Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Anthony Hill' _publ_contact_author_address ; Research School of Chemistry Australian National University Australian Capital Territory Canberra 0200 AUSTRALIA ; _publ_contact_author_email AFHILL@RSC.ANU.EDU.AU _publ_section_title ; A Homoleptic Hydrotris(methimazolyl)borate Complex of Titanium ; # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [C18.5 H28 B1 N6 O1 S3 Cl7 Ti2] is reported. ; _publ_section_comment #Text of the paper ; The crystallographic asymmetric unit consists of one molecule of [C12 15 B1 N6 S3 Ti], one molecule of [C4 H8 O1 Cl2 Ti], two molecules of dichloromethane and a third molecule of dichloromethane which is disordered. Hydrogen atoms attached to C atoms were included at idealized positions and ride on the atom to which they bonded. Hydrogens attached to boron and C7 were located but not refined. ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; Hydrogen atoms attached to C atoms were included at idealized positions and ride on the atom to which they bonded. Hydrogens attached to boron and C7 were located but not refined. ; _publ_section_exptl_prep ; The compound was prepared by MKS and recrystallized from dichloromethane/hexane. The sample ID is mks62. ; loop_ _publ_author_name 'Anthony Hill' 'Matthew K. Smith' data_c:mks62 _database_code_depnum_ccdc_archive 'CCDC 646866' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18.50 H28 B Cl7 N6 O S3 Ti' _chemical_formula_weight 747.52 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' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.409(2) _cell_length_b 13.165(3) _cell_length_c 13.445(3) _cell_angle_alpha 75.65(3) _cell_angle_beta 72.60(3) _cell_angle_gamma 72.72(3) _cell_volume 1653.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 34699 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 31.00 _exptl_crystal_description cube _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 766 _exptl_absorpt_coefficient_mu 1.039 # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.180 -1 0 0 0.140 0 1 0 0.120 0 -1 0 0.140 0 0 1 0.120 0 0 -1 0.140 1 0 2 0.121 -2 0 -3 0.125 2 -3 0 0.122 0 -9 -10 0.144 -1 19 18 0.147 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.809 _exptl_absorpt_correction_T_max 0.869 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _diffrn_ambient_temperature 200(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 _diffrn_measurement_method ' \f and \w scans with CCD ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 34902 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.62 _reflns_number_total 7629 _reflns_number_gt 5638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0530P)^2^+0.9767P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7629 _refine_ls_number_parameters 364 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1145 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.004 _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 0.5000 0.0000 0.0000 0.02490(14) Uani 1 2 d S . . Cl1 Cl 0.03960(7) 0.55120(5) 0.31203(5) 0.03569(16) Uani 1 1 d . . . O1 O -0.16815(18) 0.44154(15) 0.50379(14) 0.0362(4) Uani 1 1 d . . . C1 C -0.3062(3) 0.4714(3) 0.5725(2) 0.0455(7) Uani 1 1 d . . . H1A H -0.3632 0.5377 0.5385 0.055 Uiso 1 1 calc R . . H1B H -0.3010 0.4832 0.6410 0.055 Uiso 1 1 calc R . . B1 B 0.4187(3) 0.3314(2) -0.0723(2) 0.0318(6) Uani 1 1 d . . . Ti2 Ti 0.0000 0.5000 0.5000 0.02572(14) Uani 1 2 d S . . Cl2 Cl 0.15538(7) 0.32473(5) 0.48102(5) 0.03508(15) Uani 1 1 d . . . C2 C -0.3642(4) 0.3760(3) 0.5874(3) 0.0629(10) Uani 1 1 d . . . H2A H -0.4669 0.3962 0.6070 0.075 Uiso 1 1 calc R . . H2B H -0.3308 0.3174 0.6427 0.075 Uiso 1 1 calc R . . Cl3 Cl 0.64727(13) 0.14167(8) 0.35017(9) 0.0776(3) Uani 1 1 d . . . C3 C -0.3096(4) 0.3429(4) 0.4807(4) 0.0781(13) Uani 1 1 d . . . H3A H -0.3726 0.3832 0.4340 0.094 Uiso 1 1 calc R . . H3B H -0.2997 0.2645 0.4871 0.094 Uiso 1 1 calc R . . Cl4 Cl 0.57036(12) 0.35791(9) 0.22926(9) 0.0775(3) Uani 1 1 d . . . C4 C -0.1700(3) 0.3703(3) 0.4375(3) 0.0492(8) Uani 1 1 d . . . H4A H -0.0941 0.3041 0.4416 0.059 Uiso 1 1 calc R . . H4B H -0.1591 0.4071 0.3628 0.059 Uiso 1 1 calc R . . Cl5 Cl 0.07303(12) 0.09827(10) 0.76359(10) 0.0916(4) Uani 1 1 d . . . C5 C 0.5117(4) 0.2467(3) 0.3108(3) 0.0610(9) Uani 1 1 d . . . H5A H 0.4651 0.2190 0.2726 0.073 Uiso 1 1 calc R . . H5B H 0.4424 0.2702 0.3746 0.073 Uiso 1 1 calc R . . Cl6 Cl -0.0117(2) 0.08438(11) 0.58149(10) 0.1204(6) Uani 1 1 d . . . C6 C -0.0416(4) 0.1578(3) 0.6818(3) 0.0585(9) Uani 1 1 d . . . H6A H -0.0315 0.2321 0.6493 0.070 Uiso 1 1 calc R . . H6B H -0.1380 0.1628 0.7251 0.070 Uiso 1 1 calc R . . Cl7 Cl 0.1077(2) 0.6021(2) -0.08740(19) 0.0724(5) Uani 0.50 1 d P . . C7 C 0.0012(9) 0.5569(8) 0.0356(8) 0.063(2) Uani 0.50 1 d PD . . Cl8 Cl -0.0464(3) 0.4413(2) 0.0333(3) 0.0798(7) Uani 0.50 1 d P . . S11 S 0.56203(7) 0.10801(5) 0.09821(5) 0.02965(15) Uani 1 1 d . . . N11 N 0.5693(2) 0.29149(16) -0.05916(16) 0.0297(5) Uani 1 1 d . . . C11 C 0.6312(3) 0.2063(2) 0.00477(19) 0.0286(5) Uani 1 1 d . . . N12 N 0.7654(2) 0.20899(18) -0.01521(18) 0.0352(5) Uani 1 1 d . . . C12 C 0.6693(3) 0.3464(2) -0.1206(2) 0.0376(6) Uani 1 1 d . . . H12 H 0.6549 0.4094 -0.1728 0.045 Uiso 1 1 calc R . . C13 C 0.7894(3) 0.2959(2) -0.0940(2) 0.0421(7) Uani 1 1 d . . . H13 H 0.8752 0.3161 -0.1238 0.050 Uiso 1 1 calc R . . C14 C 0.8661(3) 0.1327(3) 0.0388(3) 0.0499(8) Uani 1 1 d . . . H14A H 0.8388 0.1396 0.1136 0.075 Uiso 1 1 calc R . . H14B H 0.9577 0.1478 0.0063 0.075 Uiso 1 1 calc R . . H14C H 0.8699 0.0590 0.0330 0.075 Uiso 1 1 calc R . . S21 S 0.60214(7) 0.09858(5) -0.17874(5) 0.03047(15) Uani 1 1 d . . . N21 N 0.4004(2) 0.29160(17) -0.16573(16) 0.0305(5) Uani 1 1 d . . . C21 C 0.4646(3) 0.2014(2) -0.20864(19) 0.0294(5) Uani 1 1 d . . . N22 N 0.4027(2) 0.20468(19) -0.28494(17) 0.0345(5) Uani 1 1 d . . . C22 C 0.2961(3) 0.3505(2) -0.2167(2) 0.0399(6) Uani 1 1 d . . . H22 H 0.2345 0.4176 -0.2023 0.048 Uiso 1 1 calc R . . C23 C 0.2971(3) 0.2965(2) -0.2897(2) 0.0417(7) Uani 1 1 d . . . H23 H 0.2364 0.3177 -0.3357 0.050 Uiso 1 1 calc R . . C24 C 0.4397(4) 0.1219(3) -0.3506(2) 0.0491(8) Uani 1 1 d . . . H24A H 0.5373 0.1127 -0.3892 0.074 Uiso 1 1 calc R . . H24B H 0.3812 0.1443 -0.4012 0.074 Uiso 1 1 calc R . . H24C H 0.4251 0.0534 -0.3055 0.074 Uiso 1 1 calc R . . S31 S 0.25943(6) 0.11623(5) 0.00881(5) 0.03094(15) Uani 1 1 d . . . N31 N 0.3147(2) 0.30083(16) 0.03345(16) 0.0301(5) Uani 1 1 d . . . C31 C 0.2543(3) 0.2170(2) 0.0723(2) 0.0307(5) Uani 1 1 d . . . N32 N 0.1834(2) 0.22502(18) 0.17328(18) 0.0370(5) Uani 1 1 d . . . C32 C 0.2810(3) 0.3611(2) 0.1131(2) 0.0396(6) Uani 1 1 d . . . H32 H 0.3097 0.4249 0.1073 0.048 Uiso 1 1 calc R . . C33 C 0.2014(3) 0.3143(2) 0.1992(2) 0.0427(7) Uani 1 1 d . . . H33 H 0.1642 0.3378 0.2656 0.051 Uiso 1 1 calc R . . C34 C 0.1029(4) 0.1507(3) 0.2453(2) 0.0535(8) Uani 1 1 d . . . H34A H 0.0184 0.1597 0.2226 0.080 Uiso 1 1 calc R . . H34B H 0.0777 0.1663 0.3172 0.080 Uiso 1 1 calc R . . H34C H 0.1584 0.0763 0.2443 0.080 Uiso 1 1 calc R . . H7A H -0.089(3) 0.608(4) 0.061(4) 0.050 Uiso 0.50 1 d PD . . H7B H 0.058(4) 0.541(5) 0.088(3) 0.050 Uiso 0.50 1 d PD . . 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 0.0253(3) 0.0241(3) 0.0250(3) -0.0032(2) -0.0072(2) -0.0054(2) Cl1 0.0424(4) 0.0374(3) 0.0240(3) -0.0022(3) -0.0068(3) -0.0088(3) O1 0.0325(9) 0.0452(11) 0.0360(10) -0.0133(8) -0.0049(8) -0.0152(9) C1 0.0317(14) 0.0612(19) 0.0445(17) -0.0145(15) -0.0020(13) -0.0157(14) B1 0.0351(15) 0.0307(15) 0.0313(15) -0.0026(12) -0.0134(12) -0.0073(13) Ti2 0.0265(3) 0.0279(3) 0.0227(3) -0.0034(2) -0.0059(2) -0.0075(3) Cl2 0.0375(3) 0.0326(3) 0.0320(3) -0.0062(3) -0.0091(3) -0.0026(3) C2 0.0455(19) 0.067(2) 0.078(3) -0.002(2) -0.0094(18) -0.0310(18) Cl3 0.1050(8) 0.0623(6) 0.0733(7) -0.0218(5) -0.0395(6) -0.0057(6) C3 0.060(2) 0.094(3) 0.105(3) -0.042(3) -0.017(2) -0.037(2) Cl4 0.0858(7) 0.0744(7) 0.0713(7) -0.0015(5) -0.0215(5) -0.0245(6) C4 0.0566(19) 0.0572(19) 0.0481(18) -0.0176(15) -0.0160(15) -0.0245(16) Cl5 0.0780(7) 0.0872(8) 0.0820(8) 0.0126(6) -0.0216(6) 0.0002(6) C5 0.064(2) 0.064(2) 0.055(2) -0.0225(18) -0.0076(17) -0.0129(18) Cl6 0.2252(18) 0.0807(8) 0.0663(7) -0.0145(6) -0.0049(9) -0.0825(10) C6 0.068(2) 0.052(2) 0.0501(19) -0.0015(16) -0.0057(17) -0.0211(18) Cl7 0.0603(12) 0.0767(14) 0.0713(13) -0.0225(11) -0.0041(10) -0.0076(11) C7 0.053(5) 0.070(5) 0.058(5) -0.020(5) -0.010(4) 0.001(4) Cl8 0.0660(16) 0.0717(15) 0.111(2) -0.0097(17) -0.0403(16) -0.0157(13) S11 0.0358(3) 0.0279(3) 0.0271(3) -0.0013(2) -0.0114(3) -0.0094(3) N11 0.0348(11) 0.0280(11) 0.0283(11) -0.0022(9) -0.0107(9) -0.0098(9) C11 0.0320(13) 0.0280(12) 0.0279(12) -0.0060(10) -0.0102(10) -0.0062(10) N12 0.0299(11) 0.0421(13) 0.0334(12) -0.0010(10) -0.0104(9) -0.0104(10) C12 0.0443(16) 0.0385(15) 0.0335(14) 0.0020(11) -0.0105(12) -0.0207(13) C13 0.0396(15) 0.0499(17) 0.0394(15) 0.0015(13) -0.0082(12) -0.0236(14) C14 0.0327(15) 0.063(2) 0.0501(19) 0.0024(15) -0.0168(13) -0.0086(14) S21 0.0307(3) 0.0302(3) 0.0276(3) -0.0022(2) -0.0064(2) -0.0061(3) N21 0.0312(11) 0.0295(11) 0.0291(11) -0.0017(9) -0.0116(9) -0.0034(9) C21 0.0298(13) 0.0331(13) 0.0265(12) -0.0001(10) -0.0087(10) -0.0116(11) N22 0.0370(12) 0.0414(13) 0.0282(11) -0.0045(9) -0.0116(9) -0.0116(10) C22 0.0380(15) 0.0402(15) 0.0388(15) -0.0015(12) -0.0185(12) -0.0006(12) C23 0.0376(15) 0.0485(17) 0.0401(16) -0.0018(13) -0.0208(12) -0.0054(13) C24 0.060(2) 0.0559(19) 0.0385(16) -0.0147(14) -0.0168(14) -0.0144(16) S31 0.0271(3) 0.0310(3) 0.0351(3) -0.0080(3) -0.0083(3) -0.0050(3) N31 0.0326(11) 0.0268(11) 0.0307(11) -0.0073(9) -0.0105(9) -0.0023(9) C31 0.0268(12) 0.0320(13) 0.0300(13) -0.0050(10) -0.0088(10) -0.0008(11) N32 0.0364(12) 0.0365(12) 0.0322(12) -0.0087(10) -0.0020(10) -0.0040(10) C32 0.0463(16) 0.0326(14) 0.0423(16) -0.0157(12) -0.0160(13) -0.0001(12) C33 0.0476(17) 0.0435(16) 0.0338(15) -0.0152(13) -0.0090(13) -0.0003(14) C34 0.056(2) 0.0533(19) 0.0419(17) -0.0089(15) 0.0053(15) -0.0161(16) _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 S11 2.4837(8) . ? Ti1 S11 2.4837(8) 2_655 ? Ti1 S31 2.5025(11) 2_655 ? Ti1 S31 2.5025(11) . ? Ti1 S21 2.5169(11) 2_655 ? Ti1 S21 2.5169(11) . ? Cl1 Ti2 2.3893(9) . ? O1 C4 1.452(3) . ? O1 C1 1.457(3) . ? O1 Ti2 2.0942(17) . ? C1 C2 1.495(4) . ? B1 N11 1.548(4) . ? B1 N31 1.553(4) . ? B1 N21 1.555(4) . ? Ti2 O1 2.0942(17) 2_566 ? Ti2 Cl1 2.3893(9) 2_566 ? Ti2 Cl2 2.4152(11) . ? Ti2 Cl2 2.4152(11) 2_566 ? C2 C3 1.499(5) . ? Cl3 C5 1.763(4) . ? C3 C4 1.511(5) . ? Cl4 C5 1.747(4) . ? Cl5 C6 1.747(4) . ? Cl6 C6 1.751(4) . ? Cl7 Cl8 0.998(3) 2_565 ? Cl7 C7 1.769(10) . ? C7 Cl8 0.904(8) 2_565 ? C7 Cl8 1.744(9) . ? C7 C7 1.977(18) 2_565 ? Cl8 C7 0.904(8) 2_565 ? Cl8 Cl7 0.998(3) 2_565 ? Cl8 Cl8 1.952(6) 2_565 ? S11 C11 1.726(3) . ? N11 C11 1.354(3) . ? N11 C12 1.388(3) . ? C11 N12 1.351(3) . ? N12 C13 1.381(4) . ? N12 C14 1.450(4) . ? C12 C13 1.337(4) . ? S21 C21 1.723(3) . ? N21 C21 1.351(3) . ? N21 C22 1.390(3) . ? C21 N22 1.351(3) . ? N22 C23 1.374(4) . ? N22 C24 1.463(4) . ? C22 C23 1.344(4) . ? S31 C31 1.727(3) . ? N31 C31 1.348(3) . ? N31 C32 1.390(3) . ? C31 N32 1.351(3) . ? N32 C33 1.382(4) . ? N32 C34 1.459(4) . ? C32 C33 1.335(4) . ? 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 S11 Ti1 S11 180 . 2_655 ? S11 Ti1 S31 85.64(3) . 2_655 ? S11 Ti1 S31 94.36(3) 2_655 2_655 ? S11 Ti1 S31 94.36(3) . . ? S11 Ti1 S31 85.64(3) 2_655 . ? S31 Ti1 S31 180 2_655 . ? S11 Ti1 S21 86.24(3) . 2_655 ? S11 Ti1 S21 93.76(3) 2_655 2_655 ? S31 Ti1 S21 94.36(4) 2_655 2_655 ? S31 Ti1 S21 85.64(4) . 2_655 ? S11 Ti1 S21 93.76(3) . . ? S11 Ti1 S21 86.24(3) 2_655 . ? S31 Ti1 S21 85.64(4) 2_655 . ? S31 Ti1 S21 94.36(4) . . ? S21 Ti1 S21 180 2_655 . ? C4 O1 C1 109.1(2) . . ? C4 O1 Ti2 126.89(17) . . ? C1 O1 Ti2 124.01(16) . . ? O1 C1 C2 103.4(3) . . ? N11 B1 N31 110.6(2) . . ? N11 B1 N21 112.4(2) . . ? N31 B1 N21 112.2(2) . . ? O1 Ti2 O1 180 2_566 . ? O1 Ti2 Cl1 89.93(6) 2_566 2_566 ? O1 Ti2 Cl1 90.07(6) . 2_566 ? O1 Ti2 Cl1 90.07(6) 2_566 . ? O1 Ti2 Cl1 89.93(6) . . ? Cl1 Ti2 Cl1 180 2_566 . ? O1 Ti2 Cl2 89.31(6) 2_566 . ? O1 Ti2 Cl2 90.69(6) . . ? Cl1 Ti2 Cl2 89.47(4) 2_566 . ? Cl1 Ti2 Cl2 90.53(4) . . ? O1 Ti2 Cl2 90.69(6) 2_566 2_566 ? O1 Ti2 Cl2 89.31(6) . 2_566 ? Cl1 Ti2 Cl2 90.53(4) 2_566 2_566 ? Cl1 Ti2 Cl2 89.47(4) . 2_566 ? Cl2 Ti2 Cl2 180 . 2_566 ? C1 C2 C3 102.9(3) . . ? C2 C3 C4 105.0(3) . . ? O1 C4 C3 105.5(3) . . ? Cl4 C5 Cl3 112.5(2) . . ? Cl5 C6 Cl6 112.1(2) . . ? Cl8 Cl7 C7 20.4(4) 2_565 . ? Cl8 C7 Cl8 89.1(7) 2_565 . ? Cl8 C7 Cl7 22.7(4) 2_565 . ? Cl8 C7 Cl7 111.7(6) . . ? Cl8 C7 C7 61.9(6) 2_565 2_565 ? Cl8 C7 C7 27.2(3) . 2_565 ? Cl7 C7 C7 84.5(6) . 2_565 ? C7 Cl8 Cl7 136.9(8) 2_565 2_565 ? C7 Cl8 C7 90.9(7) 2_565 . ? Cl7 Cl8 C7 132.0(6) 2_565 . ? C7 Cl8 Cl8 63.3(7) 2_565 2_565 ? Cl7 Cl8 Cl8 159.3(4) 2_565 2_565 ? C7 Cl8 Cl8 27.6(3) . 2_565 ? C11 S11 Ti1 106.55(9) . . ? C11 N11 C12 107.6(2) . . ? C11 N11 B1 132.0(2) . . ? C12 N11 B1 120.4(2) . . ? N12 C11 N11 107.8(2) . . ? N12 C11 S11 122.5(2) . . ? N11 C11 S11 129.67(19) . . ? C11 N12 C13 108.9(2) . . ? C11 N12 C14 124.9(2) . . ? C13 N12 C14 126.2(2) . . ? C13 C12 N11 108.6(2) . . ? C12 C13 N12 107.2(2) . . ? C21 S21 Ti1 103.91(9) . . ? C21 N21 C22 107.8(2) . . ? C21 N21 B1 132.2(2) . . ? C22 N21 B1 120.0(2) . . ? N21 C21 N22 107.5(2) . . ? N21 C21 S21 129.03(19) . . ? N22 C21 S21 123.5(2) . . ? C21 N22 C23 109.6(2) . . ? C21 N22 C24 125.4(2) . . ? C23 N22 C24 125.0(2) . . ? C23 C22 N21 108.4(3) . . ? C22 C23 N22 106.8(2) . . ? C31 S31 Ti1 103.03(9) . . ? C31 N31 C32 107.9(2) . . ? C31 N31 B1 132.7(2) . . ? C32 N31 B1 119.0(2) . . ? N31 C31 N32 107.6(2) . . ? N31 C31 S31 128.4(2) . . ? N32 C31 S31 124.0(2) . . ? C31 N32 C33 109.1(2) . . ? C31 N32 C34 126.0(2) . . ? C33 N32 C34 124.9(2) . . ? C33 C32 N31 108.4(2) . . ? C32 C33 N32 107.0(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.930 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.073