(6) . . . . ? C47 Ti1 O1 C1 155.3(5) . . . . ? C48 Ti1 O1 C1 -176.6(6) . . . . ? C44 Ti1 O1 C1 -148.4(5) . . . . ? Cl2 Ti1 O1 C1 -72.9(4) . . . . ? Cl1 Ti1 O1 C1 79.4(4) . . . . ? C6 N1 C9 C8 3.1(8) . . . . ? Ti1 N1 C9 C8 179.1(4) . . . . ? C6 N1 C9 C10 -176.6(5) . . . . ? Ti1 N1 C9 C10 -0.6(6) . . . . ? C15 C16 C17 C19 -21.3(8) . . . . ? C11 C16 C17 C19 162.5(5) . . . . ? C15 C16 C17 C25 107.5(6) . . . . ? C11 C16 C17 C25 -68.7(6) . . . . ? O1 Ti1 N2 C10 1.2(6) . . . . ? N1 Ti1 N2 C10 0.8(4) . . . . ? C46 Ti1 N2 C10 -160.7(4) . . . . ? C45 Ti1 N2 C10 165.2(4) . . . . ? C47 Ti1 N2 C10 -147.8(4) . . . . ? C48 Ti1 N2 C10 -179.2(7) . . . . ? C44 Ti1 N2 C10 150.2(4) . . . . ? Cl2 Ti1 N2 C10 78.2(4) . . . . ? Cl1 Ti1 N2 C10 -76.1(4) . . . . ? O1 Ti1 N2 C11 -179.0(4) . . . . ? N1 Ti1 N2 C11 -179.4(5) . . . . ? C46 Ti1 N2 C11 19.1(5) . . . . ? C45 Ti1 N2 C11 -15.0(5) . . . . ? C47 Ti1 N2 C11 32.1(5) . . . . ? C48 Ti1 N2 C11 0.7(8) . . . . ? C44 Ti1 N2 C11 -29.9(5) . . . . ? Cl2 Ti1 N2 C11 -101.9(4) . . . . ? Cl1 Ti1 N2 C11 103.8(4) . . . . ? C15 C16 C11 C12 -7.6(8) . . . . ? C17 C16 C11 C12 168.7(5) . . . . ? C15 C16 C11 N2 171.9(5) . . . . ? C17 C16 C11 N2 -11.7(7) . . . . ? C10 N2 C11 C16 91.8(6) . . . . ? Ti1 N2 C11 C16 -88.1(5) . . . . ? C10 N2 C11 C12 -88.7(6) . . . . ? Ti1 N2 C11 C12 91.5(5) . . . . ? C11 C16 C15 C14 1.2(8) . . . . ? C17 C16 C15 C14 -175.0(5) . . . . ? C37 C18 C31 C36 87.3(7) . . . . ? C12 C18 C31 C36 -143.8(6) . . . . ? C37 C18 C31 C32 -93.3(7) . . . . ? C12 C18 C31 C32 35.6(7) . . . . ? C31 C18 C37 C42 13.1(8) . . . . ? C12 C18 C37 C42 -114.3(6) . . . . ? C31 C18 C37 C38 -167.4(5) . . . . ? C12 C18 C37 C38 65.2(7) . . . . ? C19 C17 C25 C26 97.1(6) . . . . ? C16 C17 C25 C26 -32.5(7) . . . . ? C19 C17 C25 C30 -85.6(7) . . . . ? C16 C17 C25 C30 144.8(5) . . . . ? N1 C9 C8 C7 -1.7(9) . . . . ? C10 C9 C8 C7 178.0(6) . . . . ? C14 C13 C12 C11 -0.6(8) . . . . ? C14 C13 C12 C18 176.3(5) . . . . ? C16 C11 C12 C13 7.3(8) . . . . ? N2 C11 C12 C13 -172.3(5) . . . . ? C16 C11 C12 C18 -169.7(5) . . . . ? N2 C11 C12 C18 10.8(7) . . . . ? C37 C18 C12 C13 19.6(8) . . . . ? C31 C18 C12 C13 -108.7(6) . . . . ? C37 C18 C12 C11 -163.6(5) . . . . ? C31 C18 C12 C11 68.1(6) . . . . ? C42 C37 C38 C39 0.3(10) . . . . ? C18 C37 C38 C39 -179.2(6) . . . . ? C16 C17 C19 C20 -92.5(7) . . . . ? C25 C17 C19 C20 139.0(6) . . . . ? C16 C17 C19 C24 87.5(7) . . . . ? C25 C17 C19 C24 -41.1(8) . . . . ? C16 C15 C14 C13 5.2(9) . . . . ? C16 C15 C14 C43 -175.1(5) . . . . ? C12 C13 C14 C15 -5.6(9) . . . . ? C12 C13 C14 C43 174.8(5) . . . . ? C26 C25 C30 C29 0.0(9) . . . . ? C17 C25 C30 C29 -177.3(6) . . . . ? C11 N2 C10 C9 178.8(4) . . . . ? Ti1 N2 C10 C9 -1.4(6) . . . . ? N1 C9 C10 N2 1.3(7) . . . . ? C8 C9 C10 N2 -178.4(5) . . . . ? C9 C8 C7 C5 -1.5(10) . . . . ? C4 C5 C7 C8 -177.7(7) . . . . ? C6 C5 C7 C8 3.1(10) . . . . ? C27 C28 C29 C30 0.4(11) . . . . ? C25 C30 C29 C28 0.2(11) . . . . ? O1 Ti1 C46 C47 -9.3(6) . . . . ? N1 Ti1 C46 C47 124.4(6) . . . . ? C45 Ti1 C46 C47 -115.7(7) . . . . ? N2 Ti1 C46 C47 158.4(5) . . . . ? C48 Ti1 C46 C47 -36.7(6) . . . . ? C44 Ti1 C46 C47 -78.9(6) . . . . ? Cl2 Ti1 C46 C47 -121.5(5) . . . . ? Cl1 Ti1 C46 C47 73.6(5) . . . . ? O1 Ti1 C46 C45 106.4(5) . . . . ? N1 Ti1 C46 C45 -119.9(5) . . . . ? N2 Ti1 C46 C45 -85.9(4) . . . . ? C47 Ti1 C46 C45 115.7(7) . . . . ? C48 Ti1 C46 C45 79.0(6) . . . . ? C44 Ti1 C46 C45 36.8(5) . . . . ? Cl2 Ti1 C46 C45 -5.8(5) . . . . ? Cl1 Ti1 C46 C45 -170.7(4) . . . . ? C9 N1 C6 C1 179.4(5) . . . . ? Ti1 N1 C6 C1 3.0(6) . . . . ? C9 N1 C6 C5 -1.3(9) . . . . ? Ti1 N1 C6 C5 -177.8(5) . . . . ? C7 C5 C6 N1 -1.8(9) . . . . ? C4 C5 C6 N1 179.0(6) . . . . ? C7 C5 C6 C1 177.4(6) . . . . ? C4 C5 C6 C1 -1.8(10) . . . . ? C36 C31 C32 C33 -0.1(10) . . . . ? C18 C31 C32 C33 -179.5(6) . . . . ? C30 C25 C26 C27 -0.7(9) . . . . ? C17 C25 C26 C27 176.5(6) . . . . ? Ti1 O1 C1 C2 177.7(5) . . . . ? Ti1 O1 C1 C6 -3.1(7) . . . . ? N1 C6 C1 O1 -0.2(8) . . . . ? C5 C6 C1 O1 -179.4(6) . . . . ? N1 C6 C1 C2 179.1(6) . . . . ? C5 C6 C1 C2 -0.2(10) . . . . ? C29 C28 C27 C26 -1.2(11) . . . . ? C25 C26 C27 C28 1.3(10) . . . . ? C34 C35 C36 C31 0.9(12) . . . . ? C32 C31 C36 C35 -0.4(10) . . . . ? C18 C31 C36 C35 179.0(6) . . . . ? C47 C46 C45 C44 -1.0(8) . . . . ? Ti1 C46 C45 C44 -66.7(5) . . . . ? C47 C46 C45 Ti1 65.7(5) . . . . ? O1 Ti1 C45 C44 14.4(7) . . . . ? N1 Ti1 C45 C44 -125.8(6) . . . . ? C46 Ti1 C45 C44 115.3(8) . . . . ? N2 Ti1 C45 C44 -154.4(6) . . . . ? C47 Ti1 C45 C44 78.7(6) . . . . ? C48 Ti1 C45 C44 38.4(6) . . . . ? Cl2 Ti1 C45 C44 -69.7(6) . . . . ? Cl1 Ti1 C45 C44 125.8(6) . . . . ? O1 Ti1 C45 C46 -100.9(5) . . . . ? N1 Ti1 C45 C46 118.9(5) . . . . ? N2 Ti1 C45 C46 90.3(4) . . . . ? C47 Ti1 C45 C46 -36.7(5) . . . . ? C48 Ti1 C45 C46 -77.0(6) . . . . ? C44 Ti1 C45 C46 -115.3(8) . . . . ? Cl2 Ti1 C45 C46 175.0(4) . . . . ? Cl1 Ti1 C45 C46 10.4(5) . . . . ? C20 C19 C24 C23 1.1(10) . . . . ? C17 C19 C24 C23 -178.9(6) . . . . ? O1 C1 C2 C3 -179.3(7) . . . . ? C6 C1 C2 C3 1.5(10) . . . . ? C42 C41 C40 C39 -1.1(11) . . . . ? C24 C19 C20 C21 -1.5(10) . . . . ? C17 C19 C20 C21 178.4(7) . . . . ? C38 C37 C42 C41 -0.4(10) . . . . ? C18 C37 C42 C41 179.1(6) . . . . ? C40 C41 C42 C37 0.8(11) . . . . ? C41 C40 C39 C38 1.0(11) . . . . ? C37 C38 C39 C40 -0.6(10) . . . . ? C31 C32 C33 C34 0.1(11) . . . . ? C1 C2 C3 C4 -0.9(12) . . . . ? C32 C33 C34 C35 0.3(13) . . . . ? C36 C35 C34 C33 -0.8(13) . . . . ? C19 C24 C23 C22 0.0(11) . . . . ? C24 C23 C22 C21 -0.7(13) . . . . ? C23 C22 C21 C20 0.3(13) . . . . ? C19 C20 C21 C22 0.9(12) . . . . ? C45 C46 C47 C48 0.9(8) . . . . ? Ti1 C46 C47 C48 66.2(6) . . . . ? C45 C46 C47 Ti1 -65.3(5) . . . . ? O1 Ti1 C47 C46 172.6(5) . . . . ? N1 Ti1 C47 C46 -116.2(6) . . . . ? C45 Ti1 C47 C46 37.4(5) . . . . ? N2 Ti1 C47 C46 -24.0(6) . . . . ? C48 Ti1 C47 C46 115.9(8) . . . . ? C44 Ti1 C47 C46 77.8(6) . . . . ? Cl2 Ti1 C47 C46 82.0(6) . . . . ? Cl1 Ti1 C47 C46 -100.6(5) . . . . ? O1 Ti1 C47 C48 56.6(6) . . . . ? N1 Ti1 C47 C48 127.9(6) . . . . ? C46 Ti1 C47 C48 -115.9(8) . . . . ? C45 Ti1 C47 C48 -78.6(6) . . . . ? N2 Ti1 C47 C48 -139.9(6) . . . . ? C44 Ti1 C47 C48 -38.2(6) . . . . ? Cl2 Ti1 C47 C48 -33.9(8) . . . . ? Cl1 Ti1 C47 C48 143.4(7) . . . . ? C46 C45 C44 C48 0.8(9) . . . . ? Ti1 C45 C44 C48 -64.9(6) . . . . ? C46 C45 C44 Ti1 65.7(5) . . . . ? O1 Ti1 C44 C45 -168.7(6) . . . . ? N1 Ti1 C44 C45 116.2(6) . . . . ? C46 Ti1 C44 C45 -37.6(5) . . . . ? N2 Ti1 C44 C45 27.8(6) . . . . ? C47 Ti1 C44 C45 -78.1(6) . . . . ? C48 Ti1 C44 C45 -114.7(8) . . . . ? Cl2 Ti1 C44 C45 105.2(6) . . . . ? Cl1 Ti1 C44 C45 -76.0(7) . . . . ? O1 Ti1 C44 C48 -54.0(7) . . . . ? N1 Ti1 C44 C48 -129.0(7) . . . . ? C46 Ti1 C44 C48 77.1(6) . . . . ? C45 Ti1 C44 C48 114.7(8) . . . . ? N2 Ti1 C44 C48 142.5(7) . . . . ? C47 Ti1 C44 C48 36.7(6) . . . . ? Cl2 Ti1 C44 C48 -140.1(7) . . . . ? Cl1 Ti1 C44 C48 38.8(8) . . . . ? C2 C3 C4 C5 -1.1(12) . . . . ? C7 C5 C4 C3 -176.7(7) . . . . ? C6 C5 C4 C3 2.4(10) . . . . ? C46 C47 C48 C44 -0.5(9) . . . . ? Ti1 C47 C48 C44 65.0(6) . . . . ? C46 C47 C48 Ti1 -65.4(5) . . . . ? C45 C44 C48 C47 -0.2(10) . . . . ? Ti1 C44 C48 C47 -64.8(6) . . . . ? C45 C44 C48 Ti1 64.6(5) . . . . ? O1 Ti1 C48 C47 -120.9(7) . . . . ? N1 Ti1 C48 C47 -120.5(7) . . . . ? C46 Ti1 C48 C47 36.9(5) . . . . ? C45 Ti1 C48 C47 78.2(5) . . . . ? N2 Ti1 C48 C47 59.3(9) . . . . ? C44 Ti1 C48 C47 115.1(8) . . . . ? Cl2 Ti1 C48 C47 154.8(6) . . . . ? Cl1 Ti1 C48 C47 -36.4(6) . . . . ? O1 Ti1 C48 C44 124.0(7) . . . . ? N1 Ti1 C48 C44 124.4(7) . . . . ? C46 Ti1 C48 C44 -78.3(6) . . . . ? C45 Ti1 C48 C44 -36.9(5) . . . . ? N2 Ti1 C48 C44 -55.8(10) . . . . ? C47 Ti1 C48 C44 -115.1(8) . . . . ? Cl2 Ti1 C48 C44 39.7(6) . . . . ? Cl1 Ti1 C48 C44 -151.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.522 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.132 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 241 89 ' ' 2 0.000 0.000 0.500 34 3 ' ' 3 0.000 0.500 0.500 241 90 ' ' 4 0.000 0.500 1.000 34 3 ' ' 5 0.164 0.137 0.313 24 4 ' ' 6 0.164 0.363 0.813 24 5 ' ' 7 0.336 0.637 0.313 24 4 ' ' 8 0.336 0.863 0.813 24 5 ' ' 9 0.500 0.500 1.000 241 89 ' ' 10 0.500 1.000 0.500 241 89 ' ' 11 0.500 0.000 0.000 34 3 ' ' 12 0.500 0.500 0.500 34 3 ' ' 13 0.664 0.137 0.187 24 5 ' ' 14 0.664 0.363 0.687 24 5 ' ' 15 0.836 0.637 0.187 24 5 ' ' 16 0.836 0.863 0.687 24 5 ' ' _platon_squeeze_details ; ; #==END data_C4 _database_code_depnum_ccdc_archive 'CCDC 869825' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H32 Cl2 N2 O Ti' _chemical_formula_weight 639.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 53.675(11) _cell_length_b 10.021(2) _cell_length_c 24.886(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.29(3) _cell_angle_gamma 90.00 _cell_volume 13170(5) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20009 _cell_measurement_theta_min .77 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5312 _exptl_absorpt_coefficient_mu 0.454 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.7165 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 25332 _diffrn_reflns_av_R_equivalents 0.0639 _diffrn_reflns_av_sigmaI/netI 0.0903 _diffrn_reflns_limit_h_min -63 _diffrn_reflns_limit_h_max 63 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 0.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11535 _reflns_number_gt 8323 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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^)+(0.1157P)^2^+87.5137P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11535 _refine_ls_number_parameters 775 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.1193 _refine_ls_R_factor_gt 0.0932 _refine_ls_wR_factor_ref 0.2632 _refine_ls_wR_factor_gt 0.2446 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.005 _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 Ti2 Ti 0.19067(2) 0.04475(11) 0.27212(5) 0.0298(3) Uani 1 1 d . . . O1 O 0.04508(8) -0.6017(4) -0.21400(17) 0.0364(10) Uani 1 1 d . . . N1 N 0.08262(9) -0.4680(5) -0.1637(2) 0.0263(11) Uani 1 1 d . . . Ti1 Ti 0.04488(2) -0.49079(11) -0.14980(4) 0.0292(3) Uani 1 1 d . . . O2 O 0.18436(8) -0.0563(5) 0.33587(17) 0.0370(10) Uani 1 1 d . . . N2 N 0.06909(8) -0.3471(5) -0.08280(19) 0.0242(10) Uani 1 1 d . . . Cl2 Cl 0.06771(3) -0.67424(14) -0.09740(6) 0.0322(4) Uani 1 1 d . . . N3 N 0.15042(9) 0.0601(5) 0.2657(2) 0.0278(11) Uani 1 1 d . . . Cl4 Cl 0.17515(3) -0.15468(15) 0.21957(7) 0.0368(4) Uani 1 1 d . . . N4 N 0.17266(9) 0.1700(5) 0.1930(2) 0.0271(11) Uani 1 1 d . . . Cl3 Cl 0.18405(3) 0.25074(16) 0.32023(7) 0.0382(4) Uani 1 1 d . . . Cl1 Cl 0.04353(3) -0.29236(16) -0.20795(6) 0.0367(4) Uani 1 1 d . . . C49 C 0.18612(11) 0.2278(6) 0.1520(2) 0.0299(13) Uani 1 1 d . . . C10 C 0.09153(11) -0.3185(6) -0.0908(2) 0.0274(13) Uani 1 1 d . . . C21 C 0.06654(11) -0.5714(6) 0.0623(2) 0.0291(13) Uani 1 1 d . . . C50 C 0.19619(11) 0.3549(6) 0.1594(2) 0.0293(13) Uani 1 1 d . . . C1 C 0.06694(13) -0.6203(6) -0.2321(3) 0.0344(15) Uani 1 1 d . . . C54 C 0.18787(11) 0.1512(6) 0.1060(2) 0.0275(13) Uani 1 1 d . . . C12 C 0.05972(11) -0.2839(6) -0.0379(3) 0.0299(13) Uani 1 1 d . . . C51 C 0.21004(11) 0.4025(6) 0.1214(2) 0.0314(14) Uani 1 1 d . . . H51A H 0.2172 0.4894 0.1261 0.038 Uiso 1 1 calc R . . C58 C 0.14577(12) 0.0352(6) 0.0774(3) 0.0328(14) Uani 1 1 d . . . C44 C 0.09907(12) 0.0583(6) 0.2661(3) 0.0361(15) Uani 1 1 d . . . H44A H 0.0813 0.0577 0.2656 0.043 Uiso 1 1 calc R . . C27 C 0.10461(11) -0.4584(6) 0.0339(2) 0.0273(13) Uani 1 1 d . . . C14 C 0.03683(11) -0.1056(6) -0.0030(2) 0.0301(13) Uani 1 1 d . . . H14A H 0.0281 -0.0228 -0.0084 0.036 Uiso 1 1 calc R . . C43 C 0.14125(12) -0.0080(6) 0.3040(3) 0.0335(14) Uani 1 1 d . . . C20 C 0.07609(11) -0.4811(5) 0.0214(2) 0.0276(13) Uani 1 1 d . . . H20A H 0.0726 -0.5293 -0.0144 0.033 Uiso 1 1 calc R . . C6 C 0.08758(13) -0.5461(7) -0.2052(3) 0.0376(15) Uani 1 1 d . . . C16 C 0.05077(11) -0.2914(6) 0.0534(3) 0.0305(13) Uani 1 1 d . . . H16A H 0.0520 -0.3367 0.0873 0.037 Uiso 1 1 calc R . . C15 C 0.03814(11) -0.1696(6) 0.0467(3) 0.0309(13) Uani 1 1 d . . . C64 C 0.18659(12) -0.0737(6) 0.0588(3) 0.0313(14) Uani 1 1 d . . . C13 C 0.04755(12) -0.1559(6) -0.0451(2) 0.0312(14) Uani 1 1 d . . . C38 C 0.16065(13) -0.0751(6) 0.3424(3) 0.0364(15) Uani 1 1 d . . . C53 C 0.20247(11) 0.2049(7) 0.0684(3) 0.0335(14) Uani 1 1 d . . . H53A H 0.2044 0.1549 0.0370 0.040 Uiso 1 1 calc R . . C26 C 0.07371(13) -0.5587(6) 0.1175(3) 0.0357(15) Uani 1 1 d . . . H26A H 0.0859 -0.4933 0.1320 0.043 Uiso 1 1 calc R . . C8 C 0.12485(12) -0.3849(6) -0.1480(3) 0.0371(15) Uani 1 1 d . . . H8A H 0.1373 -0.3272 -0.1283 0.044 Uiso 1 1 calc R . . C32 C 0.11714(13) -0.3728(6) 0.0727(3) 0.0375(15) Uani 1 1 d . . . H32A H 0.1074 -0.3217 0.0936 0.045 Uiso 1 1 calc R . . C46\ C 0.13529(12) 0.1297(6) 0.2288(2) 0.0301(13) Uani 1 1 d . . . C24 C 0.04660(13) -0.7384(6) 0.1342(3) 0.0376(15) Uani 1 1 d . . . H24A H 0.0402 -0.7960 0.1588 0.045 Uiso 1 1 calc R . . C11 C 0.10910(11) -0.2171(6) -0.0589(3) 0.0314(14) Uani 1 1 d . . . H11A H 0.1008 -0.1766 -0.0308 0.047 Uiso 1 1 calc R . . H11B H 0.1131 -0.1476 -0.0838 0.047 Uiso 1 1 calc R . . H11C H 0.1248 -0.2613 -0.0415 0.047 Uiso 1 1 calc R . . C2 C 0.07126(14) -0.7034(7) -0.2735(3) 0.0423(17) Uani 1 1 d . . . H2A H 0.0577 -0.7544 -0.2932 0.051 Uiso 1 1 calc R . . C7 C 0.13065(13) -0.4633(7) -0.1892(3) 0.0415(16) Uani 1 1 d . . . H7A H 0.1473 -0.4610 -0.1973 0.050 Uiso 1 1 calc R . . C30 C 0.15786(13) -0.4251(7) 0.0524(3) 0.0436(17) Uani 1 1 d . . . H30A H 0.1757 -0.4141 0.0589 0.052 Uiso 1 1 calc R . . C57 C 0.17432(11) 0.0157(6) 0.0957(3) 0.0314(14) Uani 1 1 d . . . H57A H 0.1765 -0.0303 0.1319 0.038 Uiso 1 1 calc R . . C5 C 0.11230(13) -0.5475(7) -0.2197(3) 0.0373(15) Uani 1 1 d . . . C52 C 0.21378(11) 0.3280(6) 0.0772(3) 0.0308(14) Uani 1 1 d . . . C55 C 0.19257(14) 0.4464(7) 0.2057(3) 0.0440(17) Uani 1 1 d . . . H55A H 0.1824 0.4008 0.2292 0.066 Uiso 1 1 calc R . . H55B H 0.1838 0.5276 0.1907 0.066 Uiso 1 1 calc R . . H55C H 0.2091 0.4700 0.2271 0.066 Uiso 1 1 calc R . . C59 C 0.12871(12) -0.0328(6) 0.1047(3) 0.0336(14) Uani 1 1 d . . . H59A H 0.1351 -0.0890 0.1348 0.040 Uiso 1 1 calc R . . C29 C 0.14606(13) -0.5109(7) 0.0118(3) 0.0440(17) Uani 1 1 d . . . H29A H 0.1560 -0.5578 -0.0100 0.053 Uiso 1 1 calc R . . C48 C 0.13413(12) 0.2979(7) 0.1497(3) 0.0359(15) Uani 1 1 d . . . H48A H 0.1454 0.3352 0.1265 0.054 Uiso 1 1 calc R . . H48B H 0.1278 0.3699 0.1703 0.054 Uiso 1 1 calc R . . H48C H 0.1198 0.2529 0.1268 0.054 Uiso 1 1 calc R . . C42 C 0.11540(13) -0.0165(6) 0.3058(3) 0.0383(16) Uani 1 1 d . . . C17 C 0.06179(11) -0.3499(6) 0.0123(2) 0.0289(13) Uani 1 1 d . . . C9 C 0.10068(11) -0.3897(6) -0.1348(3) 0.0313(14) Uani 1 1 d . . . C47 C 0.14887(11) 0.1972(6) 0.1896(2) 0.0298(13) Uani 1 1 d . . . C63 C 0.13550(12) 0.1194(6) 0.0342(3) 0.0359(15) Uani 1 1 d . . . H63A H 0.1465 0.1695 0.0160 0.043 Uiso 1 1 calc R . . C37 C 0.00955(12) -0.3912(8) -0.1225(3) 0.0433(17) Uani 1 1 d . . . H37A H 0.0081 -0.2951 -0.1127 0.052 Uiso 1 1 calc R . . C62 C 0.10968(13) 0.1309(7) 0.0177(3) 0.0422(16) Uani 1 1 d . . . H62A H 0.1031 0.1858 -0.0127 0.051 Uiso 1 1 calc R . . C25 C 0.06312(13) -0.6419(6) 0.1532(3) 0.0406(16) Uani 1 1 d . . . H25A H 0.0678 -0.6293 0.1915 0.049 Uiso 1 1 calc R . . C28 C 0.12028(12) -0.5291(6) 0.0028(3) 0.0332(14) Uani 1 1 d . . . H28A H 0.1127 -0.5898 -0.0246 0.040 Uiso 1 1 calc R . . C40 C 0.12681(14) -0.1641(7) 0.3826(3) 0.0458(18) Uani 1 1 d . . . H40A H 0.1217 -0.2205 0.4093 0.055 Uiso 1 1 calc R . . C31 C 0.14324(13) -0.3571(7) 0.0827(3) 0.0443(17) Uani 1 1 d . . . H31A H 0.1510 -0.2987 0.1109 0.053 Uiso 1 1 calc R . . C45 C 0.10904(12) 0.1323(6) 0.2282(3) 0.0359(15) Uani 1 1 d . . . H45A H 0.0982 0.1846 0.2019 0.043 Uiso 1 1 calc R . . C23 C 0.03889(13) -0.7536(7) 0.0778(3) 0.0429(17) Uani 1 1 d . . . H23A H 0.0269 -0.8201 0.0636 0.051 Uiso 1 1 calc R . . C61 C 0.09319(12) 0.0635(6) 0.0449(3) 0.0375(15) Uani 1 1 d . . . H61A H 0.0754 0.0730 0.0340 0.045 Uiso 1 1 calc R . . C60 C 0.10328(13) -0.0190(6) 0.0886(3) 0.0386(16) Uani 1 1 d . . . H60A H 0.0922 -0.0663 0.1075 0.046 Uiso 1 1 calc R . . C19 C 0.02767(13) -0.1063(7) 0.0936(3) 0.0389(15) Uani 1 1 d . . . H19A H 0.0195 -0.0213 0.0815 0.058 Uiso 1 1 calc R . . H19B H 0.0415 -0.0905 0.1243 0.058 Uiso 1 1 calc R . . H19C H 0.0152 -0.1664 0.1051 0.058 Uiso 1 1 calc R . . C34 C 0.00259(13) -0.5851(8) -0.1688(3) 0.0485(19) Uani 1 1 d . . . H34A H -0.0037 -0.6516 -0.1981 0.058 Uiso 1 1 calc R . . C18 C 0.04798(15) -0.0734(7) -0.0963(3) 0.0467(18) Uani 1 1 d . . . H18A H 0.0387 0.0100 -0.0942 0.070 Uiso 1 1 calc R . . H18B H 0.0400 -0.1241 -0.1285 0.070 Uiso 1 1 calc R . . H18C H 0.0655 -0.0530 -0.0992 0.070 Uiso 1 1 calc R . . C56 C 0.22993(14) 0.3801(7) 0.0368(3) 0.0453(17) Uani 1 1 d . . . H56A H 0.2366 0.4685 0.0485 0.068 Uiso 1 1 calc R . . H56B H 0.2195 0.3868 0.0004 0.068 Uiso 1 1 calc R . . H56C H 0.2440 0.3185 0.0357 0.068 Uiso 1 1 calc R . . C22 C 0.04902(12) -0.6706(6) 0.0434(3) 0.0335(14) Uani 1 1 d . . . H22A H 0.0438 -0.6813 0.0051 0.040 Uiso 1 1 calc R . . C69 C 0.17777(13) -0.0869(7) 0.0029(3) 0.0419(16) Uani 1 1 d . . . H69A H 0.1628 -0.0413 -0.0135 0.050 Uiso 1 1 calc R . . C36 C 0.01703(13) -0.4948(7) -0.0857(3) 0.0430(17) Uani 1 1 d . . . H36A H 0.0221 -0.4856 -0.0452 0.052 Uiso 1 1 calc R . . C4 C 0.11542(14) -0.6407(7) -0.2617(3) 0.0423(17) Uani 1 1 d . . . H4A H 0.1315 -0.6513 -0.2720 0.051 Uiso 1 1 calc R . . C39 C 0.15277(14) -0.1536(7) 0.3826(3) 0.0433(17) Uani 1 1 d . . . H39A H 0.1647 -0.1985 0.4093 0.052 Uiso 1 1 calc R . . C65 C 0.20809(13) -0.1438(7) 0.0806(3) 0.0424(16) Uani 1 1 d . . . H65A H 0.2144 -0.1372 0.1187 0.051 Uiso 1 1 calc R . . C3 C 0.09551(15) -0.7133(7) -0.2868(3) 0.0473(18) Uani 1 1 d . . . H3A H 0.0980 -0.7740 -0.3146 0.057 Uiso 1 1 calc R . . C41 C 0.10802(14) -0.1003(7) 0.3473(3) 0.0421(16) Uani 1 1 d . . . H41A H 0.0907 -0.1110 0.3501 0.050 Uiso 1 1 calc R . . C67 C 0.21201(15) -0.2332(7) -0.0059(3) 0.0497(19) Uani 1 1 d . . . H67A H 0.2207 -0.2865 -0.0282 0.060 Uiso 1 1 calc R . . C66 C 0.22107(14) -0.2246(7) 0.0488(3) 0.0506(19) Uani 1 1 d . . . H66A H 0.2358 -0.2723 0.0650 0.061 Uiso 1 1 calc R . . C35 C 0.01266(13) -0.6152(8) -0.1146(3) 0.0491(19) Uani 1 1 d . . . H35A H 0.0147 -0.7067 -0.0984 0.059 Uiso 1 1 calc R . . C33 C 0.00014(12) -0.4488(8) -0.1737(3) 0.0457(18) Uani 1 1 d . . . H33A H -0.0085 -0.3997 -0.2069 0.055 Uiso 1 1 calc R . . C68 C 0.19062(15) -0.1663(8) -0.0291(3) 0.0490(18) Uani 1 1 d . . . H68A H 0.1845 -0.1739 -0.0673 0.059 Uiso 1 1 calc R . . C71 C 0.23144(16) -0.0458(12) 0.3109(5) 0.078(3) Uani 1 1 d . . . H71A H 0.2349 -0.1146 0.3404 0.093 Uiso 1 1 calc R . . C73 C 0.22941(14) 0.1438(9) 0.2635(5) 0.078(3) Uani 1 1 d . . . H73A H 0.2319 0.2386 0.2531 0.094 Uiso 1 1 calc R . . C74 C 0.22697(15) 0.0395(13) 0.2300(4) 0.069(3) Uani 1 1 d . . . H74A H 0.2268 0.0435 0.1898 0.082 Uiso 1 1 calc R . . C72 C 0.23192(16) 0.0928(13) 0.3185(4) 0.078(3) Uani 1 1 d . . . H72A H 0.2369 0.1431 0.3534 0.093 Uiso 1 1 calc R . . C70 C 0.22790(18) -0.0685(11) 0.2587(6) 0.083(3) Uani 1 1 d . . . H70A H 0.2278 -0.1599 0.2426 0.099 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti2 0.0244(6) 0.0358(6) 0.0286(6) 0.0028(5) 0.0032(4) 0.0028(4) O1 0.036(3) 0.043(3) 0.027(2) -0.002(2) -0.0043(19) -0.0051(19) N1 0.024(2) 0.029(2) 0.026(3) 0.000(2) 0.002(2) 0.002(2) Ti1 0.0243(6) 0.0330(6) 0.0289(6) -0.0011(5) 0.0008(4) 0.0003(4) O2 0.034(3) 0.048(3) 0.029(2) 0.010(2) 0.0068(19) 0.001(2) N2 0.020(2) 0.027(2) 0.024(2) -0.002(2) 0.000(2) 0.0012(19) Cl2 0.0344(8) 0.0298(7) 0.0312(8) 0.0001(6) 0.0027(6) 0.0019(6) N3 0.027(3) 0.029(3) 0.029(3) 0.000(2) 0.011(2) -0.004(2) Cl4 0.0417(9) 0.0341(8) 0.0342(8) 0.0007(7) 0.0058(7) 0.0027(6) N4 0.028(3) 0.028(2) 0.025(3) -0.002(2) 0.003(2) -0.006(2) Cl3 0.0411(9) 0.0393(9) 0.0332(8) -0.0028(7) 0.0043(7) -0.0012(7) Cl1 0.0360(8) 0.0389(8) 0.0329(8) 0.0021(7) 0.0001(7) 0.0031(6) C49 0.025(3) 0.037(3) 0.027(3) 0.010(3) 0.000(2) 0.001(2) C10 0.034(3) 0.024(3) 0.023(3) 0.003(2) 0.003(3) 0.001(2) C21 0.027(3) 0.030(3) 0.030(3) -0.001(3) 0.004(3) 0.006(2) C50 0.032(3) 0.029(3) 0.027(3) 0.003(3) 0.003(3) -0.002(2) C1 0.043(4) 0.028(3) 0.029(3) 0.001(3) -0.001(3) 0.000(3) C54 0.025(3) 0.030(3) 0.026(3) -0.004(3) 0.000(2) 0.001(2) C12 0.022(3) 0.032(3) 0.033(3) -0.003(3) -0.001(3) 0.001(2) C51 0.028(3) 0.030(3) 0.033(3) 0.005(3) -0.005(3) -0.002(2) C58 0.031(3) 0.036(3) 0.029(3) -0.003(3) 0.000(3) -0.003(3) C44 0.028(3) 0.038(3) 0.044(4) -0.006(3) 0.011(3) 0.000(3) C27 0.031(3) 0.025(3) 0.025(3) 0.006(3) 0.000(2) 0.002(2) C14 0.030(3) 0.027(3) 0.031(3) 0.002(3) -0.001(3) 0.005(2) C43 0.035(3) 0.036(3) 0.030(3) -0.006(3) 0.009(3) -0.001(3) C20 0.028(3) 0.023(3) 0.030(3) 0.003(3) -0.002(3) 0.004(2) C6 0.042(4) 0.040(4) 0.028(3) -0.001(3) 0.000(3) 0.007(3) C16 0.034(3) 0.026(3) 0.032(3) 0.003(3) 0.009(3) -0.001(2) C15 0.025(3) 0.033(3) 0.034(3) -0.003(3) 0.005(3) 0.003(2) C64 0.030(3) 0.028(3) 0.038(3) -0.004(3) 0.012(3) -0.001(2) C13 0.032(3) 0.034(3) 0.026(3) 0.002(3) 0.001(3) 0.002(3) C38 0.043(4) 0.037(3) 0.029(3) -0.001(3) 0.006(3) 0.003(3) C53 0.026(3) 0.045(4) 0.030(3) 0.002(3) 0.008(3) 0.003(3) C26 0.038(4) 0.033(3) 0.036(4) 0.005(3) 0.003(3) -0.001(3) C8 0.031(3) 0.038(4) 0.041(4) 0.001(3) 0.004(3) -0.003(3) C32 0.037(4) 0.039(4) 0.034(4) -0.003(3) 0.000(3) 0.004(3) C46\ 0.037(3) 0.026(3) 0.029(3) 0.003(3) 0.010(3) 0.000(2) C24 0.042(4) 0.032(3) 0.044(4) 0.011(3) 0.021(3) 0.000(3) C11 0.028(3) 0.030(3) 0.036(3) 0.002(3) 0.004(3) -0.003(2) C2 0.056(5) 0.035(4) 0.033(4) 0.003(3) 0.000(3) -0.005(3) C7 0.029(3) 0.052(4) 0.046(4) 0.005(4) 0.012(3) -0.001(3) C30 0.027(3) 0.043(4) 0.059(5) 0.014(4) 0.003(3) 0.009(3) C57 0.028(3) 0.038(3) 0.027(3) 0.006(3) 0.004(3) 0.003(3) C5 0.036(4) 0.041(4) 0.034(4) 0.010(3) 0.006(3) 0.011(3) C52 0.023(3) 0.037(3) 0.032(3) 0.004(3) 0.002(3) 0.005(2) C55 0.048(4) 0.043(4) 0.040(4) 0.000(3) 0.005(3) -0.008(3) C59 0.032(3) 0.028(3) 0.041(4) -0.001(3) 0.006(3) 0.006(2) C29 0.037(4) 0.043(4) 0.055(4) 0.007(4) 0.014(3) 0.005(3) C48 0.028(3) 0.040(4) 0.039(4) 0.006(3) 0.005(3) 0.003(3) C42 0.036(4) 0.036(3) 0.045(4) -0.016(3) 0.016(3) -0.007(3) C17 0.029(3) 0.026(3) 0.031(3) 0.000(3) 0.005(3) -0.005(2) C9 0.030(3) 0.026(3) 0.038(4) 0.004(3) 0.006(3) -0.001(2) C47 0.029(3) 0.033(3) 0.027(3) -0.004(3) 0.003(3) 0.000(2) C63 0.033(4) 0.039(4) 0.036(4) 0.002(3) 0.007(3) 0.003(3) C37 0.030(4) 0.052(4) 0.049(4) -0.006(4) 0.013(3) 0.003(3) C62 0.036(4) 0.047(4) 0.041(4) 0.004(3) 0.001(3) 0.005(3) C25 0.047(4) 0.037(4) 0.040(4) 0.003(3) 0.013(3) 0.013(3) C28 0.032(3) 0.034(3) 0.034(3) 0.003(3) 0.007(3) 0.005(3) C40 0.054(5) 0.038(4) 0.050(4) -0.004(3) 0.023(4) -0.006(3) C31 0.043(4) 0.037(4) 0.049(4) -0.005(3) -0.002(3) -0.005(3) C45 0.031(3) 0.035(3) 0.041(4) 0.003(3) 0.005(3) 0.004(3) C23 0.042(4) 0.038(4) 0.053(4) 0.000(3) 0.017(3) -0.001(3) C61 0.028(3) 0.032(3) 0.051(4) -0.001(3) 0.001(3) -0.001(3) C60 0.040(4) 0.028(3) 0.050(4) 0.001(3) 0.013(3) -0.007(3) C19 0.033(4) 0.040(4) 0.046(4) 0.002(3) 0.013(3) 0.005(3) C34 0.032(4) 0.069(5) 0.042(4) -0.012(4) 0.000(3) -0.009(3) C18 0.051(4) 0.042(4) 0.045(4) 0.001(3) 0.003(3) 0.012(3) C56 0.049(4) 0.045(4) 0.044(4) 0.004(3) 0.012(3) -0.005(3) C22 0.036(3) 0.027(3) 0.039(4) 0.000(3) 0.011(3) 0.001(3) C69 0.035(4) 0.051(4) 0.038(4) -0.008(3) 0.001(3) 0.003(3) C36 0.030(4) 0.062(5) 0.034(4) 0.002(4) -0.001(3) -0.008(3) C4 0.048(4) 0.049(4) 0.034(4) 0.006(3) 0.018(3) 0.011(3) C39 0.056(5) 0.038(4) 0.038(4) 0.004(3) 0.012(3) -0.003(3) C65 0.036(4) 0.052(4) 0.038(4) -0.005(3) 0.005(3) -0.003(3) C3 0.070(5) 0.044(4) 0.031(4) 0.003(3) 0.019(4) 0.007(4) C41 0.043(4) 0.046(4) 0.041(4) 0.002(3) 0.017(3) -0.005(3) C67 0.054(5) 0.044(4) 0.055(5) -0.013(4) 0.022(4) 0.002(3) C66 0.039(4) 0.046(4) 0.068(5) -0.006(4) 0.014(4) 0.007(3) C35 0.033(4) 0.048(4) 0.066(5) 0.009(4) 0.010(4) -0.011(3) C33 0.021(3) 0.065(5) 0.049(4) 0.005(4) 0.002(3) 0.003(3) C68 0.060(5) 0.055(4) 0.035(4) -0.011(4) 0.016(4) 0.004(4) C71 0.038(5) 0.109(9) 0.084(7) 0.054(7) 0.003(5) 0.010(5) C73 0.027(4) 0.054(5) 0.150(11) 0.045(6) 0.006(5) -0.001(3) C74 0.033(4) 0.120(9) 0.056(5) -0.015(6) 0.014(4) -0.002(5) C72 0.037(5) 0.134(10) 0.057(6) -0.048(6) -0.006(4) 0.003(5) C70 0.045(5) 0.075(7) 0.127(10) -0.010(7) 0.015(6) 0.021(5) _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 Ti2 O2 1.962(4) . ? Ti2 N3 2.143(5) . ? Ti2 C73 2.349(8) . ? Ti2 C72 2.356(8) . ? Ti2 C74 2.373(8) . ? Ti2 C70 2.373(9) . ? Ti2 N4 2.389(5) . ? Ti2 C71 2.406(9) . ? Ti2 Cl3 2.444(2) . ? Ti2 Cl4 2.451(2) . ? O1 C1 1.344(8) . ? O1 Ti1 1.948(4) . ? N1 C9 1.350(8) . ? N1 C6 1.360(8) . ? N1 Ti1 2.127(5) . ? Ti1 C37 2.348(7) . ? Ti1 C36 2.372(7) . ? Ti1 N2 2.402(5) . ? Ti1 C33 2.406(7) . ? Ti1 C35 2.419(7) . ? Ti1 C34 2.426(7) . ? Ti1 Cl2 2.4518(18) . ? Ti1 Cl1 2.4528(19) . ? O2 C38 1.325(8) . ? N2 C10 1.287(7) . ? N2 C12 1.450(8) . ? N3 C46\ 1.312(8) . ? N3 C43 1.336(8) . ? N4 C47 1.294(8) . ? N4 C49 1.471(8) . ? C49 C50 1.383(8) . ? C49 C54 1.395(9) . ? C10 C9 1.465(9) . ? C10 C11 1.511(8) . ? C21 C26 1.366(9) . ? C21 C22 1.391(9) . ? C21 C20 1.518(8) . ? C50 C51 1.387(9) . ? C50 C55 1.511(9) . ? C1 C2 1.375(9) . ? C1 C6 1.402(9) . ? C54 C53 1.428(9) . ? C54 C57 1.540(8) . ? C12 C17 1.400(9) . ? C12 C13 1.436(8) . ? C51 C52 1.373(9) . ? C51 H51A 0.9500 . ? C58 C63 1.398(9) . ? C58 C59 1.411(9) . ? C58 C57 1.531(8) . ? C44 C45 1.381(9) . ? C44 C42 1.412(10) . ? C44 H44A 0.9500 . ? C27 C32 1.374(9) . ? C27 C28 1.428(9) . ? C27 C20 1.524(8) . ? C14 C13 1.377(9) . ? C14 C15 1.385(9) . ? C14 H14A 0.9500 . ? C43 C42 1.399(9) . ? C43 C38 1.447(9) . ? C20 C17 1.519(8) . ? C20 H20A 1.0000 . ? C6 C5 1.435(9) . ? C16 C15 1.392(8) . ? C16 C17 1.399(8) . ? C16 H16A 0.9500 . ? C15 C19 1.521(9) . ? C64 C65 1.377(9) . ? C64 C69 1.393(9) . ? C64 C57 1.515(8) . ? C13 C18 1.524(9) . ? C38 C39 1.397(9) . ? C53 C52 1.376(9) . ? C53 H53A 0.9500 . ? C26 C25 1.409(9) . ? C26 H26A 0.9500 . ? C8 C7 1.372(10) . ? C8 C9 1.394(9) . ? C8 H8A 0.9500 . ? C32 C31 1.387(10) . ? C32 H32A 0.9500 . ? C46\ C45 1.407(9) . ? C46\ C47 1.480(8) . ? C24 C25 1.341(10) . ? C24 C23 1.397(10) . ? C24 H24A 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C2 C3 1.403(11) . ? C2 H2A 0.9500 . ? C7 C5 1.411(10) . ? C7 H7A 0.9500 . ? C30 C31 1.365(10) . ? C30 C29 1.389(10) . ? C30 H30A 0.9500 . ? C57 H57A 1.0000 . ? C5 C4 1.435(10) . ? C52 C56 1.532(9) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C59 C60 1.359(9) . ? C59 H59A 0.9500 . ? C29 C28 1.374(9) . ? C29 H29A 0.9500 . ? C48 C47 1.533(8) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C42 C41 1.439(10) . ? C63 C62 1.379(9) . ? C63 H63A 0.9500 . ? C37 C36 1.395(10) . ? C37 C33 1.407(10) . ? C37 H37A 1.0000 . ? C62 C61 1.383(10) . ? C62 H62A 0.9500 . ? C25 H25A 0.9500 . ? C28 H28A 0.9500 . ? C40 C41 1.372(10) . ? C40 C39 1.397(10) . ? C40 H40A 0.9500 . ? C31 H31A 0.9500 . ? C45 H45A 0.9500 . ? C23 C22 1.375(9) . ? C23 H23A 0.9500 . ? C61 C60 1.397(9) . ? C61 H61A 0.9500 . ? C60 H60A 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C34 C33 1.376(11) . ? C34 C35 1.393(11) . ? C34 H34A 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C22 H22A 0.9500 . ? C69 C68 1.393(10) . ? C69 H69A 0.9500 . ? C36 C35 1.402(11) . ? C36 H36A 1.0000 . ? C4 C3 1.350(11) . ? C4 H4A 0.9500 . ? C39 H39A 0.9500 . ? C65 C66 1.401(10) . ? C65 H65A 0.9500 . ? C3 H3A 0.9500 . ? C41 H41A 0.9500 . ? C67 C68 1.365(11) . ? C67 C66 1.365(11) . ? C67 H67A 0.9500 . ? C66 H66A 0.9500 . ? C35 H35A 1.0000 . ? C33 H33A 1.0000 . ? C68 H68A 0.9500 . ? C71 C70 1.301(15) . ? C71 C72 1.402(15) . ? C71 H71A 1.0000 . ? C73 C74 1.328(14) . ? C73 C72 1.444(14) . ? C73 H73A 1.0000 . ? C74 C70 1.292(15) . ? C74 H74A 1.0000 . ? C72 H72A 1.0000 . ? C70 H70A 1.0000 . ? 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 Ti2 N3 77.30(19) . . ? O2 Ti2 C73 125.2(3) . . ? N3 Ti2 C73 149.3(2) . . ? O2 Ti2 C72 89.6(3) . . ? N3 Ti2 C72 150.3(3) . . ? C73 Ti2 C72 35.8(4) . . ? O2 Ti2 C74 128.3(3) . . ? N3 Ti2 C74 149.9(3) . . ? C73 Ti2 C74 32.7(3) . . ? C72 Ti2 C74 56.4(3) . . ? O2 Ti2 C70 98.0(4) . . ? N3 Ti2 C70 152.5(3) . . ? C73 Ti2 C70 53.6(4) . . ? C72 Ti2 C70 54.9(4) . . ? C74 Ti2 C70 31.6(4) . . ? O2 Ti2 N4 146.60(18) . . ? N3 Ti2 N4 69.31(18) . . ? C73 Ti2 N4 86.4(3) . . ? C72 Ti2 N4 120.2(3) . . ? C74 Ti2 N4 83.7(3) . . ? C70 Ti2 N4 111.2(4) . . ? O2 Ti2 C71 75.9(3) . . ? N3 Ti2 C71 152.8(3) . . ? C73 Ti2 C71 55.9(3) . . ? C72 Ti2 C71 34.2(4) . . ? C74 Ti2 C71 53.8(3) . . ? C70 Ti2 C71 31.6(4) . . ? N4 Ti2 C71 137.2(3) . . ? O2 Ti2 Cl3 88.79(15) . . ? N3 Ti2 Cl3 75.12(14) . . ? C73 Ti2 Cl3 84.1(3) . . ? C72 Ti2 Cl3 78.1(3) . . ? C74 Ti2 Cl3 116.0(3) . . ? C70 Ti2 Cl3 132.3(3) . . ? N4 Ti2 Cl3 83.52(13) . . ? C71 Ti2 Cl3 108.9(3) . . ? O2 Ti2 Cl4 85.37(15) . . ? N3 Ti2 Cl4 77.10(14) . . ? C73 Ti2 Cl4 121.2(3) . . ? C72 Ti2 Cl4 128.9(3) . . ? C74 Ti2 Cl4 88.5(3) . . ? C70 Ti2 Cl4 75.5(3) . . ? N4 Ti2 Cl4 86.55(12) . . ? C71 Ti2 Cl4 96.0(3) . . ? Cl3 Ti2 Cl4 152.23(7) . . ? C1 O1 Ti1 119.2(4) . . ? C9 N1 C6 121.3(5) . . ? C9 N1 Ti1 126.2(4) . . ? C6 N1 Ti1 112.5(4) . . ? O1 Ti1 N1 77.47(19) . . ? O1 Ti1 C37 127.1(2) . . ? N1 Ti1 C37 147.5(2) . . ? O1 Ti1 C36 129.6(2) . . ? N1 Ti1 C36 147.5(2) . . ? C37 Ti1 C36 34.4(3) . . ? O1 Ti1 N2 146.09(18) . . ? N1 Ti1 N2 68.62(17) . . ? C37 Ti1 N2 84.8(2) . . ? C36 Ti1 N2 82.6(2) . . ? O1 Ti1 C33 92.8(2) . . ? N1 Ti1 C33 151.5(2) . . ? C37 Ti1 C33 34.4(2) . . ? C36 Ti1 C33 56.5(2) . . ? N2 Ti1 C33 117.3(2) . . ? O1 Ti1 C35 96.4(2) . . ? N1 Ti1 C35 151.3(2) . . ? C37 Ti1 C35 56.5(3) . . ? C36 Ti1 C35 34.0(3) . . ? N2 Ti1 C35 113.0(2) . . ? C33 Ti1 C35 55.5(3) . . ? O1 Ti1 C34 76.1(2) . . ? N1 Ti1 C34 153.5(2) . . ? C37 Ti1 C34 56.4(3) . . ? C36 Ti1 C34 56.3(2) . . ? N2 Ti1 C34 137.8(2) . . ? C33 Ti1 C34 33.1(3) . . ? C35 Ti1 C34 33.4(3) . . ? O1 Ti1 Cl2 86.16(14) . . ? N1 Ti1 Cl2 76.52(14) . . ? C37 Ti1 Cl2 121.18(19) . . ? C36 Ti1 Cl2 86.84(18) . . ? N2 Ti1 Cl2 85.60(12) . . ? C33 Ti1 Cl2 130.1(2) . . ? C35 Ti1 Cl2 75.09(19) . . ? C34 Ti1 Cl2 100.0(2) . . ? O1 Ti1 Cl1 88.99(14) . . ? N1 Ti1 Cl1 75.26(14) . . ? C37 Ti1 Cl1 83.44(19) . . ? C36 Ti1 Cl1 117.04(19) . . ? N2 Ti1 Cl1 83.04(12) . . ? C33 Ti1 Cl1 77.85(19) . . ? C35 Ti1 Cl1 133.14(19) . . ? C34 Ti1 Cl1 105.8(2) . . ? Cl2 Ti1 Cl1 151.75(7) . . ? C38 O2 Ti2 118.8(4) . . ? C10 N2 C12 118.9(5) . . ? C10 N2 Ti1 115.6(4) . . ? C12 N2 Ti1 125.3(3) . . ? C46\ N3 C43 120.7(5) . . ? C46\ N3 Ti2 125.4(4) . . ? C43 N3 Ti2 113.9(4) . . ? C47 N4 C49 118.3(5) . . ? C47 N4 Ti2 114.4(4) . . ? C49 N4 Ti2 127.0(4) . . ? C50 C49 C54 122.3(6) . . ? C50 C49 N4 120.0(5) . . ? C54 C49 N4 117.8(5) . . ? N2 C10 C9 117.0(5) . . ? N2 C10 C11 125.6(5) . . ? C9 C10 C11 117.3(5) . . ? C26 C21 C22 117.3(6) . . ? C26 C21 C20 123.5(6) . . ? C22 C21 C20 119.2(5) . . ? C49 C50 C51 118.1(6) . . ? C49 C50 C55 124.0(6) . . ? C51 C50 C55 117.9(5) . . ? O1 C1 C2 127.6(6) . . ? O1 C1 C6 115.4(6) . . ? C2 C1 C6 117.0(6) . . ? C49 C54 C53 117.1(5) . . ? C49 C54 C57 121.5(5) . . ? C53 C54 C57 121.4(5) . . ? C17 C12 C13 119.6(6) . . ? C17 C12 N2 119.9(5) . . ? C13 C12 N2 120.4(5) . . ? C52 C51 C50 122.1(6) . . ? C52 C51 H51A 119.0 . . ? C50 C51 H51A 119.0 . . ? C63 C58 C59 117.5(6) . . ? C63 C58 C57 122.8(6) . . ? C59 C58 C57 119.7(5) . . ? C45 C44 C42 119.7(6) . . ? C45 C44 H44A 120.2 . . ? C42 C44 H44A 120.2 . . ? C32 C27 C28 115.4(6) . . ? C32 C27 C20 125.8(6) . . ? C28 C27 C20 118.9(5) . . ? C13 C14 C15 123.2(5) . . ? C13 C14 H14A 118.4 . . ? C15 C14 H14A 118.4 . . ? N3 C43 C42 123.2(6) . . ? N3 C43 C38 113.3(6) . . ? C42 C43 C38 123.5(6) . . ? C21 C20 C17 113.2(5) . . ? C21 C20 C27 113.6(5) . . ? C17 C20 C27 111.3(5) . . ? C21 C20 H20A 106.0 . . ? C17 C20 H20A 106.0 . . ? C27 C20 H20A 106.0 . . ? N1 C6 C1 115.0(6) . . ? N1 C6 C5 120.7(6) . . ? C1 C6 C5 124.2(6) . . ? C15 C16 C17 122.7(6) . . ? C15 C16 H16A 118.6 . . ? C17 C16 H16A 118.6 . . ? C14 C15 C16 117.3(6) . . ? C14 C15 C19 121.7(5) . . ? C16 C15 C19 120.9(6) . . ? C65 C64 C69 117.1(6) . . ? C65 C64 C57 119.2(6) . . ? C69 C64 C57 123.7(6) . . ? C14 C13 C12 118.4(6) . . ? C14 C13 C18 120.5(6) . . ? C12 C13 C18 120.9(6) . . ? O2 C38 C39 126.0(6) . . ? O2 C38 C43 116.5(6) . . ? C39 C38 C43 117.4(6) . . ? C52 C53 C54 120.8(6) . . ? C52 C53 H53A 119.6 . . ? C54 C53 H53A 119.6 . . ? C21 C26 C25 120.4(6) . . ? C21 C26 H26A 119.8 . . ? C25 C26 H26A 119.8 . . ? C7 C8 C9 120.0(6) . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C27 C32 C31 123.3(6) . . ? C27 C32 H32A 118.3 . . ? C31 C32 H32A 118.3 . . ? N3 C46\ C45 120.7(6) . . ? N3 C46\ C47 112.8(5) . . ? C45 C46\ C47 126.5(6) . . ? C25 C24 C23 119.5(6) . . ? C25 C24 H24A 120.3 . . ? C23 C24 H24A 120.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 C2 C3 120.5(7) . . ? C1 C2 H2A 119.8 . . ? C3 C2 H2A 119.8 . . ? C8 C7 C5 121.0(6) . . ? C8 C7 H7A 119.5 . . ? C5 C7 H7A 119.5 . . ? C31 C30 C29 118.6(6) . . ? C31 C30 H30A 120.7 . . ? C29 C30 H30A 120.7 . . ? C64 C57 C58 114.6(5) . . ? C64 C57 C54 112.3(5) . . ? C58 C57 C54 110.8(5) . . ? C64 C57 H57A 106.2 . . ? C58 C57 H57A 106.2 . . ? C54 C57 H57A 106.2 . . ? C7 C5 C4 128.3(6) . . ? C7 C5 C6 116.6(6) . . ? C4 C5 C6 115.0(6) . . ? C51 C52 C53 119.5(6) . . ? C51 C52 C56 121.4(6) . . ? C53 C52 C56 119.1(6) . . ? C50 C55 H55A 109.5 . . ? C50 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C50 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C60 C59 C58 120.9(6) . . ? C60 C59 H59A 119.6 . . ? C58 C59 H59A 119.6 . . ? C28 C29 C30 121.0(7) . . ? C28 C29 H29A 119.5 . . ? C30 C29 H29A 119.5 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C43 C42 C44 116.1(6) . . ? C43 C42 C41 117.4(6) . . ? C44 C42 C41 126.5(6) . . ? C16 C17 C12 118.6(5) . . ? C16 C17 C20 121.5(5) . . ? C12 C17 C20 119.9(5) . . ? N1 C9 C8 120.4(6) . . ? N1 C9 C10 112.1(5) . . ? C8 C9 C10 127.5(6) . . ? N4 C47 C46\ 117.2(5) . . ? N4 C47 C48 124.7(5) . . ? C46\ C47 C48 118.0(5) . . ? C62 C63 C58 121.2(6) . . ? C62 C63 H63A 119.4 . . ? C58 C63 H63A 119.4 . . ? C36 C37 C33 107.6(7) . . ? C36 C37 Ti1 73.8(4) . . ? C33 C37 Ti1 75.0(4) . . ? C36 C37 H37A 125.7 . . ? C33 C37 H37A 125.7 . . ? Ti1 C37 H37A 125.7 . . ? C63 C62 C61 120.6(6) . . ? C63 C62 H62A 119.7 . . ? C61 C62 H62A 119.7 . . ? C24 C25 C26 121.4(7) . . ? C24 C25 H25A 119.3 . . ? C26 C25 H25A 119.3 . . ? C29 C28 C27 121.3(6) . . ? C29 C28 H28A 119.4 . . ? C27 C28 H28A 119.4 . . ? C41 C40 C39 125.8(7) . . ? C41 C40 H40A 117.1 . . ? C39 C40 H40A 117.1 . . ? C30 C31 C32 120.3(7) . . ? C30 C31 H31A 119.8 . . ? C32 C31 H31A 119.8 . . ? C44 C45 C46\ 119.5(6) . . ? C44 C45 H45A 120.3 . . ? C46\ C45 H45A 120.3 . . ? C22 C23 C24 118.7(7) . . ? C22 C23 H23A 120.6 . . ? C24 C23 H23A 120.6 . . ? C62 C61 C60 118.5(6) . . ? C62 C61 H61A 120.7 . . ? C60 C61 H61A 120.7 . . ? C59 C60 C61 121.3(6) . . ? C59 C60 H60A 119.4 . . ? C61 C60 H60A 119.4 . . ? C15 C19 H19A 109.5 . . ? C15 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C15 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C33 C34 C35 108.3(7) . . ? C33 C34 Ti1 72.6(4) . . ? C35 C34 Ti1 73.0(4) . . ? C33 C34 H34A 125.7 . . ? C35 C34 H34A 125.7 . . ? Ti1 C34 H34A 125.7 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C52 C56 H56A 109.5 . . ? C52 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C52 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C23 C22 C21 122.7(6) . . ? C23 C22 H22A 118.7 . . ? C21 C22 H22A 118.7 . . ? C68 C69 C64 120.8(7) . . ? C68 C69 H69A 119.6 . . ? C64 C69 H69A 119.6 . . ? C37 C36 C35 107.6(6) . . ? C37 C36 Ti1 71.9(4) . . ? C35 C36 Ti1 74.8(4) . . ? C37 C36 H36A 125.9 . . ? C35 C36 H36A 125.9 . . ? Ti1 C36 H36A 125.9 . . ? C3 C4 C5 120.1(7) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C40 C39 C38 118.1(7) . . ? C40 C39 H39A 120.9 . . ? C38 C39 H39A 120.9 . . ? C64 C65 C66 122.6(7) . . ? C64 C65 H65A 118.7 . . ? C66 C65 H65A 118.7 . . ? C4 C3 C2 123.0(7) . . ? C4 C3 H3A 118.5 . . ? C2 C3 H3A 118.5 . . ? C40 C41 C42 117.8(7) . . ? C40 C41 H41A 121.1 . . ? C42 C41 H41A 121.1 . . ? C68 C67 C66 120.9(7) . . ? C68 C67 H67A 119.5 . . ? C66 C67 H67A 119.5 . . ? C67 C66 C65 118.4(7) . . ? C67 C66 H66A 120.8 . . ? C65 C66 H66A 120.8 . . ? C34 C35 C36 108.1(7) . . ? C34 C35 Ti1 73.6(4) . . ? C36 C35 Ti1 71.2(4) . . ? C34 C35 H35A 125.8 . . ? C36 C35 H35A 125.8 . . ? Ti1 C35 H35A 125.8 . . ? C34 C33 C37 108.3(7) . . ? C34 C33 Ti1 74.3(4) . . ? C37 C33 Ti1 70.6(4) . . ? C34 C33 H33A 125.7 . . ? C37 C33 H33A 125.7 . . ? Ti1 C33 H33A 125.7 . . ? C67 C68 C69 120.2(7) . . ? C67 C68 H68A 119.9 . . ? C69 C68 H68A 119.9 . . ? C70 C71 C72 107.6(9) . . ? C70 C71 Ti2 72.8(5) . . ? C72 C71 Ti2 70.9(5) . . ? C70 C71 H71A 126.1 . . ? C72 C71 H71A 126.1 . . ? Ti2 C71 H71A 126.1 . . ? C74 C73 C72 107.4(8) . . ? C74 C73 Ti2 74.7(5) . . ? C72 C73 Ti2 72.4(5) . . ? C74 C73 H73A 126.0 . . ? C72 C73 H73A 126.0 . . ? Ti2 C73 H73A 126.0 . . ? C70 C74 C73 108.8(10) . . ? C70 C74 Ti2 74.2(6) . . ? C73 C74 Ti2 72.7(5) . . ? C70 C74 H74A 125.4 . . ? C73 C74 H74A 125.4 . . ? Ti2 C74 H74A 125.4 . . ? C71 C72 C73 103.2(8) . . ? C71 C72 Ti2 74.9(5) . . ? C73 C72 Ti2 71.8(5) . . ? C71 C72 H72A 127.7 . . ? C73 C72 H72A 127.7 . . ? Ti2 C72 H72A 127.7 . . ? C74 C70 C71 113.0(11) . . ? C74 C70 Ti2 74.2(5) . . ? C71 C70 Ti2 75.6(6) . . ? C74 C70 H70A 123.3 . . ? C71 C70 H70A 123.3 . . ? Ti2 C70 H70A 123.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 O1 Ti1 N1 5.5(4) . . . . ? C1 O1 Ti1 C37 161.7(4) . . . . ? C1 O1 Ti1 C36 -154.2(4) . . . . ? C1 O1 Ti1 N2 4.8(6) . . . . ? C1 O1 Ti1 C33 158.5(4) . . . . ? C1 O1 Ti1 C35 -146.0(4) . . . . ? C1 O1 Ti1 C34 -172.7(5) . . . . ? C1 O1 Ti1 Cl2 -71.5(4) . . . . ? C1 O1 Ti1 Cl1 80.7(4) . . . . ? C9 N1 Ti1 O1 177.5(5) . . . . ? C6 N1 Ti1 O1 -4.5(4) . . . . ? C9 N1 Ti1 C37 34.4(7) . . . . ? C6 N1 Ti1 C37 -147.6(5) . . . . ? C9 N1 Ti1 C36 -32.3(7) . . . . ? C6 N1 Ti1 C36 145.7(5) . . . . ? C9 N1 Ti1 N2 -2.9(4) . . . . ? C6 N1 Ti1 N2 175.1(4) . . . . ? C9 N1 Ti1 C33 105.3(6) . . . . ? C6 N1 Ti1 C33 -76.7(6) . . . . ? C9 N1 Ti1 C35 -102.1(6) . . . . ? C6 N1 Ti1 C35 75.9(7) . . . . ? C9 N1 Ti1 C34 -178.7(5) . . . . ? C6 N1 Ti1 C34 -0.7(7) . . . . ? C9 N1 Ti1 Cl2 -93.4(5) . . . . ? C6 N1 Ti1 Cl2 84.6(4) . . . . ? C9 N1 Ti1 Cl1 85.3(5) . . . . ? C6 N1 Ti1 Cl1 -96.7(4) . . . . ? N3 Ti2 O2 C38 4.7(4) . . . . ? C73 Ti2 O2 C38 161.6(5) . . . . ? C72 Ti2 O2 C38 157.8(5) . . . . ? C74 Ti2 O2 C38 -157.5(5) . . . . ? C70 Ti2 O2 C38 -147.7(5) . . . . ? N4 Ti2 O2 C38 3.4(6) . . . . ? C71 Ti2 O2 C38 -170.5(6) . . . . ? Cl3 Ti2 O2 C38 79.7(4) . . . . ? Cl4 Ti2 O2 C38 -73.1(4) . . . . ? O1 Ti1 N2 C10 6.5(6) . . . . ? N1 Ti1 N2 C10 5.7(4) . . . . ? C37 Ti1 N2 C10 -155.2(4) . . . . ? C36 Ti1 N2 C10 170.3(4) . . . . ? C33 Ti1 N2 C10 -143.6(4) . . . . ? C35 Ti1 N2 C10 154.7(4) . . . . ? C34 Ti1 N2 C10 -177.1(4) . . . . ? Cl2 Ti1 N2 C10 82.9(4) . . . . ? Cl1 Ti1 N2 C10 -71.1(4) . . . . ? O1 Ti1 N2 C12 -178.5(4) . . . . ? N1 Ti1 N2 C12 -179.4(5) . . . . ? C37 Ti1 N2 C12 19.8(4) . . . . ? C36 Ti1 N2 C12 -14.7(4) . . . . ? C33 Ti1 N2 C12 31.4(5) . . . . ? C35 Ti1 N2 C12 -30.4(5) . . . . ? C34 Ti1 N2 C12 -2.2(6) . . . . ? Cl2 Ti1 N2 C12 -102.1(4) . . . . ? Cl1 Ti1 N2 C12 103.8(4) . . . . ? O2 Ti2 N3 C46\ 176.1(5) . . . . ? C73 Ti2 N3 C46\ 35.1(9) . . . . ? C72 Ti2 N3 C46\ 110.3(8) . . . . ? C74 Ti2 N3 C46\ -32.5(9) . . . . ? C70 Ti2 N3 C46\ -101.1(9) . . . . ? N4 Ti2 N3 C46\ -4.7(5) . . . . ? C71 Ti2 N3 C46\ -173.7(8) . . . . ? Cl3 Ti2 N3 C46\ 83.9(5) . . . . ? Cl4 Ti2 N3 C46\ -95.8(5) . . . . ? O2 Ti2 N3 C43 -3.1(4) . . . . ? C73 Ti2 N3 C43 -144.1(7) . . . . ? C72 Ti2 N3 C43 -68.9(8) . . . . ? C74 Ti2 N3 C43 148.3(7) . . . . ? C70 Ti2 N3 C43 79.7(9) . . . . ? N4 Ti2 N3 C43 176.2(5) . . . . ? C71 Ti2 N3 C43 7.2(10) . . . . ? Cl3 Ti2 N3 C43 -95.3(4) . . . . ? Cl4 Ti2 N3 C43 85.0(4) . . . . ? O2 Ti2 N4 C47 9.1(6) . . . . ? N3 Ti2 N4 C47 7.7(4) . . . . ? C73 Ti2 N4 C47 -153.2(5) . . . . ? C72 Ti2 N4 C47 -140.9(5) . . . . ? C74 Ti2 N4 C47 174.1(5) . . . . ? C70 Ti2 N4 C47 158.2(5) . . . . ? C71 Ti2 N4 C47 -179.6(6) . . . . ? Cl3 Ti2 N4 C47 -68.8(4) . . . . ? Cl4 Ti2 N4 C47 85.3(4) . . . . ? O2 Ti2 N4 C49 -177.0(4) . . . . ? N3 Ti2 N4 C49 -178.3(5) . . . . ? C73 Ti2 N4 C49 20.7(5) . . . . ? C72 Ti2 N4 C49 33.0(6) . . . . ? C74 Ti2 N4 C49 -12.0(5) . . . . ? C70 Ti2 N4 C49 -27.8(6) . . . . ? C71 Ti2 N4 C49 -5.7(7) . . . . ? Cl3 Ti2 N4 C49 105.2(4) . . . . ? Cl4 Ti2 N4 C49 -100.8(4) . . . . ? C47 N4 C49 C50 85.2(7) . . . . ? Ti2 N4 C49 C50 -88.6(6) . . . . ? C47 N4 C49 C54 -93.9(7) . . . . ? Ti2 N4 C49 C54 92.4(6) . . . . ? C12 N2 C10 C9 177.0(5) . . . . ? Ti1 N2 C10 C9 -7.8(6) . . . . ? C12 N2 C10 C11 -3.6(8) . . . . ? Ti1 N2 C10 C11 171.7(4) . . . . ? C54 C49 C50 C51 -4.8(9) . . . . ? N4 C49 C50 C51 176.2(5) . . . . ? C54 C49 C50 C55 173.9(6) . . . . ? N4 C49 C50 C55 -5.1(9) . . . . ? Ti1 O1 C1 C2 174.0(5) . . . . ? Ti1 O1 C1 C6 -5.7(7) . . . . ? C50 C49 C54 C53 5.2(9) . . . . ? N4 C49 C54 C53 -175.8(5) . . . . ? C50 C49 C54 C57 -173.9(5) . . . . ? N4 C49 C54 C57 5.1(8) . . . . ? C10 N2 C12 C17 -95.6(7) . . . . ? Ti1 N2 C12 C17 89.6(6) . . . . ? C10 N2 C12 C13 86.5(7) . . . . ? Ti1 N2 C12 C13 -88.3(6) . . . . ? C49 C50 C51 C52 0.5(9) . . . . ? C55 C50 C51 C52 -178.3(6) . . . . ? C46\ N3 C43 C42 3.8(9) . . . . ? Ti2 N3 C43 C42 -176.9(5) . . . . ? C46\ N3 C43 C38 -178.0(5) . . . . ? Ti2 N3 C43 C38 1.2(7) . . . . ? C26 C21 C20 C17 -82.2(7) . . . . ? C22 C21 C20 C17 95.9(6) . . . . ? C26 C21 C20 C27 46.0(8) . . . . ? C22 C21 C20 C27 -135.9(6) . . . . ? C32 C27 C20 C21 -78.3(7) . . . . ? C28 C27 C20 C21 102.7(6) . . . . ? C32 C27 C20 C17 50.8(8) . . . . ? C28 C27 C20 C17 -128.2(6) . . . . ? C9 N1 C6 C1 -179.0(5) . . . . ? Ti1 N1 C6 C1 2.9(7) . . . . ? C9 N1 C6 C5 0.0(9) . . . . ? Ti1 N1 C6 C5 -178.1(5) . . . . ? O1 C1 C6 N1 1.4(8) . . . . ? C2 C1 C6 N1 -178.3(5) . . . . ? O1 C1 C6 C5 -177.5(6) . . . . ? C2 C1 C6 C5 2.8(10) . . . . ? C13 C14 C15 C16 -0.7(9) . . . . ? C13 C14 C15 C19 175.7(6) . . . . ? C17 C16 C15 C14 -0.3(9) . . . . ? C17 C16 C15 C19 -176.7(6) . . . . ? C15 C14 C13 C12 2.8(9) . . . . ? C15 C14 C13 C18 -173.1(6) . . . . ? C17 C12 C13 C14 -4.0(9) . . . . ? N2 C12 C13 C14 173.9(5) . . . . ? C17 C12 C13 C18 172.0(6) . . . . ? N2 C12 C13 C18 -10.1(9) . . . . ? Ti2 O2 C38 C39 174.3(5) . . . . ? Ti2 O2 C38 C43 -5.6(7) . . . . ? N3 C43 C38 O2 2.6(8) . . . . ? C42 C43 C38 O2 -179.3(6) . . . . ? N3 C43 C38 C39 -177.3(6) . . . . ? C42 C43 C38 C39 0.9(9) . . . . ? C49 C54 C53 C52 -1.3(9) . . . . ? C57 C54 C53 C52 177.8(5) . . . . ? C22 C21 C26 C25 -1.3(9) . . . . ? C20 C21 C26 C25 176.9(6) . . . . ? C28 C27 C32 C31 -1.7(9) . . . . ? C20 C27 C32 C31 179.2(6) . . . . ? C43 N3 C46\ C45 -1.2(9) . . . . ? Ti2 N3 C46\ C45 179.7(4) . . . . ? C43 N3 C46\ C47 -179.6(5) . . . . ? Ti2 N3 C46\ C47 1.3(7) . . . . ? O1 C1 C2 C3 -178.7(6) . . . . ? C6 C1 C2 C3 1.0(9) . . . . ? C9 C8 C7 C5 1.4(10) . . . . ? C65 C64 C57 C58 -152.4(6) . . . . ? C69 C64 C57 C58 29.5(9) . . . . ? C65 C64 C57 C54 80.2(7) . . . . ? C69 C64 C57 C54 -98.0(7) . . . . ? C63 C58 C57 C64 -76.5(8) . . . . ? C59 C58 C57 C64 104.0(7) . . . . ? C63 C58 C57 C54 51.8(8) . . . . ? C59 C58 C57 C54 -127.8(6) . . . . ? C49 C54 C57 C64 -156.7(5) . . . . ? C53 C54 C57 C64 24.3(8) . . . . ? C49 C54 C57 C58 73.8(7) . . . . ? C53 C54 C57 C58 -105.2(6) . . . . ? C8 C7 C5 C4 -176.3(6) . . . . ? C8 C7 C5 C6 0.0(10) . . . . ? N1 C6 C5 C7 -0.7(9) . . . . ? C1 C6 C5 C7 178.1(6) . . . . ? N1 C6 C5 C4 176.1(6) . . . . ? C1 C6 C5 C4 -5.1(9) . . . . ? C50 C51 C52 C53 3.3(9) . . . . ? C50 C51 C52 C56 -177.8(6) . . . . ? C54 C53 C52 C51 -2.8(9) . . . . ? C54 C53 C52 C56 178.2(6) . . . . ? C63 C58 C59 C60 1.6(9) . . . . ? C57 C58 C59 C60 -178.8(6) . . . . ? C31 C30 C29 C28 -1.1(10) . . . . ? N3 C43 C42 C44 -3.6(9) . . . . ? C38 C43 C42 C44 178.3(6) . . . . ? N3 C43 C42 C41 176.0(6) . . . . ? C38 C43 C42 C41 -2.0(9) . . . . ? C45 C44 C42 C43 0.9(9) . . . . ? C45 C44 C42 C41 -178.7(6) . . . . ? C15 C16 C17 C12 -0.9(9) . . . . ? C15 C16 C17 C20 178.3(5) . . . . ? C13 C12 C17 C16 3.0(8) . . . . ? N2 C12 C17 C16 -174.9(5) . . . . ? C13 C12 C17 C20 -176.1(5) . . . . ? N2 C12 C17 C20 6.0(8) . . . . ? C21 C20 C17 C16 29.3(8) . . . . ? C27 C20 C17 C16 -100.1(6) . . . . ? C21 C20 C17 C12 -151.6(5) . . . . ? C27 C20 C17 C12 79.1(7) . . . . ? C6 N1 C9 C8 1.5(9) . . . . ? Ti1 N1 C9 C8 179.4(4) . . . . ? C6 N1 C9 C10 -177.7(5) . . . . ? Ti1 N1 C9 C10 0.2(7) . . . . ? C7 C8 C9 N1 -2.2(9) . . . . ? C7 C8 C9 C10 176.8(6) . . . . ? N2 C10 C9 N1 5.4(7) . . . . ? C11 C10 C9 N1 -174.1(5) . . . . ? N2 C10 C9 C8 -173.8(6) . . . . ? C11 C10 C9 C8 6.8(9) . . . . ? C49 N4 C47 C46\ 175.5(5) . . . . ? Ti2 N4 C47 C46\ -10.0(7) . . . . ? C49 N4 C47 C48 -7.1(9) . . . . ? Ti2 N4 C47 C48 167.4(5) . . . . ? N3 C46\ C47 N4 6.4(8) . . . . ? C45 C46\ C47 N4 -171.9(6) . . . . ? N3 C46\ C47 C48 -171.2(5) . . . . ? C45 C46\ C47 C48 10.5(9) . . . . ? C59 C58 C63 C62 -2.7(10) . . . . ? C57 C58 C63 C62 177.7(6) . . . . ? O1 Ti1 C37 C36 108.2(4) . . . . ? N1 Ti1 C37 C36 -119.1(5) . . . . ? N2 Ti1 C37 C36 -84.5(4) . . . . ? C33 Ti1 C37 C36 113.8(6) . . . . ? C35 Ti1 C37 C36 37.5(4) . . . . ? C34 Ti1 C37 C36 77.9(5) . . . . ? Cl2 Ti1 C37 C36 -2.9(5) . . . . ? Cl1 Ti1 C37 C36 -168.1(4) . . . . ? O1 Ti1 C37 C33 -5.7(6) . . . . ? N1 Ti1 C37 C33 127.0(5) . . . . ? C36 Ti1 C37 C33 -113.8(6) . . . . ? N2 Ti1 C37 C33 161.6(5) . . . . ? C35 Ti1 C37 C33 -76.3(5) . . . . ? C34 Ti1 C37 C33 -35.9(4) . . . . ? Cl2 Ti1 C37 C33 -116.7(4) . . . . ? Cl1 Ti1 C37 C33 78.0(4) . . . . ? C58 C63 C62 C61 2.7(10) . . . . ? C23 C24 C25 C26 -2.6(10) . . . . ? C21 C26 C25 C24 2.6(10) . . . . ? C30 C29 C28 C27 1.4(10) . . . . ? C32 C27 C28 C29 0.0(9) . . . . ? C20 C27 C28 C29 179.1(6) . . . . ? C29 C30 C31 C32 -0.7(10) . . . . ? C27 C32 C31 C30 2.2(11) . . . . ? C42 C44 C45 C46\ 1.5(9) . . . . ? N3 C46\ C45 C44 -1.5(9) . . . . ? C47 C46\ C45 C44 176.7(6) . . . . ? C25 C24 C23 C22 1.5(10) . . . . ? C63 C62 C61 C60 -1.5(10) . . . . ? C58 C59 C60 C61 -0.5(10) . . . . ? C62 C61 C60 C59 0.4(10) . . . . ? O1 Ti1 C34 C33 -118.1(5) . . . . ? N1 Ti1 C34 C33 -121.9(6) . . . . ? C37 Ti1 C34 C33 37.4(4) . . . . ? C36 Ti1 C34 C33 79.0(5) . . . . ? N2 Ti1 C34 C33 63.9(6) . . . . ? C35 Ti1 C34 C33 116.1(7) . . . . ? Cl2 Ti1 C34 C33 158.4(4) . . . . ? Cl1 Ti1 C34 C33 -33.3(5) . . . . ? O1 Ti1 C34 C35 125.8(5) . . . . ? N1 Ti1 C34 C35 122.0(6) . . . . ? C37 Ti1 C34 C35 -78.7(5) . . . . ? C36 Ti1 C34 C35 -37.1(5) . . . . ? N2 Ti1 C34 C35 -52.2(6) . . . . ? C33 Ti1 C34 C35 -116.1(7) . . . . ? Cl2 Ti1 C34 C35 42.3(5) . . . . ? Cl1 Ti1 C34 C35 -149.4(4) . . . . ? C24 C23 C22 C21 -0.4(10) . . . . ? C26 C21 C22 C23 0.3(9) . . . . ? C20 C21 C22 C23 -178.0(6) . . . . ? C65 C64 C69 C68 -1.1(10) . . . . ? C57 C64 C69 C68 177.1(6) . . . . ? C33 C37 C36 C35 1.1(8) . . . . ? Ti1 C37 C36 C35 -66.8(5) . . . . ? C33 C37 C36 Ti1 68.0(5) . . . . ? O1 Ti1 C36 C37 -100.1(5) . . . . ? N1 Ti1 C36 C37 118.9(5) . . . . ? N2 Ti1 C36 C37 91.5(4) . . . . ? C33 Ti1 C36 C37 -38.3(4) . . . . ? C35 Ti1 C36 C37 -114.7(6) . . . . ? C34 Ti1 C36 C37 -78.3(5) . . . . ? Cl2 Ti1 C36 C37 177.5(4) . . . . ? Cl1 Ti1 C36 C37 13.3(5) . . . . ? O1 Ti1 C36 C35 14.6(5) . . . . ? N1 Ti1 C36 C35 -126.3(5) . . . . ? C37 Ti1 C36 C35 114.7(6) . . . . ? N2 Ti1 C36 C35 -153.7(4) . . . . ? C33 Ti1 C36 C35 76.4(5) . . . . ? C34 Ti1 C36 C35 36.4(4) . . . . ? Cl2 Ti1 C36 C35 -67.8(4) . . . . ? Cl1 Ti1 C36 C35 128.0(4) . . . . ? C7 C5 C4 C3 -179.9(7) . . . . ? C6 C5 C4 C3 3.8(9) . . . . ? C41 C40 C39 C38 -2.3(11) . . . . ? O2 C38 C39 C40 -178.6(6) . . . . ? C43 C38 C39 C40 1.2(9) . . . . ? C69 C64 C65 C66 0.7(10) . . . . ? C57 C64 C65 C66 -177.6(6) . . . . ? C5 C4 C3 C2 -0.4(11) . . . . ? C1 C2 C3 C4 -2.2(11) . . . . ? C39 C40 C41 C42 1.1(11) . . . . ? C43 C42 C41 C40 1.0(9) . . . . ? C44 C42 C41 C40 -179.4(6) . . . . ? C68 C67 C66 C65 -0.9(12) . . . . ? C64 C65 C66 C67 0.3(11) . . . . ? C33 C34 C35 C36 -1.3(8) . . . . ? Ti1 C34 C35 C36 63.2(5) . . . . ? C33 C34 C35 Ti1 -64.5(5) . . . . ? C37 C36 C35 C34 0.1(8) . . . . ? Ti1 C36 C35 C34 -64.8(5) . . . . ? C37 C36 C35 Ti1 64.9(5) . . . . ? O1 Ti1 C35 C34 -52.4(5) . . . . ? N1 Ti1 C35 C34 -128.0(5) . . . . ? C37 Ti1 C35 C34 78.3(5) . . . . ? C36 Ti1 C35 C34 116.3(7) . . . . ? N2 Ti1 C35 C34 144.8(4) . . . . ? C33 Ti1 C35 C34 36.5(5) . . . . ? Cl2 Ti1 C35 C34 -136.7(5) . . . . ? Cl1 Ti1 C35 C34 42.2(6) . . . . ? O1 Ti1 C35 C36 -168.7(4) . . . . ? N1 Ti1 C35 C36 115.7(5) . . . . ? C37 Ti1 C35 C36 -37.9(4) . . . . ? N2 Ti1 C35 C36 28.5(5) . . . . ? C33 Ti1 C35 C36 -79.8(5) . . . . ? C34 Ti1 C35 C36 -116.3(7) . . . . ? Cl2 Ti1 C35 C36 107.0(4) . . . . ? Cl1 Ti1 C35 C36 -74.1(5) . . . . ? C35 C34 C33 C37 2.0(8) . . . . ? Ti1 C34 C33 C37 -62.8(5) . . . . ? C35 C34 C33 Ti1 64.8(5) . . . . ? C36 C37 C33 C34 -2.0(8) . . . . ? Ti1 C37 C33 C34 65.2(5) . . . . ? C36 C37 C33 Ti1 -67.1(5) . . . . ? O1 Ti1 C33 C34 59.0(5) . . . . ? N1 Ti1 C33 C34 127.5(5) . . . . ? C37 Ti1 C33 C34 -116.5(7) . . . . ? C36 Ti1 C33 C34 -78.2(5) . . . . ? N2 Ti1 C33 C34 -137.2(4) . . . . ? C35 Ti1 C33 C34 -36.9(4) . . . . ? Cl2 Ti1 C33 C34 -28.4(5) . . . . ? Cl1 Ti1 C33 C34 147.3(5) . . . . ? O1 Ti1 C33 C37 175.5(4) . . . . ? N1 Ti1 C33 C37 -116.0(5) . . . . ? C36 Ti1 C33 C37 38.3(4) . . . . ? N2 Ti1 C33 C37 -20.7(5) . . . . ? C35 Ti1 C33 C37 79.6(5) . . . . ? C34 Ti1 C33 C37 116.5(7) . . . . ? Cl2 Ti1 C33 C37 88.1(5) . . . . ? Cl1 Ti1 C33 C37 -96.2(4) . . . . ? C66 C67 C68 C69 0.5(12) . . . . ? C64 C69 C68 C67 0.5(12) . . . . ? O2 Ti2 C71 C70 133.0(8) . . . . ? N3 Ti2 C71 C70 122.6(8) . . . . ? C73 Ti2 C71 C70 -74.6(8) . . . . ? C72 Ti2 C71 C70 -116.2(10) . . . . ? C74 Ti2 C71 C70 -34.4(7) . . . . ? N4 Ti2 C71 C70 -42.1(10) . . . . ? Cl3 Ti2 C71 C70 -143.3(7) . . . . ? Cl4 Ti2 C71 C70 49.3(8) . . . . ? O2 Ti2 C71 C72 -110.8(7) . . . . ? N3 Ti2 C71 C72 -121.2(7) . . . . ? C73 Ti2 C71 C72 41.6(6) . . . . ? C74 Ti2 C71 C72 81.8(7) . . . . ? C70 Ti2 C71 C72 116.2(10) . . . . ? N4 Ti2 C71 C72 74.1(9) . . . . ? Cl3 Ti2 C71 C72 -27.1(7) . . . . ? Cl4 Ti2 C71 C72 165.5(6) . . . . ? O2 Ti2 C73 C74 107.9(7) . . . . ? N3 Ti2 C73 C74 -120.8(7) . . . . ? C72 Ti2 C73 C74 114.3(8) . . . . ? C70 Ti2 C73 C74 35.8(6) . . . . ? N4 Ti2 C73 C74 -84.0(7) . . . . ? C71 Ti2 C73 C74 74.6(7) . . . . ? Cl3 Ti2 C73 C74 -167.8(7) . . . . ? Cl4 Ti2 C73 C74 -0.2(7) . . . . ? O2 Ti2 C73 C72 -6.4(8) . . . . ? N3 Ti2 C73 C72 124.9(6) . . . . ? C74 Ti2 C73 C72 -114.3(8) . . . . ? C70 Ti2 C73 C72 -78.5(7) . . . . ? N4 Ti2 C73 C72 161.7(6) . . . . ? C71 Ti2 C73 C72 -39.7(6) . . . . ? Cl3 Ti2 C73 C72 77.9(6) . . . . ? Cl4 Ti2 C73 C72 -114.5(7) . . . . ? C72 C73 C74 C70 -0.4(10) . . . . ? Ti2 C73 C74 C70 -66.0(7) . . . . ? C72 C73 C74 Ti2 65.5(6) . . . . ? O2 Ti2 C74 C70 18.7(8) . . . . ? N3 Ti2 C74 C70 -124.8(7) . . . . ? C73 Ti2 C74 C70 116.0(9) . . . . ? C72 Ti2 C74 C70 76.3(7) . . . . ? N4 Ti2 C74 C70 -150.8(7) . . . . ? C71 Ti2 C74 C70 34.4(7) . . . . ? Cl3 Ti2 C74 C70 129.5(7) . . . . ? Cl4 Ti2 C74 C70 -64.2(7) . . . . ? O2 Ti2 C74 C73 -97.3(7) . . . . ? N3 Ti2 C74 C73 119.2(6) . . . . ? C72 Ti2 C74 C73 -39.7(6) . . . . ? C70 Ti2 C74 C73 -116.0(9) . . . . ? N4 Ti2 C74 C73 93.1(6) . . . . ? C71 Ti2 C74 C73 -81.6(7) . . . . ? Cl3 Ti2 C74 C73 13.5(7) . . . . ? Cl4 Ti2 C74 C73 179.8(6) . . . . ? C70 C71 C72 C73 -2.7(10) . . . . ? Ti2 C71 C72 C73 -66.7(5) . . . . ? C70 C71 C72 Ti2 64.0(7) . . . . ? C74 C73 C72 C71 1.9(9) . . . . ? Ti2 C73 C72 C71 69.0(6) . . . . ? C74 C73 C72 Ti2 -67.1(6) . . . . ? O2 Ti2 C72 C71 65.0(7) . . . . ? N3 Ti2 C72 C71 127.9(6) . . . . ? C73 Ti2 C72 C71 -109.7(8) . . . . ? C74 Ti2 C72 C71 -73.5(7) . . . . ? C70 Ti2 C72 C71 -35.0(6) . . . . ? N4 Ti2 C72 C71 -131.0(7) . . . . ? Cl3 Ti2 C72 C71 153.9(7) . . . . ? Cl4 Ti2 C72 C71 -18.7(8) . . . . ? O2 Ti2 C72 C73 174.7(6) . . . . ? N3 Ti2 C72 C73 -122.4(6) . . . . ? C74 Ti2 C72 C73 36.2(6) . . . . ? C70 Ti2 C72 C73 74.7(6) . . . . ? N4 Ti2 C72 C73 -21.2(7) . . . . ? C71 Ti2 C72 C73 109.7(8) . . . . ? Cl3 Ti2 C72 C73 -96.4(6) . . . . ? Cl4 Ti2 C72 C73 91.0(7) . . . . ? C73 C74 C70 C71 -1.4(12) . . . . ? Ti2 C74 C70 C71 -66.4(8) . . . . ? C73 C74 C70 Ti2 65.0(6) . . . . ? C72 C71 C70 C74 2.7(12) . . . . ? Ti2 C71 C70 C74 65.5(7) . . . . ? C72 C71 C70 Ti2 -62.8(7) . . . . ? O2 Ti2 C70 C74 -165.3(7) . . . . ? N3 Ti2 C70 C74 117.0(8) . . . . ? C73 Ti2 C70 C74 -37.0(6) . . . . ? C72 Ti2 C70 C74 -81.4(7) . . . . ? N4 Ti2 C70 C74 31.3(7) . . . . ? C71 Ti2 C70 C74 -119.5(10) . . . . ? Cl3 Ti2 C70 C74 -69.6(9) . . . . ? Cl4 Ti2 C70 C74 111.7(7) . . . . ? O2 Ti2 C70 C71 -45.8(8) . . . . ? N3 Ti2 C70 C71 -123.6(8) . . . . ? C73 Ti2 C70 C71 82.4(8) . . . . ? C72 Ti2 C70 C71 38.0(7) . . . . ? C74 Ti2 C70 C71 119.5(10) . . . . ? N4 Ti2 C70 C71 150.8(7) . . . . ? Cl3 Ti2 C70 C71 49.9(10) . . . . ? Cl4 Ti2 C70 C71 -128.9(8) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.630 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.122 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.031 0.250 144 35 ' ' 2 0.000 0.030 0.750 144 35 ' ' 3 0.288 0.095 0.117 142 51 ' ' 4 0.288 -0.095 0.617 142 52 ' ' 5 0.712 0.095 0.383 142 53 ' ' 6 0.712 -0.095 0.883 142 53 ' ' 7 0.212 0.405 0.883 142 53 ' ' 8 0.788 0.405 0.617 142 52 ' ' 9 0.500 0.469 0.250 144 35 ' ' 10 0.500 0.530 0.750 144 35 ' ' 11 0.212 0.595 0.383 142 53 ' ' 12 0.788 0.595 0.117 142 51 ' ' _platon_squeeze_details ; ; #==END