# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Sheng-Di Bai' _publ_contact_author_email sdbai@sxu.edu.cn loop_ _publ_author_name 'Sheng-Di Bai' 'Fei Guan' 'Min Hu' 'Shi-Fang Yuan' 'Jian-Ping Guo' ; Wen-Hua Sun ; 'Dian-Sheng Liu' data_s119p _database_code_depnum_ccdc_archive 'CCDC 804643' #TrackingRef '- 804643-804644.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H34 Cl2 N4 Si Ti' _chemical_formula_weight 525.44 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' Si Si 0.0817 0.0704 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 22.585(5) _cell_length_b 26.749(6) _cell_length_c 9.093(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5493(2) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 2071 _cell_measurement_theta_min 2.361 _cell_measurement_theta_max 24.974 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8480 _exptl_absorpt_correction_T_max 0.8948 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 Smart area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.73 _diffrn_reflns_number 5712 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.04 _reflns_number_total 2422 _reflns_number_gt 2145 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0573P)^2^+6.3052P] 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 0.07(5) _refine_ls_number_reflns 2422 _refine_ls_number_parameters 146 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1157 _refine_ls_wR_factor_gt 0.1120 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.090 _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 0.0000 0.5000 0.16690(8) 0.0338(3) Uani 1 2 d S . . Si1 Si 0.0000 0.5000 0.48307(16) 0.0473(4) Uani 1 2 d SU . . Cl1 Cl 0.09237(5) 0.50149(4) 0.06758(15) 0.0580(3) Uani 1 1 d . . . N1 N -0.00121(14) 0.58354(11) 0.1416(3) 0.0385(8) Uani 1 1 d . . . N2 N -0.0098(2) 0.54186(12) 0.3450(4) 0.0675(11) Uani 1 1 d U . . C1 C 0.00129(16) 0.62337(14) 0.0296(4) 0.0389(9) Uani 1 1 d . . . C2 C -0.0067(2) 0.59684(18) -0.1173(5) 0.0627(13) Uani 1 1 d . . . H2A H -0.0407 0.5747 -0.1118 0.094 Uiso 1 1 calc R . . H2B H 0.0285 0.5775 -0.1394 0.094 Uiso 1 1 calc R . . H2C H -0.0131 0.6214 -0.1941 0.094 Uiso 1 1 calc R . . C3 C -0.04870(19) 0.66098(16) 0.0510(5) 0.0560(12) Uani 1 1 d . . . H3A H -0.0469 0.6745 0.1498 0.084 Uiso 1 1 calc R . . H3B H -0.0865 0.6444 0.0366 0.084 Uiso 1 1 calc R . . H3C H -0.0446 0.6879 -0.0198 0.084 Uiso 1 1 calc R . . C4 C 0.06096(19) 0.65002(16) 0.0338(5) 0.0575(12) Uani 1 1 d . . . H4A H 0.0636 0.6700 0.1226 0.086 Uiso 1 1 calc R . . H4B H 0.0647 0.6715 -0.0516 0.086 Uiso 1 1 calc R . . H4C H 0.0926 0.6255 0.0333 0.086 Uiso 1 1 calc R . . C5 C -0.00557(18) 0.58785(15) 0.2839(4) 0.0426(9) Uani 1 1 d . . . C6 C -0.00822(17) 0.63183(13) 0.3835(4) 0.0374(9) Uani 1 1 d . . . C7 C -0.0608(2) 0.64287(16) 0.4515(5) 0.0516(11) Uani 1 1 d . . . H7A H -0.0948 0.6243 0.4280 0.062 Uiso 1 1 calc R . . C8 C -0.0647(2) 0.68050(16) 0.5531(5) 0.0602(12) Uani 1 1 d . . . H8A H -0.1012 0.6879 0.5975 0.072 Uiso 1 1 calc R . . C9 C -0.0151(2) 0.70754(15) 0.5901(5) 0.0570(12) Uani 1 1 d . . . H9A H -0.0176 0.7336 0.6593 0.068 Uiso 1 1 calc R . . C10 C 0.0380(2) 0.69631(16) 0.5254(5) 0.0629(13) Uani 1 1 d . . . H10A H 0.0722 0.7142 0.5518 0.075 Uiso 1 1 calc R . . C11 C 0.04134(19) 0.65891(15) 0.4218(5) 0.0513(10) Uani 1 1 d . . . H11A H 0.0778 0.6518 0.3767 0.062 Uiso 1 1 calc R . . C12 C 0.0671(3) 0.5092(2) 0.5962(6) 0.0883(19) Uani 1 1 d . . . H12A H 0.0561 0.5109 0.6991 0.133 Uiso 1 1 calc R . . H12B H 0.0864 0.5400 0.5675 0.133 Uiso 1 1 calc R . . H12C H 0.0940 0.4813 0.5812 0.133 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 0.0522(6) 0.0251(5) 0.0242(5) 0.000 0.000 -0.0035(5) Si1 0.0830(13) 0.0337(9) 0.0253(8) 0.000 0.000 -0.0108(8) Cl1 0.0429(5) 0.0529(6) 0.0783(8) 0.0077(6) 0.0009(6) -0.0009(5) N1 0.0558(19) 0.0247(14) 0.035(2) -0.0004(13) -0.0002(15) -0.0011(14) N2 0.147(3) 0.0239(15) 0.031(2) -0.0045(15) 0.012(2) -0.0041(19) C1 0.048(2) 0.031(2) 0.037(2) 0.0091(15) -0.0003(18) -0.0010(16) C2 0.103(4) 0.050(3) 0.036(2) 0.008(2) -0.001(2) 0.011(2) C3 0.058(3) 0.049(3) 0.061(3) 0.013(2) -0.006(2) 0.010(2) C4 0.053(2) 0.060(3) 0.060(3) 0.013(2) 0.006(2) -0.008(2) C5 0.057(2) 0.037(2) 0.034(2) 0.0017(16) -0.0020(19) -0.0001(18) C6 0.054(2) 0.0230(18) 0.0356(18) 0.0001(15) 0.0052(17) 0.0027(16) C7 0.048(2) 0.056(3) 0.051(2) -0.007(2) -0.002(2) 0.003(2) C8 0.067(3) 0.060(3) 0.053(3) -0.003(2) 0.014(2) 0.025(2) C9 0.095(4) 0.030(2) 0.046(2) -0.008(2) 0.012(3) 0.004(2) C10 0.081(3) 0.046(3) 0.061(3) -0.014(2) 0.012(3) -0.023(2) C11 0.056(3) 0.042(2) 0.055(2) -0.007(2) 0.017(2) -0.006(2) C12 0.077(4) 0.135(5) 0.053(3) -0.019(3) 0.007(3) -0.025(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 Ti1 N2 1.981(3) . ? Ti1 N2 1.981(3) 2_565 ? Ti1 N1 2.247(3) 2_565 ? Ti1 N1 2.247(3) . ? Ti1 Cl1 2.2735(12) 2_565 ? Ti1 Cl1 2.2735(12) . ? Ti1 C5 2.582(4) . ? Ti1 C5 2.582(4) 2_565 ? Ti1 Si1 2.8748(17) . ? Si1 N2 1.697(4) 2_565 ? Si1 N2 1.697(4) . ? Si1 C12 1.847(6) . ? Si1 C12 1.847(6) 2_565 ? N1 C5 1.303(5) . ? N1 C1 1.475(5) . ? N2 C5 1.353(5) . ? C1 C2 1.523(6) . ? C1 C3 1.525(5) . ? C1 C4 1.525(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 C6 1.486(5) . ? C6 C7 1.372(5) . ? C6 C11 1.378(6) . ? C7 C8 1.369(6) . ? C7 H7A 0.9400 . ? C8 C9 1.375(6) . ? C8 H8A 0.9400 . ? C9 C10 1.368(7) . ? C9 H9A 0.9400 . ? C10 C11 1.376(6) . ? C10 H10A 0.9400 . ? C11 H11A 0.9400 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 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 N2 Ti1 N2 70.3(2) . 2_565 ? N2 Ti1 N1 130.34(12) . 2_565 ? N2 Ti1 N1 61.33(12) 2_565 2_565 ? N2 Ti1 N1 61.33(12) . . ? N2 Ti1 N1 130.34(12) 2_565 . ? N1 Ti1 N1 168.24(16) 2_565 . ? N2 Ti1 Cl1 103.45(14) . 2_565 ? N2 Ti1 Cl1 114.64(13) 2_565 2_565 ? N1 Ti1 Cl1 87.31(8) 2_565 2_565 ? N1 Ti1 Cl1 88.03(8) . 2_565 ? N2 Ti1 Cl1 114.64(13) . . ? N2 Ti1 Cl1 103.45(14) 2_565 . ? N1 Ti1 Cl1 88.03(8) 2_565 . ? N1 Ti1 Cl1 87.31(8) . . ? Cl1 Ti1 Cl1 133.19(8) 2_565 . ? N2 Ti1 C5 31.09(13) . . ? N2 Ti1 C5 100.55(13) 2_565 . ? N1 Ti1 C5 161.42(12) 2_565 . ? N1 Ti1 C5 30.29(12) . . ? Cl1 Ti1 C5 97.75(9) 2_565 . ? Cl1 Ti1 C5 101.09(9) . . ? N2 Ti1 C5 100.55(13) . 2_565 ? N2 Ti1 C5 31.09(13) 2_565 2_565 ? N1 Ti1 C5 30.29(12) 2_565 2_565 ? N1 Ti1 C5 161.42(12) . 2_565 ? Cl1 Ti1 C5 101.09(9) 2_565 2_565 ? Cl1 Ti1 C5 97.75(9) . 2_565 ? C5 Ti1 C5 131.36(18) . 2_565 ? N2 Ti1 Si1 35.17(10) . . ? N2 Ti1 Si1 35.17(10) 2_565 . ? N1 Ti1 Si1 95.88(8) 2_565 . ? N1 Ti1 Si1 95.88(8) . . ? Cl1 Ti1 Si1 113.40(4) 2_565 . ? Cl1 Ti1 Si1 113.40(4) . . ? C5 Ti1 Si1 65.68(9) . . ? C5 Ti1 Si1 65.68(9) 2_565 . ? N2 Si1 N2 84.5(2) 2_565 . ? N2 Si1 C12 113.1(2) 2_565 . ? N2 Si1 C12 115.5(2) . . ? N2 Si1 C12 115.5(2) 2_565 2_565 ? N2 Si1 C12 113.1(2) . 2_565 ? C12 Si1 C12 112.3(4) . 2_565 ? N2 Si1 Ti1 42.27(12) 2_565 . ? N2 Si1 Ti1 42.27(12) . . ? C12 Si1 Ti1 123.83(19) . . ? C12 Si1 Ti1 123.83(19) 2_565 . ? C5 N1 C1 128.7(3) . . ? C5 N1 Ti1 89.3(2) . . ? C1 N1 Ti1 142.1(2) . . ? C5 N2 Si1 153.5(3) . . ? C5 N2 Ti1 99.8(3) . . ? Si1 N2 Ti1 102.56(16) . . ? N1 C1 C2 105.3(3) . . ? N1 C1 C3 111.1(3) . . ? C2 C1 C3 109.4(4) . . ? N1 C1 C4 110.7(3) . . ? C2 C1 C4 110.2(4) . . ? C3 C1 C4 110.1(4) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 N2 109.4(3) . . ? N1 C5 C6 132.7(4) . . ? N2 C5 C6 117.8(3) . . ? N1 C5 Ti1 60.4(2) . . ? N2 C5 Ti1 49.1(2) . . ? C6 C5 Ti1 166.8(3) . . ? C7 C6 C11 118.4(4) . . ? C7 C6 C5 118.7(3) . . ? C11 C6 C5 122.5(4) . . ? C8 C7 C6 121.2(4) . . ? C8 C7 H7A 119.4 . . ? C6 C7 H7A 119.4 . . ? C7 C8 C9 120.0(4) . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C10 C9 C8 119.5(4) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? C9 C10 C11 120.1(4) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C10 C11 C6 120.7(4) . . ? C10 C11 H11A 119.6 . . ? C6 C11 H11A 119.6 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 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 N2 Ti1 Si1 N2 180.000(1) . . . 2_565 ? N1 Ti1 Si1 N2 10.4(2) 2_565 . . 2_565 ? N1 Ti1 Si1 N2 -169.6(2) . . . 2_565 ? Cl1 Ti1 Si1 N2 100.0(2) 2_565 . . 2_565 ? Cl1 Ti1 Si1 N2 -80.0(2) . . . 2_565 ? C5 Ti1 Si1 N2 -171.9(2) . . . 2_565 ? C5 Ti1 Si1 N2 8.1(2) 2_565 . . 2_565 ? N2 Ti1 Si1 N2 180.000(1) 2_565 . . . ? N1 Ti1 Si1 N2 -169.6(2) 2_565 . . . ? N1 Ti1 Si1 N2 10.4(2) . . . . ? Cl1 Ti1 Si1 N2 -80.0(2) 2_565 . . . ? Cl1 Ti1 Si1 N2 100.0(2) . . . . ? C5 Ti1 Si1 N2 8.1(2) . . . . ? C5 Ti1 Si1 N2 -171.9(2) 2_565 . . . ? N2 Ti1 Si1 C12 -91.9(3) . . . . ? N2 Ti1 Si1 C12 88.1(3) 2_565 . . . ? N1 Ti1 Si1 C12 98.5(3) 2_565 . . . ? N1 Ti1 Si1 C12 -81.5(3) . . . . ? Cl1 Ti1 Si1 C12 -171.9(2) 2_565 . . . ? Cl1 Ti1 Si1 C12 8.1(2) . . . . ? C5 Ti1 Si1 C12 -83.9(3) . . . . ? C5 Ti1 Si1 C12 96.1(3) 2_565 . . . ? N2 Ti1 Si1 C12 88.1(3) . . . 2_565 ? N2 Ti1 Si1 C12 -91.9(3) 2_565 . . 2_565 ? N1 Ti1 Si1 C12 -81.5(3) 2_565 . . 2_565 ? N1 Ti1 Si1 C12 98.5(3) . . . 2_565 ? Cl1 Ti1 Si1 C12 8.1(2) 2_565 . . 2_565 ? Cl1 Ti1 Si1 C12 -171.9(2) . . . 2_565 ? C5 Ti1 Si1 C12 96.1(3) . . . 2_565 ? C5 Ti1 Si1 C12 -83.9(3) 2_565 . . 2_565 ? N2 Ti1 N1 C5 2.6(2) . . . . ? N2 Ti1 N1 C5 -12.1(3) 2_565 . . . ? N1 Ti1 N1 C5 175.7(2) 2_565 . . . ? Cl1 Ti1 N1 C5 109.1(2) 2_565 . . . ? Cl1 Ti1 N1 C5 -117.5(2) . . . . ? C5 Ti1 N1 C5 -11.0(6) 2_565 . . . ? Si1 Ti1 N1 C5 -4.3(2) . . . . ? N2 Ti1 N1 C1 -177.6(4) . . . . ? N2 Ti1 N1 C1 167.7(4) 2_565 . . . ? N1 Ti1 N1 C1 -4.4(4) 2_565 . . . ? Cl1 Ti1 N1 C1 -71.1(4) 2_565 . . . ? Cl1 Ti1 N1 C1 62.3(4) . . . . ? C5 Ti1 N1 C1 179.9(5) . . . . ? C5 Ti1 N1 C1 168.8(4) 2_565 . . . ? Si1 Ti1 N1 C1 175.6(4) . . . . ? N2 Si1 N2 C5 -146.8(9) 2_565 . . . ? C12 Si1 N2 C5 -33.8(8) . . . . ? C12 Si1 N2 C5 97.7(8) 2_565 . . . ? Ti1 Si1 N2 C5 -146.8(9) . . . . ? N2 Si1 N2 Ti1 0.0 2_565 . . . ? C12 Si1 N2 Ti1 113.1(2) . . . . ? C12 Si1 N2 Ti1 -115.5(2) 2_565 . . . ? N2 Ti1 N2 C5 165.6(4) 2_565 . . . ? N1 Ti1 N2 C5 179.3(2) 2_565 . . . ? N1 Ti1 N2 C5 -2.5(2) . . . . ? Cl1 Ti1 N2 C5 -82.7(3) 2_565 . . . ? Cl1 Ti1 N2 C5 69.5(3) . . . . ? C5 Ti1 N2 C5 173.1(2) 2_565 . . . ? Si1 Ti1 N2 C5 165.6(4) . . . . ? N2 Ti1 N2 Si1 0.0 2_565 . . . ? N1 Ti1 N2 Si1 13.7(3) 2_565 . . . ? N1 Ti1 N2 Si1 -168.1(3) . . . . ? Cl1 Ti1 N2 Si1 111.70(18) 2_565 . . . ? Cl1 Ti1 N2 Si1 -96.19(17) . . . . ? C5 Ti1 N2 Si1 -165.6(4) . . . . ? C5 Ti1 N2 Si1 7.5(2) 2_565 . . . ? C5 N1 C1 C2 -168.5(4) . . . . ? Ti1 N1 C1 C2 11.7(5) . . . . ? C5 N1 C1 C3 -50.2(5) . . . . ? Ti1 N1 C1 C3 129.9(4) . . . . ? C5 N1 C1 C4 72.4(5) . . . . ? Ti1 N1 C1 C4 -107.4(4) . . . . ? C1 N1 C5 N2 176.6(4) . . . . ? Ti1 N1 C5 N2 -3.5(3) . . . . ? C1 N1 C5 C6 -1.5(7) . . . . ? Ti1 N1 C5 C6 178.4(4) . . . . ? C1 N1 C5 Ti1 -179.9(4) . . . . ? Si1 N2 C5 N1 151.2(6) . . . . ? Ti1 N2 C5 N1 4.0(4) . . . . ? Si1 N2 C5 C6 -30.3(9) . . . . ? Ti1 N2 C5 C6 -177.5(3) . . . . ? Si1 N2 C5 Ti1 147.2(9) . . . . ? N2 Ti1 C5 N1 -175.6(4) . . . . ? N2 Ti1 C5 N1 170.6(3) 2_565 . . . ? N1 Ti1 C5 N1 -177.27(16) 2_565 . . . ? Cl1 Ti1 C5 N1 -72.4(2) 2_565 . . . ? Cl1 Ti1 C5 N1 64.5(2) . . . . ? C5 Ti1 C5 N1 175.3(3) 2_565 . . . ? Si1 Ti1 C5 N1 175.3(3) . . . . ? N2 Ti1 C5 N2 -13.7(4) 2_565 . . . ? N1 Ti1 C5 N2 -1.6(5) 2_565 . . . ? N1 Ti1 C5 N2 175.6(4) . . . . ? Cl1 Ti1 C5 N2 103.2(3) 2_565 . . . ? Cl1 Ti1 C5 N2 -119.8(3) . . . . ? C5 Ti1 C5 N2 -9.0(3) 2_565 . . . ? Si1 Ti1 C5 N2 -9.0(3) . . . . ? N2 Ti1 C5 C6 9.5(11) . . . . ? N2 Ti1 C5 C6 -4.2(12) 2_565 . . . ? N1 Ti1 C5 C6 7.9(15) 2_565 . . . ? N1 Ti1 C5 C6 -174.8(14) . . . . ? Cl1 Ti1 C5 C6 112.7(12) 2_565 . . . ? Cl1 Ti1 C5 C6 -110.3(12) . . . . ? C5 Ti1 C5 C6 0.5(12) 2_565 . . . ? Si1 Ti1 C5 C6 0.5(12) . . . . ? N1 C5 C6 C7 108.7(5) . . . . ? N2 C5 C6 C7 -69.3(5) . . . . ? Ti1 C5 C6 C7 -77.4(13) . . . . ? N1 C5 C6 C11 -78.0(6) . . . . ? N2 C5 C6 C11 104.0(5) . . . . ? Ti1 C5 C6 C11 95.8(12) . . . . ? C11 C6 C7 C8 1.3(6) . . . . ? C5 C6 C7 C8 174.8(4) . . . . ? C6 C7 C8 C9 -0.9(7) . . . . ? C7 C8 C9 C10 -0.4(7) . . . . ? C8 C9 C10 C11 1.4(7) . . . . ? C9 C10 C11 C6 -1.0(7) . . . . ? C7 C6 C11 C10 -0.3(7) . . . . ? C5 C6 C11 C10 -173.6(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.456 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.066 # End data_s466p _database_code_depnum_ccdc_archive 'CCDC 804644' #TrackingRef '- 804643-804644.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H40 N4 Si Ti' _chemical_formula_weight 484.61 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' Si Si 0.0817 0.0704 '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 Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 22.957(15) _cell_length_b 26.990(18) _cell_length_c 9.165(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5679(6) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1594 _cell_measurement_theta_min 2.330 _cell_measurement_theta_max 22.126 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 0.362 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8991 _exptl_absorpt_correction_T_max 0.9311 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 Smart area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 11.44 _diffrn_reflns_number 5702 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0847 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2300 _reflns_number_gt 1815 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0707P)^2^+10.2588P] 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 0.05(6) _refine_ls_number_reflns 2300 _refine_ls_number_parameters 146 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0866 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.1818 _refine_ls_wR_factor_gt 0.1674 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.081 _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 0.7500 0.2500 0.10186(11) 0.0517(4) Uani 1 2 d S . . N1 N 0.74847(19) 0.16639(14) 0.0793(5) 0.0553(11) Uani 1 1 d . . . N2 N 0.7371(2) 0.20796(15) 0.2823(6) 0.0801(9) Uani 1 1 d U . . Si1 Si 0.7500 0.2500 0.4143(3) 0.0779(8) Uani 1 2 d SU . . C1 C 0.7520(2) 0.1252(2) -0.0246(8) 0.0606(13) Uani 1 1 d . . . C2 C 0.7456(4) 0.1490(4) -0.1739(9) 0.111(3) Uani 1 1 d . . . H2A H 0.7759 0.1731 -0.1875 0.167 Uiso 1 1 calc R . . H2B H 0.7083 0.1650 -0.1806 0.167 Uiso 1 1 calc R . . H2C H 0.7486 0.1240 -0.2480 0.167 Uiso 1 1 calc R . . C3 C 0.8100(3) 0.0996(3) -0.0170(11) 0.106(3) Uani 1 1 d . . . H3A H 0.8406 0.1236 -0.0287 0.158 Uiso 1 1 calc R . . H3B H 0.8125 0.0754 -0.0933 0.158 Uiso 1 1 calc R . . H3C H 0.8140 0.0836 0.0760 0.158 Uiso 1 1 calc R . . C4 C 0.7034(3) 0.0883(2) -0.0079(10) 0.091(2) Uani 1 1 d . . . H4A H 0.7062 0.0725 0.0857 0.137 Uiso 1 1 calc R . . H4B H 0.7063 0.0637 -0.0834 0.137 Uiso 1 1 calc R . . H4C H 0.6666 0.1050 -0.0155 0.137 Uiso 1 1 calc R . . C5 C 0.7444(3) 0.16331(17) 0.2201(7) 0.0640(15) Uani 1 1 d . . . C6 C 0.7450(2) 0.11975(19) 0.3223(6) 0.0556(14) Uani 1 1 d . . . C7 C 0.7959(3) 0.0983(2) 0.3657(9) 0.087(2) Uani 1 1 d . . . H7A H 0.8310 0.1085 0.3250 0.105 Uiso 1 1 calc R . . C8 C 0.7955(4) 0.0608(3) 0.4715(10) 0.105(2) Uani 1 1 d . . . H8A H 0.8302 0.0470 0.5043 0.126 Uiso 1 1 calc R . . C9 C 0.7446(4) 0.0450(2) 0.5250(10) 0.104(3) Uani 1 1 d . . . H9A H 0.7442 0.0190 0.5916 0.125 Uiso 1 1 calc R . . C10 C 0.6942(4) 0.0658(3) 0.4844(10) 0.105(3) Uani 1 1 d . . . H10A H 0.6593 0.0549 0.5248 0.126 Uiso 1 1 calc R . . C11 C 0.6941(3) 0.1037(2) 0.3823(8) 0.085(2) Uani 1 1 d . . . H11A H 0.6591 0.1182 0.3546 0.102 Uiso 1 1 calc R . . C12 C 0.8153(4) 0.2396(3) 0.5294(11) 0.134(3) Uani 1 1 d . . . H12A H 0.8046 0.2415 0.6304 0.202 Uiso 1 1 calc R . . H12B H 0.8440 0.2645 0.5082 0.202 Uiso 1 1 calc R . . H12C H 0.8312 0.2074 0.5089 0.202 Uiso 1 1 calc R . . C13 C 0.8323(2) 0.24782(17) -0.0039(8) 0.0659(15) Uani 1 1 d . . . H13A H 0.8267 0.2480 -0.1077 0.099 Uiso 1 1 calc R . . H13B H 0.8526 0.2182 0.0241 0.099 Uiso 1 1 calc R . . H13C H 0.8547 0.2763 0.0240 0.099 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0823(8) 0.0393(6) 0.0335(7) 0.000 0.000 0.0048(7) N1 0.089(3) 0.0398(18) 0.037(3) -0.0025(18) 0.002(2) 0.003(2) N2 0.155(2) 0.0487(14) 0.0363(15) 0.0010(9) 0.0023(10) 0.0113(14) Si1 0.152(2) 0.0473(11) 0.0345(12) 0.000 0.000 0.0133(12) C1 0.073(3) 0.053(3) 0.056(3) -0.018(3) -0.003(3) 0.001(2) C2 0.197(9) 0.087(5) 0.050(4) -0.020(4) 0.000(5) -0.006(5) C3 0.094(4) 0.109(5) 0.114(7) -0.046(5) 0.000(5) 0.023(4) C4 0.100(4) 0.072(4) 0.102(6) -0.032(5) -0.005(4) -0.014(3) C5 0.095(4) 0.038(2) 0.059(5) -0.002(2) -0.001(3) 0.007(2) C6 0.077(3) 0.040(3) 0.050(3) -0.003(2) 0.006(3) -0.002(2) C7 0.095(4) 0.073(4) 0.094(5) 0.026(4) 0.027(4) 0.024(3) C8 0.135(6) 0.086(5) 0.094(6) 0.016(4) 0.002(5) 0.047(5) C9 0.189(9) 0.050(4) 0.072(5) 0.011(3) 0.032(7) -0.007(4) C10 0.125(6) 0.102(5) 0.087(6) 0.012(5) 0.026(5) -0.051(5) C11 0.081(4) 0.092(5) 0.081(5) 0.022(4) 0.001(4) -0.014(3) C12 0.146(7) 0.176(8) 0.081(6) 0.038(7) 0.010(6) 0.028(6) C13 0.064(3) 0.062(3) 0.072(4) 0.003(3) 0.001(3) 0.000(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 N2 2.027(5) 14_655 ? Ti1 N2 2.027(5) . ? Ti1 C13 2.124(6) 14_655 ? Ti1 C13 2.124(6) . ? Ti1 N1 2.266(4) 14_655 ? Ti1 N1 2.266(4) . ? Ti1 C5 2.582(5) 14_655 ? Ti1 C5 2.582(5) . ? Ti1 Si1 2.864(3) . ? N1 C5 1.296(8) . ? N1 C1 1.465(7) . ? N2 C5 1.344(7) . ? N2 Si1 1.685(5) . ? Si1 N2 1.685(5) 14_655 ? Si1 C12 1.854(10) 14_655 ? Si1 C12 1.854(10) . ? C1 C3 1.501(8) . ? C1 C4 1.505(8) . ? C1 C2 1.519(11) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.503(8) . ? C6 C7 1.364(8) . ? C6 C11 1.364(8) . ? C7 C8 1.402(10) . ? C7 H7A 0.9300 . ? C8 C9 1.336(10) . ? C8 H8A 0.9300 . ? C9 C10 1.340(10) . ? C9 H9A 0.9300 . ? C10 C11 1.386(10) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? 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 N2 Ti1 N2 70.7(3) 14_655 . ? N2 Ti1 C13 119.2(2) 14_655 14_655 ? N2 Ti1 C13 104.9(2) . 14_655 ? N2 Ti1 C13 104.9(2) 14_655 . ? N2 Ti1 C13 119.2(2) . . ? C13 Ti1 C13 125.7(4) 14_655 . ? N2 Ti1 N1 60.97(17) 14_655 14_655 ? N2 Ti1 N1 129.33(19) . 14_655 ? C13 Ti1 N1 86.83(17) 14_655 14_655 ? C13 Ti1 N1 88.41(17) . 14_655 ? N2 Ti1 N1 129.33(19) 14_655 . ? N2 Ti1 N1 60.97(17) . . ? C13 Ti1 N1 88.41(17) 14_655 . ? C13 Ti1 N1 86.83(17) . . ? N1 Ti1 N1 169.6(3) 14_655 . ? N2 Ti1 C5 31.0(2) 14_655 14_655 ? N2 Ti1 C5 99.92(19) . 14_655 ? C13 Ti1 C5 102.18(19) 14_655 14_655 ? C13 Ti1 C5 99.92(19) . 14_655 ? N1 Ti1 C5 30.12(19) 14_655 14_655 ? N1 Ti1 C5 160.29(19) . 14_655 ? N2 Ti1 C5 99.92(19) 14_655 . ? N2 Ti1 C5 31.0(2) . . ? C13 Ti1 C5 99.92(19) 14_655 . ? C13 Ti1 C5 102.18(19) . . ? N1 Ti1 C5 160.29(19) 14_655 . ? N1 Ti1 C5 30.12(19) . . ? C5 Ti1 C5 130.4(3) 14_655 . ? N2 Ti1 Si1 35.35(14) 14_655 . ? N2 Ti1 Si1 35.35(14) . . ? C13 Ti1 Si1 117.16(19) 14_655 . ? C13 Ti1 Si1 117.16(19) . . ? N1 Ti1 Si1 95.22(13) 14_655 . ? N1 Ti1 Si1 95.22(13) . . ? C5 Ti1 Si1 65.18(14) 14_655 . ? C5 Ti1 Si1 65.18(14) . . ? C5 N1 C1 127.0(4) . . ? C5 N1 Ti1 88.5(3) . . ? C1 N1 Ti1 144.4(4) . . ? C5 N2 Si1 152.4(5) . . ? C5 N2 Ti1 97.9(4) . . ? Si1 N2 Ti1 100.5(2) . . ? N2 Si1 N2 88.2(4) 14_655 . ? N2 Si1 C12 116.7(4) 14_655 14_655 ? N2 Si1 C12 111.6(3) . 14_655 ? N2 Si1 C12 111.6(3) 14_655 . ? N2 Si1 C12 116.7(4) . . ? C12 Si1 C12 110.7(6) 14_655 . ? N2 Si1 Ti1 44.11(18) 14_655 . ? N2 Si1 Ti1 44.11(18) . . ? C12 Si1 Ti1 124.7(3) 14_655 . ? C12 Si1 Ti1 124.7(3) . . ? N1 C1 C3 111.6(5) . . ? N1 C1 C4 113.3(5) . . ? C3 C1 C4 110.4(6) . . ? N1 C1 C2 105.1(5) . . ? C3 C1 C2 108.8(6) . . ? C4 C1 C2 107.4(6) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 N2 112.0(5) . . ? N1 C5 C6 132.0(5) . . ? N2 C5 C6 116.0(6) . . ? N1 C5 Ti1 61.3(3) . . ? N2 C5 Ti1 51.1(3) . . ? C6 C5 Ti1 165.9(4) . . ? C7 C6 C11 118.9(6) . . ? C7 C6 C5 121.5(5) . . ? C11 C6 C5 119.5(5) . . ? C6 C7 C8 120.1(6) . . ? C6 C7 H7A 119.9 . . ? C8 C7 H7A 119.9 . . ? C9 C8 C7 119.4(7) . . ? C9 C8 H8A 120.3 . . ? C7 C8 H8A 120.3 . . ? C8 C9 C10 121.2(7) . . ? C8 C9 H9A 119.4 . . ? C10 C9 H9A 119.4 . . ? C9 C10 C11 119.9(7) . . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C6 C11 C10 120.4(7) . . ? C6 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Ti1 C13 H13A 109.5 . . ? Ti1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Ti1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 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 N2 Ti1 N1 C5 14.4(4) 14_655 . . . ? N2 Ti1 N1 C5 -5.0(3) . . . . ? C13 Ti1 N1 C5 -113.0(4) 14_655 . . . ? C13 Ti1 N1 C5 121.1(4) . . . . ? N1 Ti1 N1 C5 -175.9(3) 14_655 . . . ? C5 Ti1 N1 C5 10.2(8) 14_655 . . . ? Si1 Ti1 N1 C5 4.1(3) . . . . ? N2 Ti1 N1 C1 -163.1(5) 14_655 . . . ? N2 Ti1 N1 C1 177.6(6) . . . . ? C13 Ti1 N1 C1 69.5(6) 14_655 . . . ? C13 Ti1 N1 C1 -56.4(6) . . . . ? N1 Ti1 N1 C1 6.6(6) 14_655 . . . ? C5 Ti1 N1 C1 -167.3(5) 14_655 . . . ? C5 Ti1 N1 C1 -177.4(8) . . . . ? Si1 Ti1 N1 C1 -173.4(6) . . . . ? N2 Ti1 N2 C5 -159.4(5) 14_655 . . . ? C13 Ti1 N2 C5 84.4(4) 14_655 . . . ? C13 Ti1 N2 C5 -62.7(4) . . . . ? N1 Ti1 N2 C5 -177.3(3) 14_655 . . . ? N1 Ti1 N2 C5 4.8(3) . . . . ? C5 Ti1 N2 C5 -170.0(3) 14_655 . . . ? Si1 Ti1 N2 C5 -159.4(5) . . . . ? N2 Ti1 N2 Si1 0.0 14_655 . . . ? C13 Ti1 N2 Si1 -116.2(2) 14_655 . . . ? C13 Ti1 N2 Si1 96.7(3) . . . . ? N1 Ti1 N2 Si1 -17.9(3) 14_655 . . . ? N1 Ti1 N2 Si1 164.2(3) . . . . ? C5 Ti1 N2 Si1 -10.6(3) 14_655 . . . ? C5 Ti1 N2 Si1 159.4(5) . . . . ? C5 N2 Si1 N2 131.2(11) . . . 14_655 ? Ti1 N2 Si1 N2 0.000(1) . . . 14_655 ? C5 N2 Si1 C12 -110.8(10) . . . 14_655 ? Ti1 N2 Si1 C12 118.1(4) . . . 14_655 ? C5 N2 Si1 C12 17.8(11) . . . . ? Ti1 N2 Si1 C12 -113.3(4) . . . . ? C5 N2 Si1 Ti1 131.2(11) . . . . ? N2 Ti1 Si1 N2 180.000(1) . . . 14_655 ? C13 Ti1 Si1 N2 -102.9(3) 14_655 . . 14_655 ? C13 Ti1 Si1 N2 77.1(3) . . . 14_655 ? N1 Ti1 Si1 N2 -13.8(3) 14_655 . . 14_655 ? N1 Ti1 Si1 N2 166.2(3) . . . 14_655 ? C5 Ti1 Si1 N2 -11.5(3) 14_655 . . 14_655 ? C5 Ti1 Si1 N2 168.5(3) . . . 14_655 ? N2 Ti1 Si1 N2 180.000(1) 14_655 . . . ? C13 Ti1 Si1 N2 77.1(3) 14_655 . . . ? C13 Ti1 Si1 N2 -102.9(3) . . . . ? N1 Ti1 Si1 N2 166.2(3) 14_655 . . . ? N1 Ti1 Si1 N2 -13.8(3) . . . . ? C5 Ti1 Si1 N2 168.5(3) 14_655 . . . ? C5 Ti1 Si1 N2 -11.5(3) . . . . ? N2 Ti1 Si1 C12 94.0(4) 14_655 . . 14_655 ? N2 Ti1 Si1 C12 -86.0(4) . . . 14_655 ? C13 Ti1 Si1 C12 -8.9(4) 14_655 . . 14_655 ? C13 Ti1 Si1 C12 171.1(4) . . . 14_655 ? N1 Ti1 Si1 C12 80.3(4) 14_655 . . 14_655 ? N1 Ti1 Si1 C12 -99.7(4) . . . 14_655 ? C5 Ti1 Si1 C12 82.5(4) 14_655 . . 14_655 ? C5 Ti1 Si1 C12 -97.5(4) . . . 14_655 ? N2 Ti1 Si1 C12 -86.0(4) 14_655 . . . ? N2 Ti1 Si1 C12 94.0(4) . . . . ? C13 Ti1 Si1 C12 171.1(4) 14_655 . . . ? C13 Ti1 Si1 C12 -8.9(4) . . . . ? N1 Ti1 Si1 C12 -99.7(4) 14_655 . . . ? N1 Ti1 Si1 C12 80.3(4) . . . . ? C5 Ti1 Si1 C12 -97.5(4) 14_655 . . . ? C5 Ti1 Si1 C12 82.5(4) . . . . ? C5 N1 C1 C3 -71.7(8) . . . . ? Ti1 N1 C1 C3 105.1(7) . . . . ? C5 N1 C1 C4 53.6(8) . . . . ? Ti1 N1 C1 C4 -129.6(6) . . . . ? C5 N1 C1 C2 170.6(5) . . . . ? Ti1 N1 C1 C2 -12.6(8) . . . . ? C1 N1 C5 N2 -174.8(5) . . . . ? Ti1 N1 C5 N2 7.1(5) . . . . ? C1 N1 C5 C6 3.7(10) . . . . ? Ti1 N1 C5 C6 -174.5(6) . . . . ? C1 N1 C5 Ti1 178.1(6) . . . . ? Si1 N2 C5 N1 -139.7(9) . . . . ? Ti1 N2 C5 N1 -8.0(6) . . . . ? Si1 N2 C5 C6 41.6(12) . . . . ? Ti1 N2 C5 C6 173.3(4) . . . . ? Si1 N2 C5 Ti1 -131.7(11) . . . . ? N2 Ti1 C5 N1 -168.8(3) 14_655 . . . ? N2 Ti1 C5 N1 171.5(6) . . . . ? C13 Ti1 C5 N1 69.0(4) 14_655 . . . ? C13 Ti1 C5 N1 -61.0(4) . . . . ? N1 Ti1 C5 N1 177.80(19) 14_655 . . . ? C5 Ti1 C5 N1 -175.5(4) 14_655 . . . ? Si1 Ti1 C5 N1 -175.5(4) . . . . ? N2 Ti1 C5 N2 19.7(5) 14_655 . . . ? C13 Ti1 C5 N2 -102.5(4) 14_655 . . . ? C13 Ti1 C5 N2 127.5(4) . . . . ? N1 Ti1 C5 N2 6.3(7) 14_655 . . . ? N1 Ti1 C5 N2 -171.5(6) . . . . ? C5 Ti1 C5 N2 13.0(3) 14_655 . . . ? Si1 Ti1 C5 N2 13.0(3) . . . . ? N2 Ti1 C5 C6 -5.8(17) 14_655 . . . ? N2 Ti1 C5 C6 -25.5(15) . . . . ? C13 Ti1 C5 C6 -128.0(17) 14_655 . . . ? C13 Ti1 C5 C6 102.0(17) . . . . ? N1 Ti1 C5 C6 -19(2) 14_655 . . . ? N1 Ti1 C5 C6 163.0(19) . . . . ? C5 Ti1 C5 C6 -12.5(16) 14_655 . . . ? Si1 Ti1 C5 C6 -12.5(16) . . . . ? N1 C5 C6 C7 81.4(9) . . . . ? N2 C5 C6 C7 -100.2(7) . . . . ? Ti1 C5 C6 C7 -78.3(18) . . . . ? N1 C5 C6 C11 -103.9(8) . . . . ? N2 C5 C6 C11 74.5(7) . . . . ? Ti1 C5 C6 C11 96.4(17) . . . . ? C11 C6 C7 C8 -0.7(11) . . . . ? C5 C6 C7 C8 174.0(7) . . . . ? C6 C7 C8 C9 2.7(12) . . . . ? C7 C8 C9 C10 -3.2(14) . . . . ? C8 C9 C10 C11 1.7(14) . . . . ? C7 C6 C11 C10 -0.7(11) . . . . ? C5 C6 C11 C10 -175.5(7) . . . . ? C9 C10 C11 C6 0.3(12) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.556 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.063