# Electronic Supplementary Material (ESI) for Catalysis Science and Technology # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Cat.Sci.Tech. _journal_coden_cambridge 1486 #TrackingRef '- CIF.CIF' #SUBMISSION DETAILS: _publ_contact_author ; Dr. Wen-Hua Sun Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; loop_ _publ_author_name _publ_author_address 'Wei Huang' ; Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; B.Li ; Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022 China ; Y.Wang ; Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; W.Zhang ; Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; L.Wang ; School of Chemistry University of East Anglia Norwich NR4 7TJ UK ; Y.Li '' 'Wen-Hua Sun' '' 'Carl Redshaw' '' _publ_contact_author_email whsun@iccas.ac.cn _publ_contact_author_name 'Dr. Wen-Hua Sun' data_C2 _database_code_depnum_ccdc_archive 'CCDC 822119' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H26 Cl2 N2 O Ti' _chemical_formula_weight 501.29 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 23.852(5) _cell_length_b 13.832(3) _cell_length_c 16.890(3) _cell_angle_alpha 90.00 _cell_angle_beta 118.68(3) _cell_angle_gamma 90.00 _cell_volume 4888.6(17) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6948 _cell_measurement_theta_min 1.76 _cell_measurement_theta_max 25.50 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 0.590 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .0000 _exptl_absorpt_correction_T_max .0000 _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 none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 17075 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4502 _reflns_number_gt 3794 _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^)+(0.0659P)^2^+28.3476P] 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 4502 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0780 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.1862 _refine_ls_wR_factor_gt 0.1805 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_restrained_S_all 1.191 _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 0.08576(4) 0.80619(6) 0.08340(5) 0.0236(2) Uani 1 1 d . . . Cl2 Cl 0.08446(6) 0.68592(8) -0.02437(8) 0.0301(3) Uani 1 1 d . . . Cl1 Cl 0.14076(6) 0.91882(8) 0.20652(8) 0.0330(3) Uani 1 1 d . . . N1 N 0.18170(18) 0.8036(3) 0.1055(3) 0.0256(8) Uani 1 1 d . . . O1 O 0.08451(14) 0.9050(2) 0.0001(2) 0.0287(7) Uani 1 1 d . . . N2 N 0.14726(18) 0.6874(3) 0.1923(2) 0.0243(8) Uani 1 1 d . . . C9 C 0.2276(2) 0.7461(3) 0.1626(3) 0.0273(10) Uani 1 1 d . . . C6 C 0.1929(2) 0.8654(3) 0.0527(3) 0.0269(10) Uani 1 1 d . . . C12 C 0.1245(2) 0.6217(3) 0.2377(3) 0.0283(10) Uani 1 1 d . . . C5 C 0.2517(2) 0.8718(3) 0.0537(3) 0.0298(10) Uani 1 1 d . . . C7 C 0.3001(2) 0.8088(4) 0.1131(3) 0.0340(11) Uani 1 1 d . . . H7A H 0.3408 0.8092 0.1157 0.041 Uiso 1 1 calc R . . C2 C 0.1444(2) 0.9845(4) -0.0635(3) 0.0344(11) Uani 1 1 d . . . H2A H 0.1093 1.0232 -0.1037 0.041 Uiso 1 1 calc R . . C1 C 0.1379(2) 0.9208(3) -0.0052(3) 0.0271(10) Uani 1 1 d . . . C20 C 0.1568(3) 0.7445(4) 0.3648(3) 0.0375(12) Uani 1 1 d . . . H20A H 0.1979 0.7530 0.3645 0.045 Uiso 1 1 calc R . . H20B H 0.1280 0.7972 0.3279 0.045 Uiso 1 1 calc R . . C4 C 0.2563(2) 0.9379(4) -0.0069(3) 0.0349(11) Uani 1 1 d . . . H4A H 0.2952 0.9451 -0.0089 0.042 Uiso 1 1 calc R . . C10 C 0.2073(2) 0.6830(3) 0.2142(3) 0.0296(10) Uani 1 1 d . . . C17 C 0.1280(2) 0.6493(4) 0.3199(3) 0.0312(10) Uani 1 1 d . . . C13 C 0.1023(3) 0.5300(4) 0.2006(4) 0.0392(12) Uani 1 1 d . . . C26 C -0.0025(2) 0.7162(4) 0.0684(4) 0.0335(11) Uani 1 1 d . . . H26A H -0.0048 0.6442 0.0713 0.040 Uiso 1 1 calc R . . C3 C 0.2036(3) 0.9914(4) -0.0626(4) 0.0383(12) Uani 1 1 d . . . H3A H 0.2072 1.0356 -0.1029 0.046 Uiso 1 1 calc R . . C8 C 0.2885(2) 0.7466(4) 0.1673(3) 0.0318(11) Uani 1 1 d . . . H8A H 0.3212 0.7043 0.2076 0.038 Uiso 1 1 calc R . . C16 C 0.1038(2) 0.5849(4) 0.3595(4) 0.0379(12) Uani 1 1 d . . . H16A H 0.1043 0.6027 0.4141 0.046 Uiso 1 1 calc R . . C15 C 0.0794(3) 0.4966(4) 0.3220(4) 0.0424(13) Uani 1 1 d . . . H15A H 0.0622 0.4547 0.3494 0.051 Uiso 1 1 calc R . . C11 C 0.2569(2) 0.6206(4) 0.2874(4) 0.0392(12) Uani 1 1 d . . . H11A H 0.2367 0.5824 0.3157 0.059 Uiso 1 1 calc R . . H11B H 0.2902 0.6617 0.3329 0.059 Uiso 1 1 calc R . . H11C H 0.2760 0.5770 0.2612 0.059 Uiso 1 1 calc R . . C21 C 0.1687(3) 0.7559(4) 0.4600(4) 0.0430(13) Uani 1 1 d . . . H21A H 0.1872 0.8198 0.4827 0.065 Uiso 1 1 calc R . . H21B H 0.1985 0.7057 0.4980 0.065 Uiso 1 1 calc R . . H21C H 0.1283 0.7497 0.4613 0.065 Uiso 1 1 calc R . . C25 C -0.0236(2) 0.8684(4) 0.0126(4) 0.0383(12) Uani 1 1 d . . . H25A H -0.0403 0.9237 -0.0308 0.046 Uiso 1 1 calc R . . C24 C -0.0257(2) 0.7718(4) -0.0104(3) 0.0339(11) Uani 1 1 d . . . H24A H -0.0454 0.7457 -0.0733 0.041 Uiso 1 1 calc R . . C23 C 0.0008(2) 0.8748(4) 0.1055(4) 0.0425(13) Uani 1 1 d . . . H23A H 0.0036 0.9347 0.1403 0.051 Uiso 1 1 calc R . . C22 C 0.0139(2) 0.7797(4) 0.1398(4) 0.0413(13) Uani 1 1 d . . . H22A H 0.0261 0.7606 0.2032 0.050 Uiso 1 1 calc R . . C18 C 0.1045(3) 0.4926(4) 0.1180(4) 0.0519(16) Uani 1 1 d . . . H18A H 0.1109 0.5479 0.0860 0.062 Uiso 1 1 calc R . . H18B H 0.0627 0.4629 0.0768 0.062 Uiso 1 1 calc R . . C19 C 0.1568(3) 0.4187(5) 0.1386(4) 0.0624(18) Uani 1 1 d . . . H19A H 0.1551 0.3975 0.0821 0.094 Uiso 1 1 calc R . . H19B H 0.1505 0.3630 0.1692 0.094 Uiso 1 1 calc R . . H19C H 0.1985 0.4480 0.1776 0.094 Uiso 1 1 calc R . . C14 C 0.0802(3) 0.4693(4) 0.2436(4) 0.0461(14) Uani 1 1 d . . . H14A H 0.0649 0.4070 0.2190 0.055 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 0.0240(4) 0.0224(4) 0.0278(5) 0.0000(3) 0.0149(4) 0.0009(3) Cl2 0.0332(6) 0.0299(6) 0.0312(6) -0.0036(5) 0.0185(5) 0.0002(5) Cl1 0.0360(7) 0.0291(6) 0.0366(7) -0.0052(5) 0.0197(5) -0.0032(5) N1 0.026(2) 0.0259(19) 0.027(2) -0.0034(16) 0.0146(17) 0.0007(15) O1 0.0260(17) 0.0284(17) 0.0339(18) 0.0046(14) 0.0162(15) 0.0016(13) N2 0.026(2) 0.0246(19) 0.0244(19) -0.0014(15) 0.0140(16) -0.0003(15) C9 0.028(2) 0.030(2) 0.026(2) -0.0024(19) 0.015(2) 0.0046(19) C6 0.031(2) 0.025(2) 0.026(2) -0.0026(18) 0.014(2) -0.0005(18) C12 0.029(3) 0.027(2) 0.031(3) 0.0074(19) 0.016(2) 0.0041(19) C5 0.031(3) 0.032(3) 0.028(2) -0.0048(19) 0.015(2) -0.0032(19) C7 0.026(3) 0.043(3) 0.036(3) -0.011(2) 0.017(2) -0.006(2) C2 0.035(3) 0.031(3) 0.037(3) 0.004(2) 0.017(2) -0.003(2) C1 0.030(2) 0.026(2) 0.027(2) -0.0011(18) 0.015(2) -0.0024(19) C20 0.042(3) 0.039(3) 0.034(3) 0.000(2) 0.020(2) 0.000(2) C4 0.036(3) 0.040(3) 0.037(3) -0.005(2) 0.025(2) -0.006(2) C10 0.036(3) 0.026(2) 0.027(2) -0.0032(19) 0.016(2) 0.0009(19) C17 0.027(2) 0.034(3) 0.033(3) 0.006(2) 0.015(2) 0.001(2) C13 0.041(3) 0.028(3) 0.039(3) 0.009(2) 0.012(2) 0.000(2) C26 0.027(3) 0.029(2) 0.049(3) 0.003(2) 0.021(2) -0.0031(19) C3 0.050(3) 0.035(3) 0.040(3) 0.001(2) 0.030(3) -0.008(2) C8 0.029(3) 0.033(3) 0.033(3) -0.003(2) 0.014(2) 0.006(2) C16 0.037(3) 0.045(3) 0.036(3) 0.009(2) 0.021(2) 0.005(2) C15 0.037(3) 0.042(3) 0.051(3) 0.018(3) 0.024(3) 0.001(2) C11 0.030(3) 0.038(3) 0.048(3) 0.008(2) 0.017(2) 0.008(2) C21 0.043(3) 0.052(3) 0.039(3) 0.003(3) 0.024(3) 0.002(3) C25 0.026(3) 0.034(3) 0.054(3) 0.010(2) 0.018(2) 0.004(2) C24 0.025(2) 0.042(3) 0.037(3) -0.002(2) 0.017(2) -0.001(2) C23 0.029(3) 0.040(3) 0.063(4) -0.015(3) 0.025(3) 0.000(2) C22 0.024(3) 0.066(4) 0.038(3) 0.001(3) 0.018(2) -0.001(2) C18 0.086(5) 0.023(3) 0.040(3) 0.000(2) 0.025(3) -0.005(3) C19 0.076(5) 0.063(4) 0.051(4) -0.009(3) 0.032(4) 0.001(4) C14 0.047(3) 0.030(3) 0.058(4) 0.008(2) 0.023(3) -0.002(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 1.952(3) . ? Ti1 N1 2.135(4) . ? Ti1 C26 2.353(5) . ? Ti1 C22 2.356(5) . ? Ti1 N2 2.376(4) . ? Ti1 C24 2.399(5) . ? Ti1 Cl1 2.4196(15) . ? Ti1 C23 2.423(5) . ? Ti1 C25 2.446(5) . ? Ti1 Cl2 2.4551(14) . ? N1 C9 1.322(6) . ? N1 C6 1.352(6) . ? O1 C1 1.336(5) . ? N2 C10 1.298(6) . ? N2 C12 1.451(6) . ? C9 C8 1.417(6) . ? C9 C10 1.469(7) . ? C6 C5 1.397(7) . ? C6 C1 1.426(6) . ? C12 C13 1.401(7) . ? C12 C17 1.404(7) . ? C5 C7 1.410(7) . ? C5 C4 1.416(7) . ? C7 C8 1.379(7) . ? C7 H7A 0.9500 . ? C2 C1 1.385(6) . ? C2 C3 1.409(7) . ? C2 H2A 0.9500 . ? C20 C21 1.501(7) . ? C20 C17 1.510(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C4 C3 1.369(7) . ? C4 H4A 0.9500 . ? C10 C11 1.506(7) . ? C17 C16 1.393(7) . ? C13 C14 1.371(7) . ? C13 C18 1.512(8) . ? C26 C22 1.388(7) . ? C26 C24 1.401(7) . ? C26 H26A 1.0000 . ? C3 H3A 0.9500 . ? C8 H8A 0.9500 . ? C16 C15 1.369(8) . ? C16 H16A 0.9500 . ? C15 C14 1.385(8) . ? C15 H15A 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C25 C24 1.386(7) . ? C25 C23 1.389(8) . ? C25 H25A 1.0000 . ? C24 H24A 1.0000 . ? C23 C22 1.411(8) . ? C23 H23A 1.0000 . ? C22 H22A 1.0000 . ? C18 C19 1.517(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C14 H14A 0.9500 . ? 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 77.40(14) . . ? O1 Ti1 C26 126.12(16) . . ? N1 Ti1 C26 147.04(16) . . ? O1 Ti1 C22 129.69(17) . . ? N1 Ti1 C22 148.60(17) . . ? C26 Ti1 C22 34.29(18) . . ? O1 Ti1 N2 146.37(13) . . ? N1 Ti1 N2 68.98(14) . . ? C26 Ti1 N2 84.59(15) . . ? C22 Ti1 N2 82.97(17) . . ? O1 Ti1 C24 91.94(16) . . ? N1 Ti1 C24 150.10(16) . . ? C26 Ti1 C24 34.27(17) . . ? C22 Ti1 C24 56.35(18) . . ? N2 Ti1 C24 116.80(16) . . ? O1 Ti1 Cl1 89.05(10) . . ? N1 Ti1 Cl1 76.50(11) . . ? C26 Ti1 Cl1 121.41(14) . . ? C22 Ti1 Cl1 87.26(14) . . ? N2 Ti1 Cl1 84.32(10) . . ? C24 Ti1 Cl1 131.83(13) . . ? O1 Ti1 C23 96.45(17) . . ? N1 Ti1 C23 152.24(16) . . ? C26 Ti1 C23 56.79(18) . . ? C22 Ti1 C23 34.32(19) . . ? N2 Ti1 C23 113.75(17) . . ? C24 Ti1 C23 55.68(18) . . ? Cl1 Ti1 C23 76.36(14) . . ? O1 Ti1 C25 75.96(15) . . ? N1 Ti1 C25 153.34(16) . . ? C26 Ti1 C25 56.22(17) . . ? C22 Ti1 C25 55.95(19) . . ? N2 Ti1 C25 137.66(16) . . ? C24 Ti1 C25 33.23(17) . . ? Cl1 Ti1 C25 101.81(14) . . ? C23 Ti1 C25 33.16(19) . . ? O1 Ti1 Cl2 87.09(10) . . ? N1 Ti1 Cl2 75.50(11) . . ? C26 Ti1 Cl2 82.51(13) . . ? C22 Ti1 Cl2 116.22(15) . . ? N2 Ti1 Cl2 83.63(9) . . ? C24 Ti1 Cl2 76.13(13) . . ? Cl1 Ti1 Cl2 151.91(5) . . ? C23 Ti1 Cl2 131.72(14) . . ? C25 Ti1 Cl2 104.19(14) . . ? C9 N1 C6 120.4(4) . . ? C9 N1 Ti1 125.5(3) . . ? C6 N1 Ti1 114.1(3) . . ? C1 O1 Ti1 118.5(3) . . ? C10 N2 C12 117.5(4) . . ? C10 N2 Ti1 116.1(3) . . ? C12 N2 Ti1 126.4(3) . . ? N1 C9 C8 120.4(4) . . ? N1 C9 C10 113.4(4) . . ? C8 C9 C10 126.1(4) . . ? N1 C6 C5 123.2(4) . . ? N1 C6 C1 112.6(4) . . ? C5 C6 C1 124.2(4) . . ? C13 C12 C17 121.3(4) . . ? C13 C12 N2 119.2(4) . . ? C17 C12 N2 119.5(4) . . ? C6 C5 C7 116.4(4) . . ? C6 C5 C4 117.3(4) . . ? C7 C5 C4 126.3(4) . . ? C8 C7 C5 120.1(4) . . ? C8 C7 H7A 119.9 . . ? C5 C7 H7A 119.9 . . ? C1 C2 C3 119.3(5) . . ? C1 C2 H2A 120.4 . . ? C3 C2 H2A 120.4 . . ? O1 C1 C2 126.0(4) . . ? O1 C1 C6 117.3(4) . . ? C2 C1 C6 116.7(4) . . ? C21 C20 C17 115.8(4) . . ? C21 C20 H20A 108.3 . . ? C17 C20 H20A 108.3 . . ? C21 C20 H20B 108.3 . . ? C17 C20 H20B 108.3 . . ? H20A C20 H20B 107.4 . . ? C3 C4 C5 118.7(4) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? N2 C10 C9 115.8(4) . . ? N2 C10 C11 125.8(4) . . ? C9 C10 C11 118.4(4) . . ? C16 C17 C12 117.3(5) . . ? C16 C17 C20 120.7(5) . . ? C12 C17 C20 122.0(4) . . ? C14 C13 C12 118.4(5) . . ? C14 C13 C18 118.2(5) . . ? C12 C13 C18 123.4(5) . . ? C22 C26 C24 107.3(5) . . ? C22 C26 Ti1 73.0(3) . . ? C24 C26 Ti1 74.7(3) . . ? C22 C26 H26A 126.0 . . ? C24 C26 H26A 126.0 . . ? Ti1 C26 H26A 126.0 . . ? C4 C3 C2 123.8(5) . . ? C4 C3 H3A 118.1 . . ? C2 C3 H3A 118.1 . . ? C7 C8 C9 119.5(4) . . ? C7 C8 H8A 120.2 . . ? C9 C8 H8A 120.2 . . ? C15 C16 C17 122.0(5) . . ? C15 C16 H16A 119.0 . . ? C17 C16 H16A 119.0 . . ? C16 C15 C14 119.2(5) . . ? C16 C15 H15A 120.4 . . ? C14 C15 H15A 120.4 . . ? 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 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C25 C23 108.5(5) . . ? C24 C25 Ti1 71.5(3) . . ? C23 C25 Ti1 72.5(3) . . ? C24 C25 H25A 125.7 . . ? C23 C25 H25A 125.7 . . ? Ti1 C25 H25A 125.7 . . ? C25 C24 C26 108.5(5) . . ? C25 C24 Ti1 75.2(3) . . ? C26 C24 Ti1 71.0(3) . . ? C25 C24 H24A 125.5 . . ? C26 C24 H24A 125.5 . . ? Ti1 C24 H24A 125.5 . . ? C25 C23 C22 107.2(5) . . ? C25 C23 Ti1 74.3(3) . . ? C22 C23 Ti1 70.3(3) . . ? C25 C23 H23A 126.2 . . ? C22 C23 H23A 126.2 . . ? Ti1 C23 H23A 126.2 . . ? C26 C22 C23 108.5(5) . . ? C26 C22 Ti1 72.7(3) . . ? C23 C22 Ti1 75.4(3) . . ? C26 C22 H22A 125.4 . . ? C23 C22 H22A 125.4 . . ? Ti1 C22 H22A 125.4 . . ? C13 C18 C19 114.0(5) . . ? C13 C18 H18A 108.7 . . ? C19 C18 H18A 108.7 . . ? C13 C18 H18B 108.7 . . ? C19 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C13 C14 C15 121.6(5) . . ? C13 C14 H14A 119.2 . . ? C15 C14 H14A 119.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ti1 N1 C9 -179.5(4) . . . . ? C26 Ti1 N1 C9 -39.5(5) . . . . ? C22 Ti1 N1 C9 27.7(6) . . . . ? N2 Ti1 N1 C9 -0.6(3) . . . . ? C24 Ti1 N1 C9 -108.1(4) . . . . ? Cl1 Ti1 N1 C9 88.5(4) . . . . ? C23 Ti1 N1 C9 100.8(5) . . . . ? C25 Ti1 N1 C9 178.0(4) . . . . ? Cl2 Ti1 N1 C9 -89.2(4) . . . . ? O1 Ti1 N1 C6 -1.7(3) . . . . ? C26 Ti1 N1 C6 138.2(3) . . . . ? C22 Ti1 N1 C6 -154.6(4) . . . . ? N2 Ti1 N1 C6 177.2(3) . . . . ? C24 Ti1 N1 C6 69.7(5) . . . . ? Cl1 Ti1 N1 C6 -93.8(3) . . . . ? C23 Ti1 N1 C6 -81.5(5) . . . . ? C25 Ti1 N1 C6 -4.3(5) . . . . ? Cl2 Ti1 N1 C6 88.5(3) . . . . ? N1 Ti1 O1 C1 1.7(3) . . . . ? C26 Ti1 O1 C1 -152.6(3) . . . . ? C22 Ti1 O1 C1 163.7(3) . . . . ? N2 Ti1 O1 C1 -0.2(4) . . . . ? C24 Ti1 O1 C1 -150.1(3) . . . . ? Cl1 Ti1 O1 C1 78.1(3) . . . . ? C23 Ti1 O1 C1 154.2(3) . . . . ? C25 Ti1 O1 C1 -179.5(4) . . . . ? Cl2 Ti1 O1 C1 -74.1(3) . . . . ? O1 Ti1 N2 C10 5.2(5) . . . . ? N1 Ti1 N2 C10 3.2(3) . . . . ? C26 Ti1 N2 C10 163.2(3) . . . . ? C22 Ti1 N2 C10 -162.4(3) . . . . ? C24 Ti1 N2 C10 151.1(3) . . . . ? Cl1 Ti1 N2 C10 -74.5(3) . . . . ? C23 Ti1 N2 C10 -146.8(3) . . . . ? C25 Ti1 N2 C10 -175.8(3) . . . . ? Cl2 Ti1 N2 C10 80.1(3) . . . . ? O1 Ti1 N2 C12 -176.3(3) . . . . ? N1 Ti1 N2 C12 -178.3(4) . . . . ? C26 Ti1 N2 C12 -18.3(4) . . . . ? C22 Ti1 N2 C12 16.1(4) . . . . ? C24 Ti1 N2 C12 -30.4(4) . . . . ? Cl1 Ti1 N2 C12 104.1(3) . . . . ? C23 Ti1 N2 C12 31.7(4) . . . . ? C25 Ti1 N2 C12 2.7(5) . . . . ? Cl2 Ti1 N2 C12 -101.4(3) . . . . ? C6 N1 C9 C8 -1.7(6) . . . . ? Ti1 N1 C9 C8 175.9(3) . . . . ? C6 N1 C9 C10 -179.4(4) . . . . ? Ti1 N1 C9 C10 -1.8(5) . . . . ? C9 N1 C6 C5 0.8(7) . . . . ? Ti1 N1 C6 C5 -177.0(3) . . . . ? C9 N1 C6 C1 179.3(4) . . . . ? Ti1 N1 C6 C1 1.5(5) . . . . ? C10 N2 C12 C13 -89.0(5) . . . . ? Ti1 N2 C12 C13 92.5(5) . . . . ? C10 N2 C12 C17 87.9(5) . . . . ? Ti1 N2 C12 C17 -90.6(5) . . . . ? N1 C6 C5 C7 0.6(7) . . . . ? C1 C6 C5 C7 -177.7(4) . . . . ? N1 C6 C5 C4 178.4(4) . . . . ? C1 C6 C5 C4 0.1(7) . . . . ? C6 C5 C7 C8 -1.1(7) . . . . ? C4 C5 C7 C8 -178.7(5) . . . . ? Ti1 O1 C1 C2 176.7(4) . . . . ? Ti1 O1 C1 C6 -1.5(5) . . . . ? C3 C2 C1 O1 -178.4(4) . . . . ? C3 C2 C1 C6 -0.1(7) . . . . ? N1 C6 C1 O1 -0.1(6) . . . . ? C5 C6 C1 O1 178.4(4) . . . . ? N1 C6 C1 C2 -178.5(4) . . . . ? C5 C6 C1 C2 0.0(7) . . . . ? C6 C5 C4 C3 0.0(7) . . . . ? C7 C5 C4 C3 177.5(5) . . . . ? C12 N2 C10 C9 176.1(4) . . . . ? Ti1 N2 C10 C9 -5.2(5) . . . . ? C12 N2 C10 C11 -4.7(7) . . . . ? Ti1 N2 C10 C11 173.9(4) . . . . ? N1 C9 C10 N2 4.7(6) . . . . ? C8 C9 C10 N2 -172.8(4) . . . . ? N1 C9 C10 C11 -174.5(4) . . . . ? C8 C9 C10 C11 7.9(7) . . . . ? C13 C12 C17 C16 -4.9(7) . . . . ? N2 C12 C17 C16 178.2(4) . . . . ? C13 C12 C17 C20 174.8(5) . . . . ? N2 C12 C17 C20 -2.1(7) . . . . ? C21 C20 C17 C16 11.0(7) . . . . ? C21 C20 C17 C12 -168.7(5) . . . . ? C17 C12 C13 C14 4.0(8) . . . . ? N2 C12 C13 C14 -179.1(5) . . . . ? C17 C12 C13 C18 -173.0(5) . . . . ? N2 C12 C13 C18 3.9(7) . . . . ? O1 Ti1 C26 C22 -109.5(3) . . . . ? N1 Ti1 C26 C22 121.5(4) . . . . ? N2 Ti1 C26 C22 85.5(3) . . . . ? C24 Ti1 C26 C22 -113.9(4) . . . . ? Cl1 Ti1 C26 C22 5.5(4) . . . . ? C23 Ti1 C26 C22 -37.6(3) . . . . ? C25 Ti1 C26 C22 -77.6(3) . . . . ? Cl2 Ti1 C26 C22 169.7(3) . . . . ? O1 Ti1 C26 C24 4.5(4) . . . . ? N1 Ti1 C26 C24 -124.5(3) . . . . ? C22 Ti1 C26 C24 113.9(4) . . . . ? N2 Ti1 C26 C24 -160.6(3) . . . . ? Cl1 Ti1 C26 C24 119.4(3) . . . . ? C23 Ti1 C26 C24 76.3(3) . . . . ? C25 Ti1 C26 C24 36.3(3) . . . . ? Cl2 Ti1 C26 C24 -76.3(3) . . . . ? C5 C4 C3 C2 -0.1(8) . . . . ? C1 C2 C3 C4 0.2(8) . . . . ? C5 C7 C8 C9 0.3(7) . . . . ? N1 C9 C8 C7 1.2(7) . . . . ? C10 C9 C8 C7 178.6(4) . . . . ? C12 C17 C16 C15 2.0(7) . . . . ? C20 C17 C16 C15 -177.7(5) . . . . ? C17 C16 C15 C14 1.7(8) . . . . ? O1 Ti1 C25 C24 116.4(3) . . . . ? N1 Ti1 C25 C24 119.0(4) . . . . ? C26 Ti1 C25 C24 -37.5(3) . . . . ? C22 Ti1 C25 C24 -79.1(3) . . . . ? N2 Ti1 C25 C24 -63.0(4) . . . . ? Cl1 Ti1 C25 C24 -157.6(3) . . . . ? C23 Ti1 C25 C24 -117.1(5) . . . . ? Cl2 Ti1 C25 C24 33.2(3) . . . . ? O1 Ti1 C25 C23 -126.5(3) . . . . ? N1 Ti1 C25 C23 -123.9(4) . . . . ? C26 Ti1 C25 C23 79.6(3) . . . . ? C22 Ti1 C25 C23 38.0(3) . . . . ? N2 Ti1 C25 C23 54.1(4) . . . . ? C24 Ti1 C25 C23 117.1(5) . . . . ? Cl1 Ti1 C25 C23 -40.5(3) . . . . ? Cl2 Ti1 C25 C23 150.3(3) . . . . ? C23 C25 C24 C26 0.2(6) . . . . ? Ti1 C25 C24 C26 63.7(3) . . . . ? C23 C25 C24 Ti1 -63.6(4) . . . . ? C22 C26 C24 C25 -0.2(6) . . . . ? Ti1 C26 C24 C25 -66.4(4) . . . . ? C22 C26 C24 Ti1 66.3(3) . . . . ? O1 Ti1 C24 C25 -60.4(3) . . . . ? N1 Ti1 C24 C25 -128.1(4) . . . . ? C26 Ti1 C24 C25 116.0(4) . . . . ? C22 Ti1 C24 C25 77.8(3) . . . . ? N2 Ti1 C24 C25 137.8(3) . . . . ? Cl1 Ti1 C24 C25 30.1(4) . . . . ? C23 Ti1 C24 C25 36.1(3) . . . . ? Cl2 Ti1 C24 C25 -146.9(3) . . . . ? O1 Ti1 C24 C26 -176.4(3) . . . . ? N1 Ti1 C24 C26 115.9(4) . . . . ? C22 Ti1 C24 C26 -38.2(3) . . . . ? N2 Ti1 C24 C26 21.8(3) . . . . ? Cl1 Ti1 C24 C26 -85.9(3) . . . . ? C23 Ti1 C24 C26 -79.9(3) . . . . ? C25 Ti1 C24 C26 -116.0(4) . . . . ? Cl2 Ti1 C24 C26 97.1(3) . . . . ? C24 C25 C23 C22 -0.1(6) . . . . ? Ti1 C25 C23 C22 -63.0(3) . . . . ? C24 C25 C23 Ti1 62.9(4) . . . . ? O1 Ti1 C23 C25 51.7(3) . . . . ? N1 Ti1 C23 C25 126.9(4) . . . . ? C26 Ti1 C23 C25 -77.7(3) . . . . ? C22 Ti1 C23 C25 -115.3(5) . . . . ? N2 Ti1 C23 C25 -143.4(3) . . . . ? C24 Ti1 C23 C25 -36.2(3) . . . . ? Cl1 Ti1 C23 C25 139.2(3) . . . . ? Cl2 Ti1 C23 C25 -40.1(4) . . . . ? O1 Ti1 C23 C22 167.0(3) . . . . ? N1 Ti1 C23 C22 -117.9(4) . . . . ? C26 Ti1 C23 C22 37.6(3) . . . . ? N2 Ti1 C23 C22 -28.2(4) . . . . ? C24 Ti1 C23 C22 79.1(3) . . . . ? Cl1 Ti1 C23 C22 -105.6(3) . . . . ? C25 Ti1 C23 C22 115.3(5) . . . . ? Cl2 Ti1 C23 C22 75.1(4) . . . . ? C24 C26 C22 C23 0.1(5) . . . . ? Ti1 C26 C22 C23 67.5(4) . . . . ? C24 C26 C22 Ti1 -67.4(3) . . . . ? C25 C23 C22 C26 0.0(6) . . . . ? Ti1 C23 C22 C26 -65.8(3) . . . . ? C25 C23 C22 Ti1 65.7(4) . . . . ? O1 Ti1 C22 C26 98.2(3) . . . . ? N1 Ti1 C22 C26 -117.1(4) . . . . ? N2 Ti1 C22 C26 -90.7(3) . . . . ? C24 Ti1 C22 C26 38.2(3) . . . . ? Cl1 Ti1 C22 C26 -175.3(3) . . . . ? C23 Ti1 C22 C26 115.1(5) . . . . ? C25 Ti1 C22 C26 78.4(3) . . . . ? Cl2 Ti1 C22 C26 -11.4(3) . . . . ? O1 Ti1 C22 C23 -16.9(4) . . . . ? N1 Ti1 C22 C23 127.8(4) . . . . ? C26 Ti1 C22 C23 -115.1(5) . . . . ? N2 Ti1 C22 C23 154.2(3) . . . . ? C24 Ti1 C22 C23 -76.9(3) . . . . ? Cl1 Ti1 C22 C23 69.6(3) . . . . ? C25 Ti1 C22 C23 -36.6(3) . . . . ? Cl2 Ti1 C22 C23 -126.5(3) . . . . ? C14 C13 C18 C19 -72.5(7) . . . . ? C12 C13 C18 C19 104.5(6) . . . . ? C12 C13 C14 C15 -0.1(8) . . . . ? C18 C13 C14 C15 177.0(5) . . . . ? C16 C15 C14 C13 -2.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.508 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.096 _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 1.000 0.158 0.250 120 34 ' ' 2 1.000 -0.158 0.750 120 34 ' ' 3 0.500 0.342 0.750 120 34 ' ' 4 0.500 0.658 0.250 120 34 ' ' _platon_squeeze_details ; ; #==END data_C4 _database_code_depnum_ccdc_archive 'CCDC 822120' #TrackingRef '- CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H28 Cl2 N2 O Ti' _chemical_formula_weight 515.31 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.098(3) _cell_length_b 8.1446(16) _cell_length_c 17.624(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.70(3) _cell_angle_gamma 90.00 _cell_volume 2426.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7380 _cell_measurement_theta_min 1.20 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour RED _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.596 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.6901 _exptl_absorpt_correction_T_max 0.7532 _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 none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 19063 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5545 _reflns_number_gt 5203 _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^)+(0.0684P)^2^+2.9519P] 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 5545 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.1799 _refine_ls_wR_factor_gt 0.1720 _refine_ls_goodness_of_fit_ref 1.247 _refine_ls_restrained_S_all 1.247 _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 0.21876(3) 0.16179(8) 0.13194(3) 0.02828(18) Uani 1 1 d . . . Cl2 Cl 0.13816(5) -0.02239(11) 0.19705(5) 0.0381(2) Uani 1 1 d . . . Cl1 Cl 0.24758(5) 0.43307(11) 0.08483(5) 0.0364(2) Uani 1 1 d . . . O1 O 0.14549(14) 0.1277(3) 0.03664(13) 0.0330(5) Uani 1 1 d . . . N1 N 0.11874(16) 0.3056(4) 0.14932(15) 0.0296(6) Uani 1 1 d . . . C6 C 0.05830(19) 0.2973(4) 0.09129(18) 0.0306(7) Uani 1 1 d . . . N2 N 0.24255(15) 0.2965(3) 0.25312(14) 0.0277(6) Uani 1 1 d . . . C12 C 0.31391(18) 0.2885(4) 0.31042(17) 0.0280(7) Uani 1 1 d . . . C10 C 0.18448(19) 0.3851(4) 0.26999(19) 0.0312(7) Uani 1 1 d . . . C15 C 0.4513(2) 0.2673(4) 0.4195(2) 0.0350(7) Uani 1 1 d . . . C2 C 0.0151(2) 0.1839(5) -0.03362(19) 0.0348(7) Uani 1 1 d . . . H2A H 0.0231 0.1204 -0.0757 0.042 Uiso 1 1 calc R . . C13 C 0.37419(19) 0.4033(4) 0.30862(19) 0.0310(7) Uani 1 1 d . B . C5 C -0.01476(19) 0.3762(5) 0.0927(2) 0.0337(7) Uani 1 1 d . . . C17 C 0.3195(2) 0.1678(4) 0.36750(18) 0.0320(7) Uani 1 1 d . . . C1 C 0.07450(19) 0.1991(4) 0.02869(18) 0.0302(7) Uani 1 1 d . . . C7 C -0.0205(2) 0.4673(5) 0.1601(2) 0.0405(9) Uani 1 1 d . . . H7A H -0.0671 0.5233 0.1644 0.049 Uiso 1 1 calc R . . C16 C 0.3894(2) 0.1590(4) 0.42025(19) 0.0346(7) Uani 1 1 d . . . H16A H 0.3943 0.0769 0.4573 0.042 Uiso 1 1 calc R . . C24 C 0.2786(3) -0.0511(6) 0.0650(3) 0.0593(13) Uani 1 1 d . . . H24A H 0.2512 -0.1135 0.0213 0.071 Uiso 1 1 calc R . . C8 C 0.0417(2) 0.4740(5) 0.2191(2) 0.0372(8) Uani 1 1 d . . . H8A H 0.0371 0.5327 0.2634 0.045 Uiso 1 1 calc R . . C14 C 0.4425(2) 0.3891(4) 0.3634(2) 0.0335(7) Uani 1 1 d . . . H14A H 0.4834 0.4638 0.3622 0.040 Uiso 1 1 calc R . . C18 C 0.3663(2) 0.5452(5) 0.2526(2) 0.0384(8) Uani 1 1 d . . . H18A H 0.3172 0.5317 0.2175 0.046 Uiso 1 1 calc R A 1 H18B H 0.3619 0.6457 0.2811 0.046 Uiso 1 1 calc R A 1 C3 C -0.0575(2) 0.2651(5) -0.0329(2) 0.0384(8) Uani 1 1 d . . . H3A H -0.0966 0.2549 -0.0755 0.046 Uiso 1 1 calc R . . C4 C -0.0732(2) 0.3583(5) 0.0276(2) 0.0380(8) Uani 1 1 d . . . H4A H -0.1221 0.4095 0.0257 0.046 Uiso 1 1 calc R . . C9 C 0.1127(2) 0.3914(4) 0.21213(19) 0.0317(7) Uani 1 1 d . . . C11 C 0.1857(2) 0.4770(5) 0.3438(2) 0.0441(9) Uani 1 1 d . . . H11A H 0.2360 0.4614 0.3755 0.066 Uiso 1 1 calc R . . H11B H 0.1443 0.4367 0.3701 0.066 Uiso 1 1 calc R . . H11C H 0.1776 0.5919 0.3331 0.066 Uiso 1 1 calc R . . C22 C 0.5254(2) 0.2563(6) 0.4778(2) 0.0500(10) Uani 1 1 d . . . H22A H 0.5210 0.1658 0.5118 0.075 Uiso 1 1 calc R . . H22B H 0.5322 0.3564 0.5069 0.075 Uiso 1 1 calc R . . H22C H 0.5703 0.2397 0.4519 0.075 Uiso 1 1 calc R . . C26 C 0.3551(2) 0.1322(6) 0.1341(5) 0.084(2) Uani 1 1 d . . . H26A H 0.3960 0.2162 0.1476 0.101 Uiso 1 1 calc R . . C27 C 0.3322(3) 0.0076(8) 0.1827(2) 0.0644(15) Uani 1 1 d . . . H27A H 0.3529 -0.0077 0.2372 0.077 Uiso 1 1 calc R . . C25 C 0.3183(3) 0.0874(7) 0.0593(3) 0.0662(16) Uani 1 1 d . . . H25A H 0.3277 0.1393 0.0113 0.079 Uiso 1 1 calc R . . C19 C 0.4311(8) 0.565(3) 0.2069(10) 0.057(4) Uani 0.51(4) 1 d P B 1 H19A H 0.4205 0.6584 0.1736 0.086 Uiso 0.51(4) 1 calc PR B 1 H19B H 0.4350 0.4683 0.1768 0.086 Uiso 0.51(4) 1 calc PR B 1 H19C H 0.4800 0.5820 0.2407 0.086 Uiso 0.51(4) 1 calc PR B 1 C19' C 0.4402(6) 0.639(3) 0.2462(19) 0.073(8) Uani 0.49(4) 1 d P B 2 H19D H 0.4283 0.7264 0.2096 0.109 Uiso 0.49(4) 1 calc PR B 2 H19E H 0.4786 0.5669 0.2295 0.109 Uiso 0.49(4) 1 calc PR B 2 H19F H 0.4612 0.6846 0.2953 0.109 Uiso 0.49(4) 1 calc PR B 2 C23 C 0.2862(3) -0.0992(6) 0.1373(3) 0.0630(13) Uani 1 1 d . . . H23A H 0.2653 -0.2022 0.1549 0.076 Uiso 1 1 calc R . . C21 C 0.2743(3) -0.1186(6) 0.3990(3) 0.0688(15) Uani 1 1 d . . . H21A H 0.2278 -0.1811 0.4040 0.103 Uiso 1 1 calc R . . H21B H 0.3092 -0.1183 0.4471 0.103 Uiso 1 1 calc R . . H21C H 0.3008 -0.1670 0.3602 0.103 Uiso 1 1 calc R . . C20 C 0.2510(2) 0.0556(5) 0.3766(2) 0.0438(9) Uani 1 1 d . . . H20A H 0.2226 0.1016 0.4153 0.053 Uiso 1 1 calc R . . H20B H 0.2150 0.0534 0.3285 0.053 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 0.0258(3) 0.0369(3) 0.0221(3) 0.0002(2) 0.0033(2) 0.0060(2) Cl2 0.0412(5) 0.0437(5) 0.0293(4) -0.0009(3) 0.0049(3) -0.0070(4) Cl1 0.0347(4) 0.0422(5) 0.0323(4) 0.0063(3) 0.0057(3) 0.0028(4) O1 0.0323(12) 0.0413(13) 0.0246(11) -0.0017(10) 0.0013(9) 0.0072(10) N1 0.0255(13) 0.0377(15) 0.0257(13) -0.0015(11) 0.0040(10) 0.0035(12) C6 0.0250(16) 0.0380(18) 0.0281(15) 0.0022(13) 0.0016(12) -0.0006(13) N2 0.0229(13) 0.0347(14) 0.0251(13) 0.0010(11) 0.0028(10) -0.0015(11) C12 0.0228(15) 0.0358(17) 0.0248(14) -0.0009(13) 0.0018(11) -0.0011(13) C10 0.0260(16) 0.0397(18) 0.0281(15) -0.0057(14) 0.0050(12) -0.0031(14) C15 0.0315(17) 0.0362(18) 0.0347(17) -0.0003(14) -0.0027(14) -0.0005(15) C2 0.0373(18) 0.0401(19) 0.0256(15) -0.0018(14) 0.0004(13) -0.0008(15) C13 0.0270(16) 0.0326(17) 0.0329(17) 0.0032(14) 0.0036(13) -0.0024(14) C5 0.0237(16) 0.0435(19) 0.0333(17) 0.0022(15) 0.0024(13) 0.0007(14) C17 0.0340(18) 0.0377(18) 0.0240(15) -0.0027(13) 0.0038(12) -0.0082(15) C1 0.0287(16) 0.0343(17) 0.0268(15) 0.0018(13) 0.0019(12) 0.0016(14) C7 0.0274(17) 0.054(2) 0.042(2) -0.0018(17) 0.0109(15) 0.0080(16) C16 0.0385(19) 0.0354(18) 0.0276(16) 0.0030(13) -0.0028(13) -0.0032(15) C24 0.061(3) 0.061(3) 0.052(3) -0.017(2) -0.004(2) 0.032(2) C8 0.0285(17) 0.051(2) 0.0332(17) -0.0081(16) 0.0084(14) 0.0054(16) C14 0.0258(16) 0.0342(17) 0.0387(18) 0.0011(14) -0.0014(13) -0.0049(14) C18 0.0314(18) 0.0352(19) 0.047(2) 0.0085(16) -0.0016(15) -0.0051(15) C3 0.0319(18) 0.048(2) 0.0325(17) 0.0038(15) -0.0061(14) -0.0031(16) C4 0.0214(16) 0.051(2) 0.0403(19) 0.0059(16) -0.0006(13) 0.0028(15) C9 0.0261(16) 0.0374(18) 0.0315(16) -0.0060(14) 0.0039(13) 0.0006(14) C11 0.0348(19) 0.057(2) 0.039(2) -0.0196(18) 0.0014(15) 0.0012(17) C22 0.038(2) 0.053(2) 0.052(2) 0.0132(19) -0.0125(17) -0.0069(18) C26 0.0192(19) 0.048(3) 0.186(7) -0.041(4) 0.016(3) 0.0051(18) C27 0.057(3) 0.097(4) 0.036(2) -0.007(2) -0.0044(19) 0.052(3) C25 0.066(3) 0.080(4) 0.063(3) 0.026(3) 0.044(3) 0.045(3) C19 0.042(6) 0.073(9) 0.058(7) 0.026(7) 0.010(5) -0.008(6) C19' 0.032(5) 0.064(10) 0.118(17) 0.052(11) -0.004(6) -0.011(5) C23 0.051(3) 0.047(3) 0.094(4) 0.011(3) 0.020(3) 0.019(2) C21 0.073(3) 0.042(2) 0.102(4) -0.019(3) 0.044(3) -0.020(2) C20 0.042(2) 0.057(2) 0.0296(17) 0.0097(16) -0.0029(15) -0.0207(18) _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 1.957(2) . ? Ti1 N1 2.133(3) . ? Ti1 C26 2.339(4) . ? Ti1 C25 2.358(4) . ? Ti1 C27 2.370(4) . ? Ti1 N2 2.381(3) . ? Ti1 C24 2.410(4) . ? Ti1 C23 2.413(4) . ? Ti1 Cl1 2.4368(12) . ? Ti1 Cl2 2.4381(11) . ? O1 C1 1.334(4) . ? N1 C9 1.326(4) . ? N1 C6 1.341(4) . ? C6 C5 1.409(5) . ? C6 C1 1.423(5) . ? N2 C10 1.298(4) . ? N2 C12 1.463(4) . ? C12 C13 1.395(5) . ? C12 C17 1.399(5) . ? C10 C9 1.473(4) . ? C10 C11 1.498(5) . ? C15 C16 1.379(5) . ? C15 C14 1.393(5) . ? C15 C22 1.509(5) . ? C2 C1 1.384(4) . ? C2 C3 1.409(5) . ? C2 H2A 0.9300 . ? C13 C14 1.403(4) . ? C13 C18 1.513(5) . ? C5 C4 1.412(5) . ? C5 C7 1.416(5) . ? C17 C16 1.401(5) . ? C17 C20 1.512(5) . ? C7 C8 1.371(5) . ? C7 H7A 0.9300 . ? C16 H16A 0.9300 . ? C24 C23 1.321(7) . ? C24 C25 1.329(8) . ? C24 H24A 0.9800 . ? C8 C9 1.409(5) . ? C8 H8A 0.9300 . ? C14 H14A 0.9300 . ? C18 C19 1.474(11) . ? C18 C19' 1.497(11) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C3 C4 1.368(5) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C26 C25 1.419(8) . ? C26 C27 1.421(8) . ? C26 H26A 0.9800 . ? C27 C23 1.351(7) . ? C27 H27A 0.9800 . ? C25 H25A 0.9800 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C19' H19D 0.9600 . ? C19' H19E 0.9600 . ? C19' H19F 0.9600 . ? C23 H23A 0.9800 . ? C21 C20 1.510(7) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? 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 77.17(10) . . ? O1 Ti1 C26 120.4(2) . . ? N1 Ti1 C26 150.85(14) . . ? O1 Ti1 C25 85.35(17) . . ? N1 Ti1 C25 151.56(14) . . ? C26 Ti1 C25 35.2(2) . . ? O1 Ti1 C27 129.03(14) . . ? N1 Ti1 C27 149.93(13) . . ? C26 Ti1 C27 35.1(2) . . ? C25 Ti1 C27 56.74(17) . . ? O1 Ti1 N2 146.66(10) . . ? N1 Ti1 N2 69.51(10) . . ? C26 Ti1 N2 89.90(18) . . ? C25 Ti1 N2 124.45(18) . . ? C27 Ti1 N2 83.51(13) . . ? O1 Ti1 C24 75.04(13) . . ? N1 Ti1 C24 150.94(14) . . ? C26 Ti1 C24 55.82(18) . . ? C25 Ti1 C24 32.34(19) . . ? C27 Ti1 C24 54.51(16) . . ? N2 Ti1 C24 138.00(13) . . ? O1 Ti1 C23 98.55(16) . . ? N1 Ti1 C23 150.08(15) . . ? C26 Ti1 C23 55.91(18) . . ? C25 Ti1 C23 54.22(18) . . ? C27 Ti1 C23 32.79(18) . . ? N2 Ti1 C23 110.81(16) . . ? C24 Ti1 C23 31.78(17) . . ? O1 Ti1 Cl1 88.41(8) . . ? N1 Ti1 Cl1 76.05(8) . . ? C26 Ti1 Cl1 81.16(16) . . ? C25 Ti1 Cl1 81.27(14) . . ? C27 Ti1 Cl1 114.39(17) . . ? N2 Ti1 Cl1 82.63(7) . . ? C24 Ti1 Cl1 111.28(15) . . ? C23 Ti1 Cl1 133.79(13) . . ? O1 Ti1 Cl2 89.01(8) . . ? N1 Ti1 Cl2 75.38(8) . . ? C26 Ti1 Cl2 124.21(18) . . ? C25 Ti1 Cl2 127.10(15) . . ? C27 Ti1 Cl2 89.15(16) . . ? N2 Ti1 Cl2 83.88(7) . . ? C24 Ti1 Cl2 95.72(15) . . ? C23 Ti1 Cl2 74.95(13) . . ? Cl1 Ti1 Cl2 151.17(4) . . ? C1 O1 Ti1 118.9(2) . . ? C9 N1 C6 121.0(3) . . ? C9 N1 Ti1 125.1(2) . . ? C6 N1 Ti1 113.9(2) . . ? N1 C6 C5 123.1(3) . . ? N1 C6 C1 113.7(3) . . ? C5 C6 C1 123.2(3) . . ? C10 N2 C12 117.0(3) . . ? C10 N2 Ti1 115.4(2) . . ? C12 N2 Ti1 127.6(2) . . ? C13 C12 C17 121.1(3) . . ? C13 C12 N2 119.7(3) . . ? C17 C12 N2 119.1(3) . . ? N2 C10 C9 116.5(3) . . ? N2 C10 C11 124.5(3) . . ? C9 C10 C11 119.0(3) . . ? C16 C15 C14 117.5(3) . . ? C16 C15 C22 121.5(3) . . ? C14 C15 C22 121.0(3) . . ? C1 C2 C3 119.5(3) . . ? C1 C2 H2A 120.2 . . ? C3 C2 H2A 120.2 . . ? C12 C13 C14 118.0(3) . . ? C12 C13 C18 122.2(3) . . ? C14 C13 C18 119.7(3) . . ? C6 C5 C4 117.3(3) . . ? C6 C5 C7 115.4(3) . . ? C4 C5 C7 127.3(3) . . ? C12 C17 C16 118.1(3) . . ? C12 C17 C20 122.0(3) . . ? C16 C17 C20 119.7(3) . . ? O1 C1 C2 126.2(3) . . ? O1 C1 C6 116.4(3) . . ? C2 C1 C6 117.4(3) . . ? C8 C7 C5 120.8(3) . . ? C8 C7 H7A 119.6 . . ? C5 C7 H7A 119.6 . . ? C15 C16 C17 122.7(3) . . ? C15 C16 H16A 118.6 . . ? C17 C16 H16A 118.6 . . ? C23 C24 C25 110.3(5) . . ? C23 C24 Ti1 74.2(3) . . ? C25 C24 Ti1 71.7(3) . . ? C23 C24 H24A 124.7 . . ? C25 C24 H24A 124.7 . . ? Ti1 C24 H24A 124.7 . . ? C7 C8 C9 119.7(3) . . ? C7 C8 H8A 120.2 . . ? C9 C8 H8A 120.2 . . ? C15 C14 C13 122.4(3) . . ? C15 C14 H14A 118.8 . . ? C13 C14 H14A 118.8 . . ? C19 C18 C19' 35.8(8) . . ? C19 C18 C13 116.1(6) . . ? C19' C18 C13 116.6(6) . . ? C19 C18 H18A 108.3 . . ? C19' C18 H18A 131.9 . . ? C13 C18 H18A 108.3 . . ? C19 C18 H18B 108.3 . . ? C19' C18 H18B 74.9 . . ? C13 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? C4 C3 C2 123.0(3) . . ? C4 C3 H3A 118.5 . . ? C2 C3 H3A 118.5 . . ? C3 C4 C5 119.5(3) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? N1 C9 C8 120.0(3) . . ? N1 C9 C10 113.4(3) . . ? C8 C9 C10 126.5(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 . . ? C15 C22 H22A 109.5 . . ? C15 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C15 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C25 C26 C27 104.6(4) . . ? C25 C26 Ti1 73.2(2) . . ? C27 C26 Ti1 73.6(3) . . ? C25 C26 H26A 127.1 . . ? C27 C26 H26A 127.1 . . ? Ti1 C26 H26A 127.1 . . ? C23 C27 C26 107.0(4) . . ? C23 C27 Ti1 75.4(3) . . ? C26 C27 Ti1 71.3(2) . . ? C23 C27 H27A 126.1 . . ? C26 C27 H27A 126.1 . . ? Ti1 C27 H27A 126.1 . . ? C24 C25 C26 108.0(5) . . ? C24 C25 Ti1 76.0(3) . . ? C26 C25 Ti1 71.7(2) . . ? C24 C25 H25A 125.7 . . ? C26 C25 H25A 125.7 . . ? Ti1 C25 H25A 125.7 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C19' H19D 109.5 . . ? C18 C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? C18 C19' H19F 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? C24 C23 C27 110.1(5) . . ? C24 C23 Ti1 74.0(3) . . ? C27 C23 Ti1 71.8(3) . . ? C24 C23 H23A 124.9 . . ? C27 C23 H23A 124.9 . . ? Ti1 C23 H23A 124.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C21 C20 C17 114.7(4) . . ? C21 C20 H20A 108.6 . . ? C17 C20 H20A 108.6 . . ? C21 C20 H20B 108.6 . . ? C17 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? 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 N1 Ti1 O1 C1 -1.4(2) . . . . ? C26 Ti1 O1 C1 -156.3(3) . . . . ? C25 Ti1 O1 C1 -158.8(3) . . . . ? C27 Ti1 O1 C1 161.9(3) . . . . ? N2 Ti1 O1 C1 -3.5(3) . . . . ? C24 Ti1 O1 C1 170.0(3) . . . . ? C23 Ti1 O1 C1 148.4(3) . . . . ? Cl1 Ti1 O1 C1 -77.5(2) . . . . ? Cl2 Ti1 O1 C1 73.8(2) . . . . ? O1 Ti1 N1 C9 179.2(3) . . . . ? C26 Ti1 N1 C9 -49.7(6) . . . . ? C25 Ti1 N1 C9 -127.4(4) . . . . ? C27 Ti1 N1 C9 25.6(5) . . . . ? N2 Ti1 N1 C9 -2.0(3) . . . . ? C24 Ti1 N1 C9 161.9(4) . . . . ? C23 Ti1 N1 C9 94.3(4) . . . . ? Cl1 Ti1 N1 C9 -89.3(3) . . . . ? Cl2 Ti1 N1 C9 86.8(3) . . . . ? O1 Ti1 N1 C6 2.0(2) . . . . ? C26 Ti1 N1 C6 133.2(5) . . . . ? C25 Ti1 N1 C6 55.5(5) . . . . ? C27 Ti1 N1 C6 -151.6(4) . . . . ? N2 Ti1 N1 C6 -179.2(3) . . . . ? C24 Ti1 N1 C6 -15.2(5) . . . . ? C23 Ti1 N1 C6 -82.8(4) . . . . ? Cl1 Ti1 N1 C6 93.6(2) . . . . ? Cl2 Ti1 N1 C6 -90.3(2) . . . . ? C9 N1 C6 C5 -0.5(5) . . . . ? Ti1 N1 C6 C5 176.8(3) . . . . ? C9 N1 C6 C1 -179.5(3) . . . . ? Ti1 N1 C6 C1 -2.3(4) . . . . ? O1 Ti1 N2 C10 3.4(3) . . . . ? N1 Ti1 N2 C10 1.3(2) . . . . ? C26 Ti1 N2 C10 160.2(3) . . . . ? C25 Ti1 N2 C10 153.1(3) . . . . ? C27 Ti1 N2 C10 -165.2(3) . . . . ? C24 Ti1 N2 C10 -167.1(3) . . . . ? C23 Ti1 N2 C10 -146.7(3) . . . . ? Cl1 Ti1 N2 C10 79.1(2) . . . . ? Cl2 Ti1 N2 C10 -75.4(2) . . . . ? O1 Ti1 N2 C12 -177.7(2) . . . . ? N1 Ti1 N2 C12 -179.8(3) . . . . ? C26 Ti1 N2 C12 -20.9(3) . . . . ? C25 Ti1 N2 C12 -27.9(3) . . . . ? C27 Ti1 N2 C12 13.7(3) . . . . ? C24 Ti1 N2 C12 11.8(4) . . . . ? C23 Ti1 N2 C12 32.2(3) . . . . ? Cl1 Ti1 N2 C12 -102.0(2) . . . . ? Cl2 Ti1 N2 C12 103.5(2) . . . . ? C10 N2 C12 C13 -90.1(4) . . . . ? Ti1 N2 C12 C13 91.0(3) . . . . ? C10 N2 C12 C17 88.3(4) . . . . ? Ti1 N2 C12 C17 -90.7(3) . . . . ? C12 N2 C10 C9 -179.6(3) . . . . ? Ti1 N2 C10 C9 -0.5(4) . . . . ? C12 N2 C10 C11 -0.6(5) . . . . ? Ti1 N2 C10 C11 178.4(3) . . . . ? C17 C12 C13 C14 3.2(5) . . . . ? N2 C12 C13 C14 -178.5(3) . . . . ? C17 C12 C13 C18 -173.7(3) . . . . ? N2 C12 C13 C18 4.6(5) . . . . ? N1 C6 C5 C4 179.6(3) . . . . ? C1 C6 C5 C4 -1.5(5) . . . . ? N1 C6 C5 C7 0.4(5) . . . . ? C1 C6 C5 C7 179.3(3) . . . . ? C13 C12 C17 C16 -3.7(5) . . . . ? N2 C12 C17 C16 178.0(3) . . . . ? C13 C12 C17 C20 172.3(3) . . . . ? N2 C12 C17 C20 -6.0(5) . . . . ? Ti1 O1 C1 C2 -177.9(3) . . . . ? Ti1 O1 C1 C6 0.7(4) . . . . ? C3 C2 C1 O1 178.9(3) . . . . ? C3 C2 C1 C6 0.3(5) . . . . ? N1 C6 C1 O1 1.2(4) . . . . ? C5 C6 C1 O1 -177.8(3) . . . . ? N1 C6 C1 C2 179.9(3) . . . . ? C5 C6 C1 C2 0.9(5) . . . . ? C6 C5 C7 C8 -0.7(6) . . . . ? C4 C5 C7 C8 -179.8(4) . . . . ? C14 C15 C16 C17 0.0(6) . . . . ? C22 C15 C16 C17 179.1(4) . . . . ? C12 C17 C16 C15 2.1(5) . . . . ? C20 C17 C16 C15 -174.0(4) . . . . ? O1 Ti1 C24 C23 -136.3(4) . . . . ? N1 Ti1 C24 C23 -118.9(4) . . . . ? C26 Ti1 C24 C23 79.0(4) . . . . ? C25 Ti1 C24 C23 118.3(5) . . . . ? C27 Ti1 C24 C23 35.9(3) . . . . ? N2 Ti1 C24 C23 38.3(5) . . . . ? Cl1 Ti1 C24 C23 141.4(3) . . . . ? Cl2 Ti1 C24 C23 -48.9(3) . . . . ? O1 Ti1 C24 C25 105.4(3) . . . . ? N1 Ti1 C24 C25 122.8(4) . . . . ? C26 Ti1 C24 C25 -39.2(3) . . . . ? C27 Ti1 C24 C25 -82.3(4) . . . . ? N2 Ti1 C24 C25 -80.0(4) . . . . ? C23 Ti1 C24 C25 -118.3(5) . . . . ? Cl1 Ti1 C24 C25 23.1(3) . . . . ? Cl2 Ti1 C24 C25 -167.2(3) . . . . ? C5 C7 C8 C9 1.0(6) . . . . ? C16 C15 C14 C13 -0.5(5) . . . . ? C22 C15 C14 C13 -179.7(4) . . . . ? C12 C13 C14 C15 -1.1(5) . . . . ? C18 C13 C14 C15 176.0(3) . . . . ? C12 C13 C18 C19 -128.3(12) . . . . ? C14 C13 C18 C19 54.8(12) . . . . ? C12 C13 C18 C19' -168.4(17) . . . . ? C14 C13 C18 C19' 14.7(17) . . . . ? C1 C2 C3 C4 -0.9(6) . . . . ? C2 C3 C4 C5 0.3(6) . . . . ? C6 C5 C4 C3 0.9(5) . . . . ? C7 C5 C4 C3 179.9(4) . . . . ? C6 N1 C9 C8 0.8(5) . . . . ? Ti1 N1 C9 C8 -176.1(3) . . . . ? C6 N1 C9 C10 179.4(3) . . . . ? Ti1 N1 C9 C10 2.5(4) . . . . ? C7 C8 C9 N1 -1.1(6) . . . . ? C7 C8 C9 C10 -179.5(4) . . . . ? N2 C10 C9 N1 -1.0(5) . . . . ? C11 C10 C9 N1 179.9(3) . . . . ? N2 C10 C9 C8 177.4(4) . . . . ? C11 C10 C9 C8 -1.6(6) . . . . ? O1 Ti1 C26 C25 -4.5(4) . . . . ? N1 Ti1 C26 C25 -126.1(4) . . . . ? C27 Ti1 C26 C25 111.3(4) . . . . ? N2 Ti1 C26 C25 -169.9(3) . . . . ? C24 Ti1 C26 C25 36.0(3) . . . . ? C23 Ti1 C26 C25 74.6(3) . . . . ? Cl1 Ti1 C26 C25 -87.4(3) . . . . ? Cl2 Ti1 C26 C25 107.6(4) . . . . ? O1 Ti1 C26 C27 -115.7(3) . . . . ? N1 Ti1 C26 C27 122.6(3) . . . . ? C25 Ti1 C26 C27 -111.3(4) . . . . ? N2 Ti1 C26 C27 78.8(3) . . . . ? C24 Ti1 C26 C27 -75.3(3) . . . . ? C23 Ti1 C26 C27 -36.7(3) . . . . ? Cl1 Ti1 C26 C27 161.4(3) . . . . ? Cl2 Ti1 C26 C27 -3.7(4) . . . . ? C25 C26 C27 C23 0.3(5) . . . . ? Ti1 C26 C27 C23 67.5(3) . . . . ? C25 C26 C27 Ti1 -67.2(3) . . . . ? O1 Ti1 C27 C23 -25.2(4) . . . . ? N1 Ti1 C27 C23 120.9(3) . . . . ? C26 Ti1 C27 C23 -114.1(4) . . . . ? C25 Ti1 C27 C23 -74.1(3) . . . . ? N2 Ti1 C27 C23 146.8(3) . . . . ? C24 Ti1 C27 C23 -34.8(3) . . . . ? Cl1 Ti1 C27 C23 -134.4(3) . . . . ? Cl2 Ti1 C27 C23 62.8(3) . . . . ? O1 Ti1 C27 C26 88.9(4) . . . . ? N1 Ti1 C27 C26 -125.0(4) . . . . ? C25 Ti1 C27 C26 39.9(3) . . . . ? N2 Ti1 C27 C26 -99.1(3) . . . . ? C24 Ti1 C27 C26 79.3(3) . . . . ? C23 Ti1 C27 C26 114.1(4) . . . . ? Cl1 Ti1 C27 C26 -20.3(3) . . . . ? Cl2 Ti1 C27 C26 176.9(3) . . . . ? C23 C24 C25 C26 0.4(5) . . . . ? Ti1 C24 C25 C26 65.0(3) . . . . ? C23 C24 C25 Ti1 -64.7(3) . . . . ? C27 C26 C25 C24 -0.4(5) . . . . ? Ti1 C26 C25 C24 -67.9(3) . . . . ? C27 C26 C25 Ti1 67.5(3) . . . . ? O1 Ti1 C25 C24 -69.2(3) . . . . ? N1 Ti1 C25 C24 -121.0(4) . . . . ? C26 Ti1 C25 C24 114.7(4) . . . . ? C27 Ti1 C25 C24 74.8(3) . . . . ? N2 Ti1 C25 C24 127.0(3) . . . . ? C23 Ti1 C25 C24 34.9(3) . . . . ? Cl1 Ti1 C25 C24 -158.3(3) . . . . ? Cl2 Ti1 C25 C24 16.0(4) . . . . ? O1 Ti1 C25 C26 176.1(4) . . . . ? N1 Ti1 C25 C26 124.3(4) . . . . ? C27 Ti1 C25 C26 -39.9(3) . . . . ? N2 Ti1 C25 C26 12.3(4) . . . . ? C24 Ti1 C25 C26 -114.7(4) . . . . ? C23 Ti1 C25 C26 -79.8(4) . . . . ? Cl1 Ti1 C25 C26 87.0(3) . . . . ? Cl2 Ti1 C25 C26 -98.7(4) . . . . ? C25 C24 C23 C27 -0.2(5) . . . . ? Ti1 C24 C23 C27 -63.2(3) . . . . ? C25 C24 C23 Ti1 63.1(3) . . . . ? C26 C27 C23 C24 -0.1(5) . . . . ? Ti1 C27 C23 C24 64.6(3) . . . . ? C26 C27 C23 Ti1 -64.7(3) . . . . ? O1 Ti1 C23 C24 42.4(4) . . . . ? N1 Ti1 C23 C24 121.5(4) . . . . ? C26 Ti1 C23 C24 -78.7(4) . . . . ? C25 Ti1 C23 C24 -35.5(3) . . . . ? C27 Ti1 C23 C24 -118.1(5) . . . . ? N2 Ti1 C23 C24 -153.7(3) . . . . ? Cl1 Ti1 C23 C24 -53.6(4) . . . . ? Cl2 Ti1 C23 C24 129.0(4) . . . . ? O1 Ti1 C23 C27 160.5(3) . . . . ? N1 Ti1 C23 C27 -120.4(3) . . . . ? C26 Ti1 C23 C27 39.4(3) . . . . ? C25 Ti1 C23 C27 82.6(4) . . . . ? N2 Ti1 C23 C27 -35.6(4) . . . . ? C24 Ti1 C23 C27 118.1(5) . . . . ? Cl1 Ti1 C23 C27 64.4(4) . . . . ? Cl2 Ti1 C23 C27 -112.9(3) . . . . ? C12 C17 C20 C21 142.8(4) . . . . ? C16 C17 C20 C21 -41.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.458 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.108 #==END