# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef '2011_dalton.txt' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ying Mu' _publ_contact_author_email YMU@JLU.EDU.CN _publ_section_title ; Synthesis and Structures of (R)-Cyclopentadienyl-BINOL Titanium(IV) Complexes and Catalytic Properties for Olefin Polymerization ; loop_ _publ_author_name 'Ying Mu' 'Li Wang' 'Qiaolin Wu' 'Hao Xu' # Attachment 'CIFs.txt' data_complex4 _database_code_depnum_ccdc_archive 'CCDC 859491' #TrackingRef '2011_dalton.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H29 Cl3 N0 O2 Ti' _chemical_formula_weight 587.79 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 'P2(1)2(1)2(1) ' 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' _cell_length_a 8.4968(10) _cell_length_b 13.2926(16) _cell_length_c 24.819(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2803.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.618 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9184 _exptl_absorpt_correction_T_max 0.9580 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 9.0cm _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14631 _diffrn_reflns_av_R_equivalents 0.1224 _diffrn_reflns_av_sigmaI/netI 0.1563 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4964 _reflns_number_gt 2841 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0316P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.10(5) _refine_ls_number_reflns 4964 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1458 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.39919(14) 0.36858(8) 0.15688(5) 0.0332(3) Uani 1 1 d . . . Cl2 Cl 0.5869(2) 0.35414(16) 0.21891(7) 0.0577(6) Uani 1 1 d . . . Cl1 Cl 0.3637(2) 0.53393(11) 0.15143(8) 0.0491(5) Uani 1 1 d . . . Cl3 Cl 0.5237(2) 0.33319(13) 0.07946(7) 0.0514(5) Uani 1 1 d . . . O1 O 0.0404(5) 0.2033(3) 0.29219(16) 0.0305(11) Uani 1 1 d . . . O2 O -0.2659(5) 0.3539(3) 0.37732(17) 0.0414(12) Uani 1 1 d . . . C17 C 0.0987(7) 0.4295(4) 0.3751(2) 0.0213(15) Uani 1 1 d . . . C12 C 0.1887(6) 0.4894(4) 0.3391(3) 0.0267(16) Uani 1 1 d . . . C28 C -0.1946(8) 0.1482(5) 0.4724(3) 0.0368(18) Uani 1 1 d . . . H28 H -0.2484 0.1108 0.4994 0.044 Uiso 1 1 calc R . . C21 C -0.0356(8) 0.2641(5) 0.3968(3) 0.0263(16) Uani 1 1 d . . . C15 C 0.1112(8) 0.5634(5) 0.4405(3) 0.0374(17) Uani 1 1 d . . . H15 H 0.0837 0.5896 0.4749 0.045 Uiso 1 1 calc R . . C18 C 0.0511(7) 0.3314(5) 0.3589(2) 0.0280(17) Uani 1 1 d . . . C11 C 0.2242(7) 0.4520(5) 0.2871(2) 0.0287(16) Uani 1 1 d . . . H11 H 0.2855 0.4919 0.2632 0.034 Uiso 1 1 calc R . . C30 C -0.1922(8) 0.2792(5) 0.4067(3) 0.0327(18) Uani 1 1 d . . . C10 C 0.1714(6) 0.3583(4) 0.2701(2) 0.0228(15) Uani 1 1 d . . . C1 C 0.1947(7) 0.3202(4) 0.2149(3) 0.0268(16) Uani 1 1 d . . . C22 C 0.0455(7) 0.1875(4) 0.4250(2) 0.0229(15) Uani 1 1 d . . . C19 C 0.0877(8) 0.2989(4) 0.3079(2) 0.0284(16) Uani 1 1 d . . . C26 C 0.0438(10) 0.0497(5) 0.4906(3) 0.042(2) Uani 1 1 d . . . H26 H -0.0095 0.0112 0.5172 0.050 Uiso 1 1 calc R . . C27 C -0.0367(8) 0.1267(5) 0.4628(2) 0.0291(17) Uani 1 1 d . . . C16 C 0.0605(7) 0.4690(4) 0.4261(3) 0.0331(17) Uani 1 1 d . . . H16 H -0.0003 0.4303 0.4506 0.040 Uiso 1 1 calc R . . C6 C 0.3564(8) 0.1587(5) 0.2383(2) 0.043(2) Uani 1 1 d . . . H6A H 0.2820 0.1062 0.2493 0.065 Uiso 1 1 calc R . . H6B H 0.3929 0.1953 0.2702 0.065 Uiso 1 1 calc R . . H6C H 0.4466 0.1277 0.2202 0.065 Uiso 1 1 calc R . . C5 C 0.1234(7) 0.3602(4) 0.1675(2) 0.0286(15) Uani 1 1 d . . . C13 C 0.2387(8) 0.5850(5) 0.3565(3) 0.0381(18) Uani 1 1 d . . . H13 H 0.3003 0.6252 0.3329 0.046 Uiso 1 1 calc R . . C24 C 0.2821(8) 0.0888(5) 0.4419(3) 0.0369(19) Uani 1 1 d . . . H24 H 0.3900 0.0752 0.4350 0.044 Uiso 1 1 calc R . . C2 C 0.2766(7) 0.2303(4) 0.2006(3) 0.0280(17) Uani 1 1 d . . . C29 C -0.2762(8) 0.2208(5) 0.4449(3) 0.0371(19) Uani 1 1 d . . . H29 H -0.3851 0.2317 0.4512 0.044 Uiso 1 1 calc R . . C23 C 0.2063(8) 0.1651(5) 0.4153(3) 0.0326(17) Uani 1 1 d . . . H23 H 0.2630 0.2041 0.3898 0.039 Uiso 1 1 calc R . . C4 C 0.1642(8) 0.2985(5) 0.1243(3) 0.0332(18) Uani 1 1 d . . . C20 C -0.1072(9) 0.2031(5) 0.2651(3) 0.052(2) Uani 1 1 d . . . H20A H -0.1875 0.2331 0.2884 0.078 Uiso 1 1 calc R . . H20B H -0.1370 0.1337 0.2564 0.078 Uiso 1 1 calc R . . H20C H -0.0987 0.2422 0.2318 0.078 Uiso 1 1 calc R . . C14 C 0.2016(7) 0.6212(5) 0.4059(3) 0.0365(18) Uani 1 1 d . . . H14 H 0.2373 0.6858 0.4167 0.044 Uiso 1 1 calc R . . C31 C -0.4325(7) 0.3496(6) 0.3718(3) 0.053(2) Uani 1 1 d . . . H31A H -0.4633 0.2826 0.3591 0.080 Uiso 1 1 calc R . . H31B H -0.4669 0.4004 0.3457 0.080 Uiso 1 1 calc R . . H31C H -0.4820 0.3628 0.4067 0.080 Uiso 1 1 calc R . . C9 C 0.0093(7) 0.4464(4) 0.1654(2) 0.0381(18) Uani 1 1 d . . . H9A H 0.0341 0.4894 0.1345 0.057 Uiso 1 1 calc R . . H9B H 0.0173 0.4858 0.1987 0.057 Uiso 1 1 calc R . . H9C H -0.0980 0.4203 0.1617 0.057 Uiso 1 1 calc R . . C25 C 0.1972(9) 0.0305(5) 0.4795(3) 0.041(2) Uani 1 1 d . . . H25 H 0.2486 -0.0234 0.4974 0.050 Uiso 1 1 calc R . . C3 C 0.2575(8) 0.2180(4) 0.1438(3) 0.0330(17) Uani 1 1 d . . . C7 C 0.3170(8) 0.1284(5) 0.1130(2) 0.0428(19) Uani 1 1 d . . . H7A H 0.2405 0.0734 0.1156 0.064 Uiso 1 1 calc R . . H7B H 0.4179 0.1065 0.1281 0.064 Uiso 1 1 calc R . . H7C H 0.3315 0.1468 0.0751 0.064 Uiso 1 1 calc R . . C8 C 0.1130(8) 0.3132(5) 0.0665(2) 0.0462(19) Uani 1 1 d . . . H8A H -0.0003 0.3007 0.0635 0.069 Uiso 1 1 calc R . . H8B H 0.1702 0.2661 0.0433 0.069 Uiso 1 1 calc R . . H8C H 0.1359 0.3824 0.0553 0.069 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 0.0364(8) 0.0271(7) 0.0361(7) 0.0052(6) 0.0039(7) 0.0032(6) Cl2 0.0410(11) 0.0785(15) 0.0535(13) 0.0147(12) -0.0087(10) -0.0037(11) Cl1 0.0590(13) 0.0258(10) 0.0624(12) 0.0068(10) 0.0186(11) 0.0012(9) Cl3 0.0636(13) 0.0441(12) 0.0464(12) 0.0044(10) 0.0205(10) 0.0070(10) O1 0.035(3) 0.025(3) 0.032(3) 0.000(2) 0.001(2) -0.003(2) O2 0.031(3) 0.034(3) 0.059(3) 0.007(3) -0.001(2) 0.006(3) C17 0.022(4) 0.021(4) 0.021(4) 0.000(3) -0.002(3) 0.010(3) C12 0.024(4) 0.023(4) 0.033(4) 0.001(3) 0.002(3) 0.004(3) C28 0.050(5) 0.029(4) 0.032(4) 0.000(4) 0.013(4) -0.009(4) C21 0.031(4) 0.024(4) 0.025(4) 0.001(3) 0.008(3) 0.000(3) C15 0.040(4) 0.033(4) 0.040(4) -0.006(3) -0.005(4) 0.004(4) C18 0.028(4) 0.034(4) 0.022(4) 0.005(3) -0.002(3) 0.004(3) C11 0.027(4) 0.030(4) 0.030(4) 0.012(3) 0.005(3) 0.011(3) C30 0.042(5) 0.027(4) 0.029(5) -0.005(3) 0.005(4) -0.003(4) C10 0.024(4) 0.014(4) 0.030(4) 0.005(3) 0.004(3) 0.008(3) C1 0.029(4) 0.023(4) 0.028(4) 0.007(3) 0.001(3) -0.002(3) C22 0.032(4) 0.020(4) 0.017(4) -0.006(3) -0.003(3) -0.007(3) C19 0.035(4) 0.020(4) 0.030(4) 0.004(3) 0.000(4) -0.005(3) C26 0.067(6) 0.034(5) 0.026(4) 0.004(4) 0.003(4) -0.013(4) C27 0.042(5) 0.021(4) 0.024(4) 0.000(3) 0.009(3) -0.005(4) C16 0.033(5) 0.025(4) 0.041(4) 0.004(3) 0.000(4) -0.006(3) C6 0.060(5) 0.031(4) 0.038(4) 0.008(3) 0.007(4) 0.015(4) C5 0.037(4) 0.021(3) 0.028(4) 0.005(3) -0.001(3) 0.003(3) C13 0.044(5) 0.029(4) 0.042(5) 0.001(3) -0.001(4) 0.001(3) C24 0.038(5) 0.029(4) 0.043(5) -0.001(4) 0.002(4) 0.000(4) C2 0.034(4) 0.019(4) 0.032(4) 0.005(3) 0.007(4) -0.005(3) C29 0.031(4) 0.041(5) 0.039(5) -0.003(4) 0.014(4) -0.010(4) C23 0.040(5) 0.027(4) 0.031(4) 0.000(3) 0.002(4) 0.006(3) C4 0.043(5) 0.028(4) 0.028(4) 0.002(3) -0.002(3) -0.002(3) C20 0.057(5) 0.032(4) 0.067(6) 0.006(4) -0.022(5) -0.025(4) C14 0.040(4) 0.017(4) 0.053(5) -0.002(4) -0.003(4) -0.009(3) C31 0.035(5) 0.062(5) 0.062(5) -0.010(4) -0.007(4) 0.005(4) C9 0.032(4) 0.041(4) 0.041(5) 0.009(4) 0.001(4) 0.002(4) C25 0.067(6) 0.024(4) 0.033(5) 0.006(4) -0.015(4) -0.002(4) C3 0.040(4) 0.027(4) 0.032(5) 0.002(3) 0.003(4) 0.002(3) C7 0.058(5) 0.022(4) 0.048(5) -0.013(4) 0.001(4) 0.004(4) C8 0.051(5) 0.048(5) 0.039(5) 0.004(4) -0.007(4) 0.001(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 Cl1 2.2227(18) . ? Ti1 Cl2 2.225(2) . ? Ti1 Cl3 2.243(2) . ? Ti1 C1 2.347(6) . ? Ti1 C4 2.347(7) . ? Ti1 C3 2.358(6) . ? Ti1 C5 2.360(6) . ? Ti1 C2 2.375(6) . ? O1 C19 1.388(6) . ? O1 C20 1.423(7) . ? O2 C30 1.382(7) . ? O2 C31 1.423(7) . ? C17 C16 1.408(8) . ? C17 C12 1.420(8) . ? C17 C18 1.423(8) . ? C12 C13 1.407(7) . ? C12 C11 1.417(8) . ? C28 C29 1.370(8) . ? C28 C27 1.393(8) . ? C28 H28 0.9500 . ? C21 C30 1.368(8) . ? C21 C22 1.415(8) . ? C21 C18 1.492(8) . ? C15 C16 1.374(8) . ? C15 C14 1.385(8) . ? C15 H15 0.9500 . ? C18 C19 1.374(8) . ? C11 C10 1.389(8) . ? C11 H11 0.9500 . ? C30 C29 1.418(8) . ? C10 C19 1.417(7) . ? C10 C1 1.474(8) . ? C1 C5 1.426(7) . ? C1 C2 1.428(8) . ? C22 C23 1.419(8) . ? C22 C27 1.422(8) . ? C26 C25 1.356(9) . ? C26 C27 1.412(8) . ? C26 H26 0.9500 . ? C16 H16 0.9500 . ? C6 C2 1.498(8) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C5 C4 1.393(8) . ? C5 C9 1.503(7) . ? C13 C14 1.354(8) . ? C13 H13 0.9500 . ? C24 C23 1.370(8) . ? C24 C25 1.411(8) . ? C24 H24 0.9500 . ? C2 C3 1.426(8) . ? C29 H29 0.9500 . ? C23 H23 0.9500 . ? C4 C3 1.418(8) . ? C4 C8 1.510(8) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C14 H14 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C25 H25 0.9500 . ? C3 C7 1.504(8) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? 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 Cl1 Ti1 Cl2 102.98(9) . . ? Cl1 Ti1 Cl3 102.67(8) . . ? Cl2 Ti1 Cl3 103.68(9) . . ? Cl1 Ti1 C1 102.00(16) . . ? Cl2 Ti1 C1 94.72(16) . . ? Cl3 Ti1 C1 144.83(16) . . ? Cl1 Ti1 C4 104.83(18) . . ? Cl2 Ti1 C4 144.51(17) . . ? Cl3 Ti1 C4 91.31(17) . . ? C1 Ti1 C4 58.2(2) . . ? Cl1 Ti1 C3 139.63(18) . . ? Cl2 Ti1 C3 112.80(17) . . ? Cl3 Ti1 C3 86.86(16) . . ? C1 Ti1 C3 58.2(2) . . ? C4 Ti1 C3 35.1(2) . . ? Cl1 Ti1 C5 85.35(15) . . ? Cl2 Ti1 C5 129.07(15) . . ? Cl3 Ti1 C5 123.63(16) . . ? C1 Ti1 C5 35.28(18) . . ? C4 Ti1 C5 34.4(2) . . ? C3 Ti1 C5 57.9(2) . . ? Cl1 Ti1 C2 137.21(17) . . ? Cl2 Ti1 C2 86.08(17) . . ? Cl3 Ti1 C2 115.82(16) . . ? C1 Ti1 C2 35.21(19) . . ? C4 Ti1 C2 58.5(2) . . ? C3 Ti1 C2 35.1(2) . . ? C5 Ti1 C2 58.5(2) . . ? C19 O1 C20 113.0(4) . . ? C30 O2 C31 118.3(6) . . ? C16 C17 C12 118.7(5) . . ? C16 C17 C18 122.0(6) . . ? C12 C17 C18 119.3(6) . . ? C13 C12 C11 122.2(6) . . ? C13 C12 C17 118.4(6) . . ? C11 C12 C17 119.4(6) . . ? C29 C28 C27 123.1(7) . . ? C29 C28 H28 118.4 . . ? C27 C28 H28 118.4 . . ? C30 C21 C22 119.4(6) . . ? C30 C21 C18 120.4(6) . . ? C22 C21 C18 120.2(6) . . ? C16 C15 C14 121.2(6) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C19 C18 C17 119.0(6) . . ? C19 C18 C21 120.2(6) . . ? C17 C18 C21 120.8(6) . . ? C10 C11 C12 121.5(6) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C21 C30 O2 116.8(6) . . ? C21 C30 C29 122.0(7) . . ? O2 C30 C29 121.2(6) . . ? C11 C10 C19 117.5(5) . . ? C11 C10 C1 123.1(5) . . ? C19 C10 C1 119.4(5) . . ? C5 C1 C2 108.2(5) . . ? C5 C1 C10 125.6(5) . . ? C2 C1 C10 125.8(5) . . ? C5 C1 Ti1 72.9(3) . . ? C2 C1 Ti1 73.5(3) . . ? C10 C1 Ti1 125.2(4) . . ? C21 C22 C23 122.4(6) . . ? C21 C22 C27 119.8(6) . . ? C23 C22 C27 117.7(6) . . ? C18 C19 O1 118.8(6) . . ? C18 C19 C10 123.2(6) . . ? O1 C19 C10 118.0(5) . . ? C25 C26 C27 120.1(7) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C28 C27 C26 122.1(7) . . ? C28 C27 C22 118.0(6) . . ? C26 C27 C22 119.8(6) . . ? C15 C16 C17 120.1(6) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C5 C1 108.1(5) . . ? C4 C5 C9 125.6(6) . . ? C1 C5 C9 125.9(5) . . ? C4 C5 Ti1 72.3(4) . . ? C1 C5 Ti1 71.8(3) . . ? C9 C5 Ti1 126.9(4) . . ? C14 C13 C12 121.8(6) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C23 C24 C25 118.9(6) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C3 C2 C1 106.6(6) . . ? C3 C2 C6 126.6(6) . . ? C1 C2 C6 126.6(6) . . ? C3 C2 Ti1 71.8(3) . . ? C1 C2 Ti1 71.3(3) . . ? C6 C2 Ti1 125.4(4) . . ? C28 C29 C30 117.7(7) . . ? C28 C29 H29 121.2 . . ? C30 C29 H29 121.2 . . ? C24 C23 C22 121.8(6) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C5 C4 C3 108.6(6) . . ? C5 C4 C8 125.7(6) . . ? C3 C4 C8 125.7(6) . . ? C5 C4 Ti1 73.3(4) . . ? C3 C4 Ti1 72.9(4) . . ? C8 C4 Ti1 121.4(4) . . ? O1 C20 H20A 109.5 . . ? O1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C13 C14 C15 119.6(6) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? O2 C31 H31A 109.5 . . ? O2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C26 C25 C24 121.6(7) . . ? C26 C25 H25 119.2 . . ? C24 C25 H25 119.2 . . ? C4 C3 C2 108.4(6) . . ? C4 C3 C7 127.7(6) . . ? C2 C3 C7 123.7(6) . . ? C4 C3 Ti1 72.1(4) . . ? C2 C3 Ti1 73.1(4) . . ? C7 C3 Ti1 124.8(4) . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? 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 C16 C17 C12 C13 1.4(9) . . . . ? C18 C17 C12 C13 -178.1(5) . . . . ? C16 C17 C12 C11 -178.2(5) . . . . ? C18 C17 C12 C11 2.4(8) . . . . ? C16 C17 C18 C19 177.8(6) . . . . ? C12 C17 C18 C19 -2.8(9) . . . . ? C16 C17 C18 C21 -2.9(9) . . . . ? C12 C17 C18 C21 176.5(6) . . . . ? C30 C21 C18 C19 -103.9(8) . . . . ? C22 C21 C18 C19 79.8(8) . . . . ? C30 C21 C18 C17 76.8(8) . . . . ? C22 C21 C18 C17 -99.5(7) . . . . ? C13 C12 C11 C10 -178.7(6) . . . . ? C17 C12 C11 C10 0.8(8) . . . . ? C22 C21 C30 O2 -179.0(5) . . . . ? C18 C21 C30 O2 4.7(9) . . . . ? C22 C21 C30 C29 0.4(10) . . . . ? C18 C21 C30 C29 -175.9(6) . . . . ? C31 O2 C30 C21 158.2(6) . . . . ? C31 O2 C30 C29 -21.2(8) . . . . ? C12 C11 C10 C19 -3.4(8) . . . . ? C12 C11 C10 C1 174.9(5) . . . . ? C11 C10 C1 C5 -67.1(8) . . . . ? C19 C10 C1 C5 111.1(7) . . . . ? C11 C10 C1 C2 120.9(7) . . . . ? C19 C10 C1 C2 -60.9(8) . . . . ? C11 C10 C1 Ti1 26.4(8) . . . . ? C19 C10 C1 Ti1 -155.4(5) . . . . ? Cl1 Ti1 C1 C5 63.7(3) . . . . ? Cl2 Ti1 C1 C5 168.0(3) . . . . ? Cl3 Ti1 C1 C5 -70.0(4) . . . . ? C4 Ti1 C1 C5 -36.5(3) . . . . ? C3 Ti1 C1 C5 -78.0(4) . . . . ? C2 Ti1 C1 C5 -115.6(5) . . . . ? Cl1 Ti1 C1 C2 179.3(3) . . . . ? Cl2 Ti1 C1 C2 -76.3(4) . . . . ? Cl3 Ti1 C1 C2 45.6(5) . . . . ? C4 Ti1 C1 C2 79.2(4) . . . . ? C3 Ti1 C1 C2 37.6(4) . . . . ? C5 Ti1 C1 C2 115.6(5) . . . . ? Cl1 Ti1 C1 C10 -58.2(5) . . . . ? Cl2 Ti1 C1 C10 46.1(5) . . . . ? Cl3 Ti1 C1 C10 168.1(3) . . . . ? C4 Ti1 C1 C10 -158.4(6) . . . . ? C3 Ti1 C1 C10 160.1(6) . . . . ? C5 Ti1 C1 C10 -121.9(6) . . . . ? C2 Ti1 C1 C10 122.5(7) . . . . ? C30 C21 C22 C23 177.6(6) . . . . ? C18 C21 C22 C23 -6.0(9) . . . . ? C30 C21 C22 C27 0.7(9) . . . . ? C18 C21 C22 C27 177.1(5) . . . . ? C17 C18 C19 O1 -179.7(5) . . . . ? C21 C18 C19 O1 1.0(9) . . . . ? C17 C18 C19 C10 0.1(10) . . . . ? C21 C18 C19 C10 -179.2(6) . . . . ? C20 O1 C19 C18 93.5(7) . . . . ? C20 O1 C19 C10 -86.3(7) . . . . ? C11 C10 C19 C18 3.0(9) . . . . ? C1 C10 C19 C18 -175.3(6) . . . . ? C11 C10 C19 O1 -177.2(5) . . . . ? C1 C10 C19 O1 4.5(8) . . . . ? C29 C28 C27 C26 -178.2(6) . . . . ? C29 C28 C27 C22 4.1(10) . . . . ? C25 C26 C27 C28 179.2(6) . . . . ? C25 C26 C27 C22 -3.2(10) . . . . ? C21 C22 C27 C28 -2.8(9) . . . . ? C23 C22 C27 C28 -179.9(6) . . . . ? C21 C22 C27 C26 179.4(6) . . . . ? C23 C22 C27 C26 2.3(9) . . . . ? C14 C15 C16 C17 -0.7(10) . . . . ? C12 C17 C16 C15 -0.6(9) . . . . ? C18 C17 C16 C15 178.9(6) . . . . ? C2 C1 C5 C4 -1.9(7) . . . . ? C10 C1 C5 C4 -175.0(6) . . . . ? Ti1 C1 C5 C4 63.6(4) . . . . ? C2 C1 C5 C9 171.6(6) . . . . ? C10 C1 C5 C9 -1.5(9) . . . . ? Ti1 C1 C5 C9 -122.9(6) . . . . ? C2 C1 C5 Ti1 -65.5(4) . . . . ? C10 C1 C5 Ti1 121.4(6) . . . . ? Cl1 Ti1 C5 C4 124.9(4) . . . . ? Cl2 Ti1 C5 C4 -132.1(3) . . . . ? Cl3 Ti1 C5 C4 22.8(4) . . . . ? C1 Ti1 C5 C4 -116.6(5) . . . . ? C3 Ti1 C5 C4 -37.5(3) . . . . ? C2 Ti1 C5 C4 -79.1(4) . . . . ? Cl1 Ti1 C5 C1 -118.4(3) . . . . ? Cl2 Ti1 C5 C1 -15.5(4) . . . . ? Cl3 Ti1 C5 C1 139.4(3) . . . . ? C4 Ti1 C5 C1 116.6(5) . . . . ? C3 Ti1 C5 C1 79.1(4) . . . . ? C2 Ti1 C5 C1 37.6(3) . . . . ? Cl1 Ti1 C5 C9 3.3(5) . . . . ? Cl2 Ti1 C5 C9 106.2(5) . . . . ? Cl3 Ti1 C5 C9 -98.8(5) . . . . ? C1 Ti1 C5 C9 121.7(7) . . . . ? C4 Ti1 C5 C9 -121.6(7) . . . . ? C3 Ti1 C5 C9 -159.2(6) . . . . ? C2 Ti1 C5 C9 159.3(6) . . . . ? C11 C12 C13 C14 178.6(6) . . . . ? C17 C12 C13 C14 -0.9(9) . . . . ? C5 C1 C2 C3 1.5(7) . . . . ? C10 C1 C2 C3 174.6(5) . . . . ? Ti1 C1 C2 C3 -63.6(4) . . . . ? C5 C1 C2 C6 -174.2(6) . . . . ? C10 C1 C2 C6 -1.1(10) . . . . ? Ti1 C1 C2 C6 120.7(6) . . . . ? C5 C1 C2 Ti1 65.1(4) . . . . ? C10 C1 C2 Ti1 -121.8(6) . . . . ? Cl1 Ti1 C2 C3 114.4(4) . . . . ? Cl2 Ti1 C2 C3 -140.7(4) . . . . ? Cl3 Ti1 C2 C3 -37.4(4) . . . . ? C1 Ti1 C2 C3 115.4(6) . . . . ? C4 Ti1 C2 C3 37.2(4) . . . . ? C5 Ti1 C2 C3 77.8(4) . . . . ? Cl1 Ti1 C2 C1 -1.0(5) . . . . ? Cl2 Ti1 C2 C1 103.9(3) . . . . ? Cl3 Ti1 C2 C1 -152.8(3) . . . . ? C4 Ti1 C2 C1 -78.3(4) . . . . ? C3 Ti1 C2 C1 -115.4(6) . . . . ? C5 Ti1 C2 C1 -37.6(3) . . . . ? Cl1 Ti1 C2 C6 -123.1(5) . . . . ? Cl2 Ti1 C2 C6 -18.2(5) . . . . ? Cl3 Ti1 C2 C6 85.1(5) . . . . ? C1 Ti1 C2 C6 -122.1(7) . . . . ? C4 Ti1 C2 C6 159.6(6) . . . . ? C3 Ti1 C2 C6 122.5(7) . . . . ? C5 Ti1 C2 C6 -159.8(6) . . . . ? C27 C28 C29 C30 -3.0(10) . . . . ? C21 C30 C29 C28 0.6(10) . . . . ? O2 C30 C29 C28 180.0(6) . . . . ? C25 C24 C23 C22 0.5(10) . . . . ? C21 C22 C23 C24 -178.0(6) . . . . ? C27 C22 C23 C24 -1.0(9) . . . . ? C1 C5 C4 C3 1.5(7) . . . . ? C9 C5 C4 C3 -172.1(6) . . . . ? Ti1 C5 C4 C3 64.8(5) . . . . ? C1 C5 C4 C8 179.7(6) . . . . ? C9 C5 C4 C8 6.1(10) . . . . ? Ti1 C5 C4 C8 -117.0(6) . . . . ? C1 C5 C4 Ti1 -63.3(4) . . . . ? C9 C5 C4 Ti1 123.1(6) . . . . ? Cl1 Ti1 C4 C5 -57.7(4) . . . . ? Cl2 Ti1 C4 C5 82.8(4) . . . . ? Cl3 Ti1 C4 C5 -161.2(3) . . . . ? C1 Ti1 C4 C5 37.4(3) . . . . ? C3 Ti1 C4 C5 116.2(5) . . . . ? C2 Ti1 C4 C5 79.0(4) . . . . ? Cl1 Ti1 C4 C3 -173.9(3) . . . . ? Cl2 Ti1 C4 C3 -33.4(5) . . . . ? Cl3 Ti1 C4 C3 82.7(4) . . . . ? C1 Ti1 C4 C3 -78.8(4) . . . . ? C5 Ti1 C4 C3 -116.2(5) . . . . ? C2 Ti1 C4 C3 -37.1(4) . . . . ? Cl1 Ti1 C4 C8 64.3(5) . . . . ? Cl2 Ti1 C4 C8 -155.2(4) . . . . ? Cl3 Ti1 C4 C8 -39.2(5) . . . . ? C1 Ti1 C4 C8 159.4(6) . . . . ? C3 Ti1 C4 C8 -121.8(7) . . . . ? C5 Ti1 C4 C8 122.0(7) . . . . ? C2 Ti1 C4 C8 -159.0(6) . . . . ? C12 C13 C14 C15 -0.4(10) . . . . ? C16 C15 C14 C13 1.2(10) . . . . ? C27 C26 C25 C24 2.6(10) . . . . ? C23 C24 C25 C26 -1.3(10) . . . . ? C5 C4 C3 C2 -0.5(8) . . . . ? C8 C4 C3 C2 -178.7(6) . . . . ? Ti1 C4 C3 C2 64.6(5) . . . . ? C5 C4 C3 C7 174.4(6) . . . . ? C8 C4 C3 C7 -3.8(11) . . . . ? Ti1 C4 C3 C7 -120.5(7) . . . . ? C5 C4 C3 Ti1 -65.1(4) . . . . ? C8 C4 C3 Ti1 116.7(6) . . . . ? C1 C2 C3 C4 -0.6(7) . . . . ? C6 C2 C3 C4 175.1(6) . . . . ? Ti1 C2 C3 C4 -63.9(5) . . . . ? C1 C2 C3 C7 -175.8(6) . . . . ? C6 C2 C3 C7 0.0(11) . . . . ? Ti1 C2 C3 C7 121.0(6) . . . . ? C1 C2 C3 Ti1 63.2(4) . . . . ? C6 C2 C3 Ti1 -121.0(7) . . . . ? Cl1 Ti1 C3 C4 9.2(5) . . . . ? Cl2 Ti1 C3 C4 159.7(3) . . . . ? Cl3 Ti1 C3 C4 -96.8(4) . . . . ? C1 Ti1 C3 C4 78.6(4) . . . . ? C5 Ti1 C3 C4 36.8(4) . . . . ? C2 Ti1 C3 C4 116.4(6) . . . . ? Cl1 Ti1 C3 C2 -107.2(4) . . . . ? Cl2 Ti1 C3 C2 43.3(4) . . . . ? Cl3 Ti1 C3 C2 146.8(4) . . . . ? C1 Ti1 C3 C2 -37.8(4) . . . . ? C4 Ti1 C3 C2 -116.4(6) . . . . ? C5 Ti1 C3 C2 -79.6(4) . . . . ? Cl1 Ti1 C3 C7 133.1(5) . . . . ? Cl2 Ti1 C3 C7 -76.4(5) . . . . ? Cl3 Ti1 C3 C7 27.1(5) . . . . ? C1 Ti1 C3 C7 -157.5(6) . . . . ? C4 Ti1 C3 C7 123.9(7) . . . . ? C5 Ti1 C3 C7 160.7(6) . . . . ? C2 Ti1 C3 C7 -119.7(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.439 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.071 #===END data_complex5 _database_code_depnum_ccdc_archive 'CCDC 859492' #TrackingRef '2011_dalton.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H34 Br4 O2 Ti2' _chemical_formula_weight 938.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P4(1)2(1)2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 12.1649(4) _cell_length_b 12.1649(4) _cell_length_c 24.8696(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3680.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2265 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 4.809 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.379 _exptl_absorpt_correction_T_max 0.535 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20717 _diffrn_reflns_av_R_equivalents 0.0915 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.04 _reflns_number_total 3265 _reflns_number_gt 2511 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0372P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.016(15) _refine_ls_number_reflns 3265 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.51478(8) 0.22877(9) 0.08301(4) 0.0259(3) Uani 1 1 d . . . Br1 Br 0.61327(6) 0.36665(6) 0.03296(3) 0.0471(2) Uani 1 1 d . . . Br2 Br 0.61611(6) 0.06289(6) 0.06813(3) 0.0495(2) Uani 1 1 d . . . O1 O 0.3868(3) 0.2116(3) 0.04534(14) 0.0259(9) Uani 1 1 d . . . C1 C 0.3796(5) 0.2562(5) 0.1459(2) 0.0256(13) Uani 1 1 d . . . C2 C 0.4420(5) 0.1674(5) 0.1654(2) 0.0268(14) Uani 1 1 d . . . C3 C 0.5489(5) 0.2110(5) 0.1769(2) 0.0304(15) Uani 1 1 d . . . C4 C 0.5499(5) 0.3237(5) 0.1649(2) 0.0337(15) Uani 1 1 d . . . C5 C 0.4434(5) 0.3530(4) 0.1450(2) 0.0268(14) Uani 1 1 d . . . C6 C 0.4053(5) 0.0501(5) 0.1711(3) 0.0390(17) Uani 1 1 d . . . H6A H 0.3561 0.0438 0.2011 0.058 Uiso 1 1 calc R . . H6B H 0.4682 0.0039 0.1769 0.058 Uiso 1 1 calc R . . H6C H 0.3683 0.0274 0.1388 0.058 Uiso 1 1 calc R . . C7 C 0.6422(5) 0.1473(6) 0.2020(2) 0.0427(18) Uani 1 1 d . . . H7A H 0.7099 0.1864 0.1967 0.064 Uiso 1 1 calc R . . H7B H 0.6473 0.0762 0.1854 0.064 Uiso 1 1 calc R . . H7C H 0.6289 0.1386 0.2398 0.064 Uiso 1 1 calc R . . C8 C 0.6417(5) 0.4046(5) 0.1738(3) 0.0465(18) Uani 1 1 d . . . H8A H 0.6279 0.4457 0.2060 0.070 Uiso 1 1 calc R . . H8B H 0.6459 0.4539 0.1437 0.070 Uiso 1 1 calc R . . H8C H 0.7100 0.3657 0.1773 0.070 Uiso 1 1 calc R . . C9 C 0.4077(5) 0.4626(5) 0.1251(3) 0.0435(18) Uani 1 1 d . . . H9A H 0.3574 0.4533 0.0957 0.065 Uiso 1 1 calc R . . H9B H 0.4707 0.5034 0.1132 0.065 Uiso 1 1 calc R . . H9C H 0.3719 0.5019 0.1537 0.065 Uiso 1 1 calc R . . C10 C 0.2690(4) 0.2449(4) 0.1188(2) 0.0223(13) Uani 1 1 d . . . C11 C 0.1683(5) 0.2581(4) 0.1398(2) 0.0267(14) Uani 1 1 d . . . H11 H 0.1608 0.2739 0.1762 0.032 Uiso 1 1 calc R . . C12 C 0.0732(5) 0.2483(4) 0.1073(2) 0.0255(14) Uani 1 1 d . . . C13 C -0.0330(5) 0.2576(5) 0.1284(3) 0.0377(17) Uani 1 1 d . . . H13 H -0.0420 0.2729 0.1648 0.045 Uiso 1 1 calc R . . C14 C -0.1230(6) 0.2449(6) 0.0970(3) 0.054(2) Uani 1 1 d . . . H14 H -0.1928 0.2500 0.1121 0.064 Uiso 1 1 calc R . . C15 C -0.1113(5) 0.2240(6) 0.0418(3) 0.0479(19) Uani 1 1 d . . . H15 H -0.1731 0.2170 0.0201 0.058 Uiso 1 1 calc R . . C16 C -0.0095(5) 0.2142(5) 0.0206(2) 0.0350(16) Uani 1 1 d . . . H16 H -0.0028 0.1995 -0.0160 0.042 Uiso 1 1 calc R . . C17 C 0.0868(4) 0.2253(4) 0.0516(2) 0.0203(13) Uani 1 1 d . . . C18 C 0.1928(4) 0.2118(4) 0.0297(2) 0.0174(12) Uani 1 1 d . . . C19 C 0.2806(4) 0.2214(4) 0.0628(2) 0.0210(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0199(6) 0.0337(7) 0.0241(6) -0.0030(5) -0.0002(5) 0.0007(5) Br1 0.0407(4) 0.0578(5) 0.0426(4) 0.0047(4) 0.0096(3) -0.0090(4) Br2 0.0460(4) 0.0542(5) 0.0483(4) -0.0094(4) -0.0050(4) 0.0202(4) O1 0.024(2) 0.034(2) 0.019(2) -0.0034(17) 0.0035(19) 0.004(2) C1 0.025(3) 0.037(4) 0.014(3) -0.006(3) 0.001(3) -0.004(3) C2 0.031(3) 0.034(4) 0.015(3) -0.005(3) -0.001(3) 0.000(3) C3 0.027(3) 0.045(4) 0.020(3) -0.005(3) -0.001(3) -0.004(3) C4 0.026(3) 0.052(4) 0.023(3) -0.011(3) 0.004(3) -0.006(3) C5 0.039(4) 0.023(3) 0.018(3) -0.006(2) 0.005(3) -0.005(3) C6 0.039(4) 0.044(4) 0.035(4) 0.004(3) -0.006(3) -0.007(3) C7 0.027(4) 0.071(5) 0.030(4) 0.003(3) -0.010(3) -0.008(3) C8 0.037(4) 0.059(5) 0.043(4) -0.014(4) -0.007(3) -0.014(3) C9 0.044(4) 0.034(4) 0.052(5) -0.013(3) 0.011(4) 0.000(3) C10 0.025(3) 0.020(3) 0.022(3) -0.001(3) 0.000(3) -0.003(2) C11 0.036(4) 0.027(3) 0.017(3) -0.003(3) 0.002(3) -0.002(3) C12 0.024(3) 0.019(3) 0.034(4) 0.002(3) 0.005(3) 0.004(2) C13 0.028(4) 0.059(5) 0.027(3) -0.006(3) 0.007(3) 0.003(3) C14 0.024(4) 0.094(6) 0.043(4) 0.000(4) 0.010(3) -0.002(4) C15 0.027(4) 0.082(5) 0.035(4) -0.004(4) -0.001(3) 0.005(4) C16 0.028(4) 0.058(4) 0.019(3) -0.001(3) 0.006(3) 0.000(3) C17 0.024(3) 0.018(3) 0.019(3) 0.001(2) -0.004(2) -0.001(2) C18 0.021(3) 0.008(3) 0.023(3) 0.002(2) 0.002(3) 0.000(2) C19 0.018(3) 0.018(3) 0.027(3) 0.005(3) 0.006(3) -0.003(2) _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 1.829(4) . ? Ti1 C1 2.294(5) . ? Ti1 C5 2.327(5) . ? Ti1 C2 2.353(6) . ? Ti1 C4 2.380(6) . ? Ti1 C3 2.382(6) . ? Ti1 Br2 2.3934(13) . ? Ti1 Br1 2.4080(12) . ? O1 C19 1.369(6) . ? C1 C2 1.407(8) . ? C1 C5 1.410(7) . ? C1 C10 1.511(8) . ? C2 C3 1.434(7) . ? C2 C6 1.502(8) . ? C3 C4 1.404(8) . ? C3 C7 1.509(8) . ? C4 C5 1.432(8) . ? C4 C8 1.504(8) . ? C5 C9 1.487(8) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.343(7) . ? C10 C19 1.429(7) . ? C11 C12 1.417(8) . ? C11 H11 0.9300 . ? C12 C13 1.399(8) . ? C12 C17 1.424(7) . ? C13 C14 1.354(9) . ? C13 H13 0.9300 . ? C14 C15 1.403(9) . ? C14 H14 0.9300 . ? C15 C16 1.353(8) . ? C15 H15 0.9300 . ? C16 C17 1.409(7) . ? C16 H16 0.9300 . ? C17 C18 1.409(7) . ? C18 C19 1.353(7) . ? C18 C18 1.513(10) 7 ? 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 C1 75.86(18) . . ? O1 Ti1 C5 95.51(19) . . ? C1 Ti1 C5 35.51(18) . . ? O1 Ti1 C2 95.12(18) . . ? C1 Ti1 C2 35.21(19) . . ? C5 Ti1 C2 59.3(2) . . ? O1 Ti1 C4 130.30(18) . . ? C1 Ti1 C4 58.32(19) . . ? C5 Ti1 C4 35.41(19) . . ? C2 Ti1 C4 58.5(2) . . ? O1 Ti1 C3 129.82(18) . . ? C1 Ti1 C3 57.99(19) . . ? C5 Ti1 C3 58.3(2) . . ? C2 Ti1 C3 35.26(18) . . ? C4 Ti1 C3 34.3(2) . . ? O1 Ti1 Br2 105.24(12) . . ? C1 Ti1 Br2 126.69(15) . . ? C5 Ti1 Br2 147.36(15) . . ? C2 Ti1 Br2 93.48(15) . . ? C4 Ti1 Br2 116.68(16) . . ? C3 Ti1 Br2 89.14(15) . . ? O1 Ti1 Br1 103.79(12) . . ? C1 Ti1 Br1 127.42(15) . . ? C5 Ti1 Br1 94.36(14) . . ? C2 Ti1 Br1 149.13(14) . . ? C4 Ti1 Br1 90.84(15) . . ? C3 Ti1 Br1 118.90(15) . . ? Br2 Ti1 Br1 104.54(5) . . ? C19 O1 Ti1 129.2(3) . . ? C2 C1 C5 110.5(5) . . ? C2 C1 C10 124.3(5) . . ? C5 C1 C10 124.0(5) . . ? C2 C1 Ti1 74.7(3) . . ? C5 C1 Ti1 73.5(3) . . ? C10 C1 Ti1 108.7(3) . . ? C1 C2 C3 105.9(5) . . ? C1 C2 C6 127.1(5) . . ? C3 C2 C6 127.0(5) . . ? C1 C2 Ti1 70.1(3) . . ? C3 C2 Ti1 73.5(3) . . ? C6 C2 Ti1 119.7(4) . . ? C4 C3 C2 109.0(5) . . ? C4 C3 C7 125.7(5) . . ? C2 C3 C7 125.1(5) . . ? C4 C3 Ti1 72.7(3) . . ? C2 C3 Ti1 71.3(3) . . ? C7 C3 Ti1 125.6(4) . . ? C3 C4 C5 108.0(5) . . ? C3 C4 C8 127.8(6) . . ? C5 C4 C8 124.1(6) . . ? C3 C4 Ti1 72.9(3) . . ? C5 C4 Ti1 70.3(3) . . ? C8 C4 Ti1 125.2(4) . . ? C1 C5 C4 106.6(5) . . ? C1 C5 C9 126.4(5) . . ? C4 C5 C9 127.0(5) . . ? C1 C5 Ti1 70.9(3) . . ? C4 C5 Ti1 74.3(3) . . ? C9 C5 Ti1 118.1(4) . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C19 119.6(5) . . ? C11 C10 C1 128.9(5) . . ? C19 C10 C1 111.4(5) . . ? C10 C11 C12 120.8(5) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C13 C12 C11 122.1(5) . . ? C13 C12 C17 119.3(5) . . ? C11 C12 C17 118.5(5) . . ? C14 C13 C12 121.3(6) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 120.3(6) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 119.4(6) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C17 122.6(6) . . ? C15 C16 H16 118.7 . . ? C17 C16 H16 118.7 . . ? C16 C17 C18 122.6(5) . . ? C16 C17 C12 117.0(5) . . ? C18 C17 C12 120.3(5) . . ? C19 C18 C17 118.5(5) . . ? C19 C18 C18 119.1(5) . 7 ? C17 C18 C18 122.3(5) . 7 ? C18 C19 O1 123.0(5) . . ? C18 C19 C10 122.2(5) . . ? O1 C19 C10 114.8(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.476 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.093 #===END data_complex6 _database_code_depnum_ccdc_archive 'CCDC 859493' #TrackingRef '2011_dalton.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H24 Br2 O2 Ti' _chemical_formula_weight 612.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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' _cell_length_a 14.4117(6) _cell_length_b 15.2587(6) _cell_length_c 23.3763(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5140.5(4) _cell_formula_units_Z 8 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 3.466 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6811 _exptl_absorpt_correction_T_max 0.7231 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29033 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.03 _reflns_number_total 10135 _reflns_number_gt 7875 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0338P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.015(6) _refine_ls_number_reflns 10135 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0774 _refine_ls_wR_factor_gt 0.0720 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _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 Br1 Br 0.04911(3) 0.47003(4) 0.33221(2) 0.04825(14) Uani 1 1 d . . . Br2 Br 0.15689(4) 0.69685(3) 0.34375(2) 0.05110(14) Uani 1 1 d . . . Br3 Br 0.37036(3) 1.18380(3) 0.23549(2) 0.04364(13) Uani 1 1 d . . . Br4 Br 0.44872(3) 0.94714(3) 0.21047(2) 0.04451(13) Uani 1 1 d . . . C1 C 0.3374(2) 0.4835(3) 0.36561(16) 0.0258(9) Uani 1 1 d . . . C2 C 0.3501(3) 0.5628(3) 0.33499(17) 0.0307(10) Uani 1 1 d . . . C3 C 0.3041(3) 0.5523(3) 0.28145(16) 0.0291(9) Uani 1 1 d . . . C4 C 0.2658(3) 0.4673(3) 0.27935(16) 0.0289(10) Uani 1 1 d . . . C5 C 0.2853(3) 0.4245(3) 0.33149(17) 0.0285(10) Uani 1 1 d . . . C6 C 0.4039(3) 0.6399(3) 0.35497(19) 0.0412(12) Uani 1 1 d . . . H6A H 0.4703 0.6292 0.3491 0.062 Uiso 1 1 calc R . . H6B H 0.3919 0.6496 0.3958 0.062 Uiso 1 1 calc R . . H6C H 0.3850 0.6919 0.3333 0.062 Uiso 1 1 calc R . . C7 C 0.3032(3) 0.6170(3) 0.23362(19) 0.0434(12) Uani 1 1 d . . . H7A H 0.3406 0.5947 0.2018 0.065 Uiso 1 1 calc R . . H7B H 0.3290 0.6728 0.2469 0.065 Uiso 1 1 calc R . . H7C H 0.2392 0.6261 0.2207 0.065 Uiso 1 1 calc R . . C8 C 0.2172(3) 0.4270(3) 0.22834(17) 0.0406(11) Uani 1 1 d . . . H8A H 0.1768 0.4709 0.2104 0.061 Uiso 1 1 calc R . . H8B H 0.1797 0.3771 0.2410 0.061 Uiso 1 1 calc R . . H8C H 0.2635 0.4070 0.2006 0.061 Uiso 1 1 calc R . . C9 C 0.2571(3) 0.3337(3) 0.34862(19) 0.0408(12) Uani 1 1 d . . . H9A H 0.3039 0.2917 0.3354 0.061 Uiso 1 1 calc R . . H9B H 0.1971 0.3194 0.3313 0.061 Uiso 1 1 calc R . . H9C H 0.2519 0.3304 0.3904 0.061 Uiso 1 1 calc R . . C10 C 0.3559(3) 0.4713(3) 0.42798(15) 0.0261(9) Uani 1 1 d . . . C11 C 0.4342(3) 0.4374(3) 0.45191(17) 0.0294(10) Uani 1 1 d . . . H11 H 0.4857 0.4228 0.4284 0.035 Uiso 1 1 calc R . . C12 C 0.4389(3) 0.4238(2) 0.51193(17) 0.0247(9) Uani 1 1 d . . . C13 C 0.5169(3) 0.3848(3) 0.53785(19) 0.0342(11) Uani 1 1 d . . . H13 H 0.5702 0.3722 0.5154 0.041 Uiso 1 1 calc R . . C14 C 0.5167(3) 0.3650(3) 0.59474(19) 0.0363(11) Uani 1 1 d . . . H14 H 0.5691 0.3372 0.6114 0.044 Uiso 1 1 calc R . . C15 C 0.4398(3) 0.3854(3) 0.62849(18) 0.0362(11) Uani 1 1 d . . . H15 H 0.4405 0.3718 0.6682 0.043 Uiso 1 1 calc R . . C16 C 0.3645(3) 0.4243(3) 0.60532(17) 0.0314(10) Uani 1 1 d . . . H16 H 0.3131 0.4379 0.6291 0.038 Uiso 1 1 calc R . . C17 C 0.3604(2) 0.4454(3) 0.54589(15) 0.0251(9) Uani 1 1 d . . . C18 C 0.2794(3) 0.4841(3) 0.52095(16) 0.0251(9) Uani 1 1 d . . . C19 C 0.2798(3) 0.4956(3) 0.46269(16) 0.0256(9) Uani 1 1 d . . . C20 C 0.1968(3) 0.5079(3) 0.55700(16) 0.0274(10) Uani 1 1 d . . . C21 C 0.1367(3) 0.4426(3) 0.57800(15) 0.0282(9) Uani 1 1 d . . . C22 C 0.1483(3) 0.3524(3) 0.56486(18) 0.0364(11) Uani 1 1 d . . . H22 H 0.1988 0.3351 0.5413 0.044 Uiso 1 1 calc R . . C23 C 0.0897(3) 0.2904(3) 0.5849(2) 0.0466(13) Uani 1 1 d . . . H23 H 0.0990 0.2305 0.5752 0.056 Uiso 1 1 calc R . . C24 C 0.0146(3) 0.3148(4) 0.6202(2) 0.0509(13) Uani 1 1 d . . . H24 H -0.0264 0.2711 0.6343 0.061 Uiso 1 1 calc R . . C25 C 0.0003(3) 0.3996(4) 0.6341(2) 0.0516(14) Uani 1 1 d . . . H25 H -0.0507 0.4148 0.6579 0.062 Uiso 1 1 calc R . . C26 C 0.0607(3) 0.4666(3) 0.61376(17) 0.0351(11) Uani 1 1 d . . . C27 C 0.0495(3) 0.5553(4) 0.62876(18) 0.0438(12) Uani 1 1 d . . . H27 H 0.0009 0.5716 0.6540 0.053 Uiso 1 1 calc R . . C28 C 0.1065(3) 0.6171(3) 0.60799(19) 0.0418(12) Uani 1 1 d . . . H28 H 0.0973 0.6767 0.6184 0.050 Uiso 1 1 calc R . . C29 C 0.1799(3) 0.5945(3) 0.57078(18) 0.0367(11) Uani 1 1 d . . . C30 C 0.1656(2) 0.9859(3) 0.24169(16) 0.0260(9) Uani 1 1 d . . . C31 C 0.2111(3) 0.9328(3) 0.20024(16) 0.0283(10) Uani 1 1 d . . . C32 C 0.2371(3) 0.9883(3) 0.15391(16) 0.0292(10) Uani 1 1 d . . . C33 C 0.2063(3) 1.0736(3) 0.16639(18) 0.0297(10) Uani 1 1 d . . . C34 C 0.1618(3) 1.0731(3) 0.22010(16) 0.0261(9) Uani 1 1 d . . . C35 C 0.2259(3) 0.8358(3) 0.2047(2) 0.0430(12) Uani 1 1 d . . . H35A H 0.2289 0.8189 0.2451 0.065 Uiso 1 1 calc R . . H35B H 0.2843 0.8200 0.1858 0.065 Uiso 1 1 calc R . . H35C H 0.1743 0.8051 0.1862 0.065 Uiso 1 1 calc R . . C36 C 0.2863(3) 0.9598(3) 0.10011(17) 0.0429(12) Uani 1 1 d . . . H36A H 0.3250 0.9085 0.1084 0.064 Uiso 1 1 calc R . . H36B H 0.3255 1.0077 0.0861 0.064 Uiso 1 1 calc R . . H36C H 0.2404 0.9445 0.0708 0.064 Uiso 1 1 calc R . . C37 C 0.2117(3) 1.1510(3) 0.12616(19) 0.0420(12) Uani 1 1 d . . . H37A H 0.1585 1.1498 0.1000 0.063 Uiso 1 1 calc R . . H37B H 0.2694 1.1479 0.1041 0.063 Uiso 1 1 calc R . . H37C H 0.2106 1.2055 0.1483 0.063 Uiso 1 1 calc R . . C38 C 0.1170(3) 1.1502(3) 0.24958(19) 0.0420(12) Uani 1 1 d . . . H38A H 0.1534 1.2032 0.2421 0.063 Uiso 1 1 calc R . . H38B H 0.1147 1.1394 0.2909 0.063 Uiso 1 1 calc R . . H38C H 0.0538 1.1581 0.2349 0.063 Uiso 1 1 calc R . . C39 C 0.1447(2) 0.9590(2) 0.30127(15) 0.0253(9) Uani 1 1 d . . . C40 C 0.0647(3) 0.9241(2) 0.32228(17) 0.0282(10) Uani 1 1 d . . . H40 H 0.0129 0.9172 0.2976 0.034 Uiso 1 1 calc R . . C41 C 0.0571(3) 0.8979(2) 0.38056(18) 0.0265(9) Uani 1 1 d . . . C42 C -0.0253(3) 0.8609(3) 0.40229(19) 0.0340(11) Uani 1 1 d . . . H42 H -0.0779 0.8552 0.3781 0.041 Uiso 1 1 calc R . . C43 C -0.0302(3) 0.8332(3) 0.4574(2) 0.0424(12) Uani 1 1 d . . . H43 H -0.0859 0.8078 0.4715 0.051 Uiso 1 1 calc R . . C44 C 0.0468(3) 0.8423(3) 0.4936(2) 0.0422(12) Uani 1 1 d . . . H44 H 0.0430 0.8224 0.5320 0.051 Uiso 1 1 calc R . . C45 C 0.1262(3) 0.8791(3) 0.47448(17) 0.0336(10) Uani 1 1 d . . . H45 H 0.1770 0.8858 0.5000 0.040 Uiso 1 1 calc R . . C46 C 0.1352(3) 0.9083(2) 0.41643(17) 0.0274(10) Uani 1 1 d . . . C47 C 0.2206(3) 0.9447(3) 0.39554(16) 0.0252(9) Uani 1 1 d . . . C48 C 0.2225(3) 0.9694(2) 0.33846(16) 0.0243(9) Uani 1 1 d . . . C49 C 0.3027(3) 0.9560(3) 0.43436(15) 0.0252(9) Uani 1 1 d . . . C50 C 0.3540(3) 0.8837(3) 0.45000(17) 0.0321(10) Uani 1 1 d . . . C51 C 0.4318(3) 0.8921(3) 0.48742(18) 0.0389(12) Uani 1 1 d . . . H51 H 0.4686 0.8423 0.4964 0.047 Uiso 1 1 calc R . . C52 C 0.4530(3) 0.9710(3) 0.51005(18) 0.0361(11) Uani 1 1 d . . . H52 H 0.5047 0.9759 0.5350 0.043 Uiso 1 1 calc R . . C53 C 0.4004(3) 1.0462(3) 0.49761(17) 0.0308(10) Uani 1 1 d . . . C54 C 0.4183(3) 1.1278(3) 0.52368(19) 0.0397(12) Uani 1 1 d . . . H54 H 0.4699 1.1334 0.5487 0.048 Uiso 1 1 calc R . . C55 C 0.3630(3) 1.1993(3) 0.51376(19) 0.0450(12) Uani 1 1 d . . . H55 H 0.3740 1.2531 0.5331 0.054 Uiso 1 1 calc R . . C56 C 0.2898(3) 1.1913(3) 0.47455(19) 0.0391(11) Uani 1 1 d . . . H56 H 0.2520 1.2409 0.4668 0.047 Uiso 1 1 calc R . . C57 C 0.2719(3) 1.1148(3) 0.44755(18) 0.0310(10) Uani 1 1 d . . . H57 H 0.2227 1.1122 0.4205 0.037 Uiso 1 1 calc R . . C58 C 0.3243(3) 1.0389(3) 0.45862(15) 0.0246(9) Uani 1 1 d . . . O1 O 0.20592(16) 0.52981(18) 0.43356(10) 0.0301(7) Uani 1 1 d . . . O2 O 0.2331(2) 0.6624(2) 0.55156(16) 0.0540(9) Uani 1 1 d . . . H2 H 0.2674 0.6449 0.5249 0.081 Uiso 1 1 calc R . . O3 O 0.29852(17) 1.00489(18) 0.31306(11) 0.0297(7) Uani 1 1 d . . . O4 O 0.3360(2) 0.80096(19) 0.43119(14) 0.0500(8) Uani 1 1 d . . . H4 H 0.2860 0.8007 0.4127 0.075 Uiso 1 1 calc R . . Ti1 Ti 0.19196(5) 0.54350(5) 0.35588(3) 0.02707(17) Uani 1 1 d . . . Ti2 Ti 0.31607(4) 1.03400(5) 0.23748(3) 0.02609(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0312(2) 0.0764(4) 0.0371(3) -0.0059(3) -0.0037(2) -0.0043(2) Br2 0.0616(3) 0.0402(3) 0.0516(3) 0.0026(3) 0.0104(3) 0.0192(2) Br3 0.0490(3) 0.0427(3) 0.0392(3) 0.0016(2) -0.0022(2) -0.0149(2) Br4 0.0307(2) 0.0646(3) 0.0382(3) 0.0004(2) 0.0044(2) 0.0074(2) C1 0.0166(19) 0.037(2) 0.023(2) -0.0021(19) 0.0063(16) 0.0073(18) C2 0.024(2) 0.041(3) 0.027(2) -0.003(2) 0.0094(18) 0.0073(19) C3 0.031(2) 0.033(2) 0.023(2) 0.0001(19) 0.0089(17) 0.0080(19) C4 0.030(2) 0.037(3) 0.020(2) -0.0025(19) 0.0032(17) 0.0097(19) C5 0.027(2) 0.035(2) 0.023(2) -0.0005(19) 0.0070(18) 0.0042(18) C6 0.042(3) 0.044(3) 0.038(3) -0.006(2) 0.007(2) -0.001(2) C7 0.057(3) 0.043(3) 0.030(3) 0.005(2) 0.009(2) 0.001(2) C8 0.053(3) 0.043(3) 0.026(3) -0.008(2) -0.002(2) 0.003(2) C9 0.053(3) 0.040(3) 0.029(3) 0.002(2) -0.006(2) 0.003(2) C10 0.023(2) 0.035(2) 0.020(2) -0.0034(18) 0.0014(17) 0.0021(18) C11 0.023(2) 0.037(2) 0.028(2) -0.001(2) 0.0027(18) 0.0070(19) C12 0.022(2) 0.030(2) 0.022(2) -0.0040(17) -0.0013(18) -0.0010(18) C13 0.027(2) 0.043(3) 0.033(3) -0.005(2) -0.003(2) 0.002(2) C14 0.027(2) 0.047(3) 0.035(3) 0.004(2) -0.007(2) 0.005(2) C15 0.034(3) 0.051(3) 0.023(2) 0.002(2) -0.007(2) -0.002(2) C16 0.027(2) 0.042(3) 0.025(2) -0.0023(19) -0.0008(19) -0.005(2) C17 0.024(2) 0.030(2) 0.022(2) -0.0036(18) -0.0052(17) -0.0022(18) C18 0.024(2) 0.030(2) 0.022(2) -0.0048(18) 0.0006(17) -0.0006(17) C19 0.021(2) 0.035(2) 0.021(2) -0.0024(18) -0.0012(17) -0.0007(18) C20 0.023(2) 0.044(3) 0.016(2) -0.0040(19) -0.0017(17) 0.0087(19) C21 0.025(2) 0.042(3) 0.018(2) 0.0014(19) -0.0035(17) 0.003(2) C22 0.021(2) 0.058(3) 0.031(3) -0.002(2) 0.0002(19) 0.000(2) C23 0.039(3) 0.055(3) 0.046(3) 0.005(3) -0.003(2) -0.002(2) C24 0.033(3) 0.071(4) 0.049(3) 0.021(3) 0.004(2) -0.005(3) C25 0.030(3) 0.089(5) 0.036(3) 0.020(3) 0.005(2) 0.006(3) C26 0.022(2) 0.060(3) 0.024(2) 0.001(2) -0.0006(18) 0.010(2) C27 0.030(2) 0.080(4) 0.022(2) -0.003(2) 0.006(2) 0.020(3) C28 0.039(3) 0.057(3) 0.029(3) -0.013(2) 0.000(2) 0.016(2) C29 0.035(3) 0.051(3) 0.025(2) -0.008(2) -0.001(2) 0.003(2) C30 0.019(2) 0.039(2) 0.020(2) -0.0003(19) -0.0053(16) -0.0052(18) C31 0.030(2) 0.034(2) 0.021(2) -0.0018(19) -0.0054(18) -0.0040(19) C32 0.034(2) 0.038(3) 0.017(2) 0.0018(19) -0.0042(17) -0.0032(19) C33 0.028(2) 0.036(3) 0.025(2) 0.0020(19) -0.0063(19) -0.0033(19) C34 0.022(2) 0.034(2) 0.022(2) -0.0031(18) -0.0007(17) -0.0008(18) C35 0.050(3) 0.042(3) 0.037(3) -0.004(2) 0.005(2) -0.005(2) C36 0.050(3) 0.054(3) 0.024(2) -0.004(2) -0.002(2) -0.004(2) C37 0.048(3) 0.048(3) 0.030(3) 0.010(2) -0.003(2) 0.002(2) C38 0.041(3) 0.043(3) 0.042(3) -0.002(2) 0.013(2) 0.003(2) C39 0.023(2) 0.030(2) 0.023(2) -0.0019(18) -0.0010(17) -0.0001(18) C40 0.026(2) 0.029(2) 0.030(2) -0.0009(18) -0.0013(18) 0.0009(18) C41 0.025(2) 0.023(2) 0.031(2) -0.0005(18) 0.003(2) 0.0017(18) C42 0.027(2) 0.032(3) 0.042(3) 0.009(2) 0.0044(19) -0.0019(19) C43 0.037(3) 0.039(3) 0.051(3) 0.015(2) 0.015(2) -0.002(2) C44 0.047(3) 0.044(3) 0.036(3) 0.012(2) 0.018(2) 0.005(2) C45 0.042(3) 0.032(2) 0.028(2) 0.002(2) 0.001(2) 0.002(2) C46 0.037(3) 0.019(2) 0.026(2) -0.0013(17) 0.007(2) 0.0037(19) C47 0.028(2) 0.024(2) 0.023(2) -0.0007(18) 0.0009(17) 0.0003(18) C48 0.027(2) 0.024(2) 0.022(2) 0.0000(18) 0.0047(17) -0.0029(17) C49 0.030(2) 0.033(2) 0.0122(19) 0.0045(18) 0.0039(16) 0.0021(19) C50 0.042(3) 0.028(2) 0.026(2) -0.0030(19) 0.002(2) 0.007(2) C51 0.040(3) 0.049(3) 0.027(3) 0.004(2) -0.003(2) 0.017(2) C52 0.031(2) 0.051(3) 0.026(2) 0.002(2) -0.0017(19) 0.001(2) C53 0.032(2) 0.037(3) 0.024(2) 0.005(2) 0.0036(18) 0.001(2) C54 0.035(3) 0.053(3) 0.032(3) 0.000(2) -0.004(2) -0.014(2) C55 0.067(3) 0.030(3) 0.038(3) -0.005(2) 0.002(3) -0.013(3) C56 0.053(3) 0.024(2) 0.040(3) 0.004(2) 0.000(2) 0.001(2) C57 0.034(3) 0.035(3) 0.024(2) 0.006(2) 0.0025(19) 0.003(2) C58 0.024(2) 0.036(2) 0.0141(19) 0.0031(19) 0.0018(16) -0.0038(19) O1 0.0221(14) 0.0500(19) 0.0183(14) -0.0019(14) -0.0003(11) 0.0103(13) O2 0.052(2) 0.043(2) 0.067(3) -0.0141(18) 0.0190(18) -0.0024(17) O3 0.0261(15) 0.0445(18) 0.0186(14) 0.0029(12) -0.0008(12) -0.0080(13) O4 0.066(2) 0.0365(18) 0.048(2) -0.0117(17) -0.0151(17) 0.0150(17) Ti1 0.0260(4) 0.0359(4) 0.0193(4) 0.0002(3) 0.0009(3) 0.0073(3) Ti2 0.0242(4) 0.0361(4) 0.0180(4) 0.0012(3) -0.0003(3) -0.0044(3) _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 Br1 Ti1 2.4086(8) . ? Br2 Ti1 2.4107(9) . ? Br3 Ti2 2.4164(8) . ? Br4 Ti2 2.4104(8) . ? C1 C2 1.418(6) . ? C1 C5 1.418(5) . ? C1 C10 1.493(5) . ? C1 Ti1 2.299(4) . ? C2 C3 1.425(5) . ? C2 C6 1.485(6) . ? C2 Ti1 2.350(4) . ? C3 C4 1.410(6) . ? C3 C7 1.491(5) . ? C3 Ti1 2.379(4) . ? C4 C5 1.412(5) . ? C4 C8 1.514(5) . ? C4 Ti1 2.384(4) . ? C5 C9 1.498(5) . ? C5 Ti1 2.331(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.362(5) . ? C10 C19 1.414(5) . ? C11 C12 1.420(5) . ? C11 H11 0.9500 . ? C12 C13 1.408(5) . ? C12 C17 1.421(5) . ? C13 C14 1.364(6) . ? C13 H13 0.9500 . ? C14 C15 1.395(6) . ? C14 H14 0.9500 . ? C15 C16 1.350(6) . ? C15 H15 0.9500 . ? C16 C17 1.427(5) . ? C16 H16 0.9500 . ? C17 C18 1.432(5) . ? C18 C19 1.373(5) . ? C18 C20 1.503(5) . ? C19 O1 1.367(4) . ? C20 C29 1.381(6) . ? C20 C21 1.409(5) . ? C21 C22 1.420(6) . ? C21 C26 1.425(5) . ? C22 C23 1.352(6) . ? C22 H22 0.9500 . ? C23 C24 1.411(6) . ? C23 H23 0.9500 . ? C24 C25 1.349(7) . ? C24 H24 0.9500 . ? C25 C26 1.424(6) . ? C25 H25 0.9500 . ? C26 C27 1.408(7) . ? C27 C28 1.342(7) . ? C27 H27 0.9500 . ? C28 C29 1.413(6) . ? C28 H28 0.9500 . ? C29 O2 1.365(5) . ? C30 C31 1.423(5) . ? C30 C34 1.424(5) . ? C30 C39 1.483(5) . ? C30 Ti2 2.291(4) . ? C31 C32 1.425(5) . ? C31 C35 1.498(6) . ? C31 Ti2 2.331(4) . ? C32 C33 1.406(6) . ? C32 C36 1.508(5) . ? C32 Ti2 2.366(4) . ? C33 C34 1.410(6) . ? C33 C37 1.511(6) . ? C33 Ti2 2.373(4) . ? C34 C38 1.509(5) . ? C34 Ti2 2.338(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.362(5) . ? C39 C48 1.427(5) . ? C40 C41 1.424(5) . ? C40 H40 0.9500 . ? C41 C42 1.410(5) . ? C41 C46 1.413(6) . ? C42 C43 1.358(6) . ? C42 H42 0.9500 . ? C43 C44 1.402(6) . ? C43 H43 0.9500 . ? C44 C45 1.352(6) . ? C44 H44 0.9500 . ? C45 C46 1.434(5) . ? C45 H45 0.9500 . ? C46 C47 1.435(5) . ? C47 C48 1.387(5) . ? C47 C49 1.501(5) . ? C48 O3 1.359(4) . ? C49 C50 1.377(5) . ? C49 C58 1.421(6) . ? C50 O4 1.362(5) . ? C50 C51 1.428(6) . ? C51 C52 1.350(6) . ? C51 H51 0.9500 . ? C52 C53 1.405(6) . ? C52 H52 0.9500 . ? C53 C54 1.410(6) . ? C53 C58 1.430(5) . ? C54 C55 1.370(6) . ? C54 H54 0.9500 . ? C55 C56 1.402(6) . ? C55 H55 0.9500 . ? C56 C57 1.353(6) . ? C56 H56 0.9500 . ? C57 C58 1.407(6) . ? C57 H57 0.9500 . ? O1 Ti1 1.839(3) . ? O2 H2 0.8400 . ? O3 Ti2 1.839(3) . ? O4 H4 0.8400 . ? 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 C2 C1 C5 109.0(4) . . ? C2 C1 C10 125.1(4) . . ? C5 C1 C10 124.4(4) . . ? C2 C1 Ti1 74.2(2) . . ? C5 C1 Ti1 73.4(2) . . ? C10 C1 Ti1 108.0(2) . . ? C1 C2 C3 106.8(4) . . ? C1 C2 C6 125.8(4) . . ? C3 C2 C6 127.4(4) . . ? C1 C2 Ti1 70.3(2) . . ? C3 C2 Ti1 73.6(2) . . ? C6 C2 Ti1 122.7(3) . . ? C4 C3 C2 108.4(4) . . ? C4 C3 C7 125.4(4) . . ? C2 C3 C7 126.1(4) . . ? C4 C3 Ti1 73.0(2) . . ? C2 C3 Ti1 71.3(2) . . ? C7 C3 Ti1 125.4(3) . . ? C3 C4 C5 108.6(4) . . ? C3 C4 C8 125.6(4) . . ? C5 C4 C8 125.7(4) . . ? C3 C4 Ti1 72.6(2) . . ? C5 C4 Ti1 70.5(2) . . ? C8 C4 Ti1 125.6(3) . . ? C4 C5 C1 107.3(4) . . ? C4 C5 C9 127.3(4) . . ? C1 C5 C9 125.5(4) . . ? C4 C5 Ti1 74.6(2) . . ? C1 C5 Ti1 71.0(2) . . ? C9 C5 Ti1 119.9(3) . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C19 120.5(4) . . ? C11 C10 C1 126.6(3) . . ? C19 C10 C1 112.9(3) . . ? C10 C11 C12 120.1(4) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 121.6(4) . . ? C13 C12 C17 119.5(4) . . ? C11 C12 C17 118.7(3) . . ? C14 C13 C12 120.8(4) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.3(4) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 120.6(4) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 121.5(4) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C12 C17 C16 117.3(3) . . ? C12 C17 C18 121.1(3) . . ? C16 C17 C18 121.6(3) . . ? C19 C18 C17 117.0(3) . . ? C19 C18 C20 121.9(3) . . ? C17 C18 C20 121.1(3) . . ? O1 C19 C18 122.7(3) . . ? O1 C19 C10 114.7(3) . . ? C18 C19 C10 122.6(4) . . ? C29 C20 C21 119.2(4) . . ? C29 C20 C18 120.1(4) . . ? C21 C20 C18 120.7(4) . . ? C20 C21 C22 122.5(4) . . ? C20 C21 C26 119.7(4) . . ? C22 C21 C26 117.8(4) . . ? C23 C22 C21 122.0(4) . . ? C23 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? C22 C23 C24 119.7(5) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 120.8(5) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 120.9(5) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C27 C26 C25 122.5(4) . . ? C27 C26 C21 118.7(4) . . ? C25 C26 C21 118.8(4) . . ? C28 C27 C26 121.1(4) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 120.6(5) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? O2 C29 C20 123.4(4) . . ? O2 C29 C28 115.9(4) . . ? C20 C29 C28 120.6(4) . . ? C31 C30 C34 108.0(3) . . ? C31 C30 C39 125.1(3) . . ? C34 C30 C39 125.7(3) . . ? C31 C30 Ti2 73.6(2) . . ? C34 C30 Ti2 73.9(2) . . ? C39 C30 Ti2 108.7(2) . . ? C30 C31 C32 107.5(4) . . ? C30 C31 C35 125.5(4) . . ? C32 C31 C35 127.0(4) . . ? C30 C31 Ti2 70.5(2) . . ? C32 C31 Ti2 73.7(2) . . ? C35 C31 Ti2 122.4(3) . . ? C33 C32 C31 108.0(4) . . ? C33 C32 C36 126.1(4) . . ? C31 C32 C36 125.9(4) . . ? C33 C32 Ti2 73.0(2) . . ? C31 C32 Ti2 71.0(2) . . ? C36 C32 Ti2 123.2(3) . . ? C32 C33 C34 108.8(4) . . ? C32 C33 C37 125.3(4) . . ? C34 C33 C37 125.6(4) . . ? C32 C33 Ti2 72.5(2) . . ? C34 C33 Ti2 71.2(2) . . ? C37 C33 Ti2 126.9(3) . . ? C33 C34 C30 107.6(3) . . ? C33 C34 C38 126.6(4) . . ? C30 C34 C38 125.7(4) . . ? C33 C34 Ti2 73.9(2) . . ? C30 C34 Ti2 70.3(2) . . ? C38 C34 Ti2 121.8(3) . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C32 C36 H36A 109.5 . . ? C32 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C32 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C33 C37 H37A 109.5 . . ? C33 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C33 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C48 119.3(3) . . ? C40 C39 C30 128.2(3) . . ? C48 C39 C30 112.4(3) . . ? C39 C40 C41 121.3(4) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C42 C41 C46 120.2(4) . . ? C42 C41 C40 121.4(4) . . ? C46 C41 C40 118.4(4) . . ? C43 C42 C41 120.7(4) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C42 C43 C44 120.0(4) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 120.8(4) . . ? C45 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C44 C45 C46 121.3(4) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 119.4 . . ? C41 C46 C45 117.0(4) . . ? C41 C46 C47 121.6(4) . . ? C45 C46 C47 121.3(4) . . ? C48 C47 C46 116.7(4) . . ? C48 C47 C49 122.3(3) . . ? C46 C47 C49 121.0(3) . . ? O3 C48 C47 123.0(3) . . ? O3 C48 C39 114.3(3) . . ? C47 C48 C39 122.7(3) . . ? C50 C49 C58 119.2(4) . . ? C50 C49 C47 119.5(4) . . ? C58 C49 C47 121.1(3) . . ? O4 C50 C49 123.7(4) . . ? O4 C50 C51 115.5(4) . . ? C49 C50 C51 120.9(4) . . ? C52 C51 C50 119.8(4) . . ? C52 C51 H51 120.1 . . ? C50 C51 H51 120.1 . . ? C51 C52 C53 121.7(4) . . ? C51 C52 H52 119.2 . . ? C53 C52 H52 119.2 . . ? C52 C53 C54 122.2(4) . . ? C52 C53 C58 118.8(4) . . ? C54 C53 C58 119.0(4) . . ? C55 C54 C53 121.6(4) . . ? C55 C54 H54 119.2 . . ? C53 C54 H54 119.2 . . ? C54 C55 C56 118.6(4) . . ? C54 C55 H55 120.7 . . ? C56 C55 H55 120.7 . . ? C57 C56 C55 121.6(4) . . ? C57 C56 H56 119.2 . . ? C55 C56 H56 119.2 . . ? C56 C57 C58 121.5(4) . . ? C56 C57 H57 119.3 . . ? C58 C57 H57 119.3 . . ? C57 C58 C49 122.8(3) . . ? C57 C58 C53 117.7(4) . . ? C49 C58 C53 119.5(4) . . ? C19 O1 Ti1 128.3(2) . . ? C29 O2 H2 109.5 . . ? C48 O3 Ti2 128.8(2) . . ? C50 O4 H4 109.5 . . ? O1 Ti1 C1 75.96(12) . . ? O1 Ti1 C5 95.16(13) . . ? C1 Ti1 C5 35.67(14) . . ? O1 Ti1 C2 96.51(13) . . ? C1 Ti1 C2 35.49(14) . . ? C5 Ti1 C2 59.13(14) . . ? O1 Ti1 C3 130.88(12) . . ? C1 Ti1 C3 58.36(13) . . ? C5 Ti1 C3 58.21(14) . . ? C2 Ti1 C3 35.08(13) . . ? O1 Ti1 C4 129.56(13) . . ? C1 Ti1 C4 58.20(13) . . ? C5 Ti1 C4 34.82(13) . . ? C2 Ti1 C4 58.12(14) . . ? C3 Ti1 C4 34.45(13) . . ? O1 Ti1 Br1 105.52(9) . . ? C1 Ti1 Br1 128.07(10) . . ? C5 Ti1 Br1 94.26(10) . . ? C2 Ti1 Br1 147.10(11) . . ? C3 Ti1 Br1 116.04(10) . . ? C4 Ti1 Br1 88.98(10) . . ? O1 Ti1 Br2 104.44(9) . . ? C1 Ti1 Br2 126.13(10) . . ? C5 Ti1 Br2 148.06(10) . . ? C2 Ti1 Br2 93.30(11) . . ? C3 Ti1 Br2 90.07(10) . . ? C4 Ti1 Br2 118.58(10) . . ? Br1 Ti1 Br2 104.22(3) . . ? O3 Ti2 C30 75.59(12) . . ? O3 Ti2 C31 96.28(13) . . ? C30 Ti2 C31 35.84(13) . . ? O3 Ti2 C34 95.60(13) . . ? C30 Ti2 C34 35.81(13) . . ? C31 Ti2 C34 59.11(14) . . ? O3 Ti2 C32 130.98(13) . . ? C30 Ti2 C32 59.06(14) . . ? C31 Ti2 C32 35.32(13) . . ? C34 Ti2 C32 58.28(14) . . ? O3 Ti2 C33 129.99(13) . . ? C30 Ti2 C33 58.72(13) . . ? C31 Ti2 C33 58.30(14) . . ? C34 Ti2 C33 34.83(13) . . ? C32 Ti2 C33 34.53(14) . . ? O3 Ti2 Br4 103.17(9) . . ? C30 Ti2 Br4 125.84(10) . . ? C31 Ti2 Br4 93.02(10) . . ? C34 Ti2 Br4 148.12(10) . . ? C32 Ti2 Br4 90.18(10) . . ? C33 Ti2 Br4 119.05(11) . . ? O3 Ti2 Br3 106.94(9) . . ? C30 Ti2 Br3 127.62(10) . . ? C31 Ti2 Br3 146.09(10) . . ? C34 Ti2 Br3 93.64(10) . . ? C32 Ti2 Br3 114.76(10) . . ? C33 Ti2 Br3 87.79(10) . . ? Br4 Ti2 Br3 104.97(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.787 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.074 #===END