data_04181 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H62 N2 Si Ti' _chemical_formula_weight 622.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ti' 'Ti' 0.2776 0.4457 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 19.0300(15) _cell_length_b 11.3547(11) _cell_length_c 18.2460(15) _cell_angle_alpha 90.00 _cell_angle_beta 108.729(3) _cell_angle_gamma 90.00 _cell_volume 3733.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 122(2) _cell_measurement_reflns_used 948 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 23.97 _exptl_crystal_description 'cleaved' _exptl_crystal_colour 'ruby' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.288 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 122(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details ' 0.30 degree frames measured for 2.17 seconds each' _diffrn_measurement_method '\w scans' _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 20961 _diffrn_reflns_av_R_equivalents 0.0805 _diffrn_reflns_av_sigmaI/netI 0.1518 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.53 _reflns_number_total 8538 _reflns_number_gt 4168 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local program) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8538 _refine_ls_number_parameters 627 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1031 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 0.714 _refine_ls_restrained_S_all 0.714 _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 0.21905(2) 0.98492(4) 0.21985(2) 0.01831(11) Uani 1 1 d . . . H62 H 0.4072(15) 1.148(2) 0.4236(17) 0.056(10) Uiso 1 1 d . . . H64 H 0.135(2) 1.286(3) 0.227(2) 0.110(16) Uiso 1 1 d . . . N2 N 0.31289(10) 0.99092(16) 0.31289(10) 0.0181(4) Uani 1 1 d . . . C3 C 0.31858(13) 1.1067(2) 0.33084(13) 0.0193(6) Uani 1 1 d . . . C4 C 0.25599(13) 1.1786(2) 0.31038(14) 0.0197(6) Uani 1 1 d . . . C5 C 0.17854(13) 1.1505(2) 0.29294(13) 0.0197(6) Uani 1 1 d . . . C6 C 0.14921(13) 1.0394(2) 0.29359(14) 0.0203(6) Uani 1 1 d . . . C7 C 0.37044(12) 0.90976(19) 0.35252(14) 0.0180(5) Uani 1 1 d . . . C8 C 0.41424(13) 0.8571(2) 0.31358(14) 0.0199(6) Uani 1 1 d . . . C9 C 0.46445(14) 0.7707(2) 0.35187(16) 0.0247(6) Uani 1 1 d . . . C10 C 0.47197(14) 0.7379(2) 0.42662(16) 0.0268(6) Uani 1 1 d . . . C11 C 0.42967(14) 0.7936(2) 0.46560(16) 0.0254(6) Uani 1 1 d . . . C12 C 0.37784(13) 0.8804(2) 0.43008(14) 0.0202(6) Uani 1 1 d . . . C13 C 0.33247(14) 0.9363(2) 0.47528(15) 0.0244(6) Uani 1 1 d . . . C14 C 0.27376(17) 0.8527(3) 0.48437(18) 0.0305(7) Uani 1 1 d . . . C15 C 0.38056(17) 0.9832(3) 0.55378(16) 0.0310(7) Uani 1 1 d . . . C16 C 0.41072(14) 0.8929(2) 0.23211(15) 0.0223(6) Uani 1 1 d . . . C17 C 0.3932(2) 0.7894(3) 0.17640(19) 0.0368(8) Uani 1 1 d . . . C18 C 0.48254(18) 0.9519(3) 0.2321(2) 0.0366(8) Uani 1 1 d . . . C19 C 0.39332(15) 1.1607(3) 0.36981(18) 0.0267(6) Uani 1 1 d . . . C20 C 0.12906(18) 1.2573(3) 0.2691(2) 0.0308(7) Uani 1 1 d . . . C21 C 0.07054(12) 1.0040(2) 0.28946(14) 0.0238(6) Uani 1 1 d . . . C22 C 0.07171(18) 0.8722(3) 0.3054(2) 0.0427(9) Uani 1 1 d . . . C23 C 0.01416(16) 1.0251(3) 0.20921(17) 0.0342(7) Uani 1 1 d . . . C24 C 0.04589(19) 1.0684(4) 0.3508(2) 0.0439(9) Uani 1 1 d . . . N25 N 0.19607(10) 0.84290(16) 0.18739(10) 0.0188(5) Uani 1 1 d . . . C26 C 0.17283(13) 0.7327(2) 0.15430(14) 0.0198(6) Uani 1 1 d . . . C27 C 0.11436(12) 0.7249(2) 0.08235(14) 0.0194(6) Uani 1 1 d . . . C28 C 0.09248(14) 0.6148(2) 0.04990(15) 0.0228(6) Uani 1 1 d . . . C29 C 0.12637(13) 0.5121(2) 0.08567(15) 0.0242(6) Uani 1 1 d . . . C30 C 0.18313(14) 0.5201(2) 0.15517(15) 0.0247(6) Uani 1 1 d . . . C31 C 0.20668(13) 0.6273(2) 0.19116(14) 0.0223(6) Uani 1 1 d . . . C32 C 0.26508(15) 0.6311(2) 0.27057(16) 0.0265(6) Uani 1 1 d . . . C33 C 0.2271(2) 0.6158(3) 0.33221(19) 0.0431(8) Uani 1 1 d . . . C34 C 0.32722(18) 0.5411(3) 0.2817(2) 0.0380(8) Uani 1 1 d . . . C35 C 0.07915(14) 0.8346(2) 0.03939(15) 0.0228(6) Uani 1 1 d . . . C36 C 0.11867(18) 0.8696(3) -0.01804(17) 0.0312(7) Uani 1 1 d . . . C37 C -0.00420(17) 0.8236(3) -0.0016(2) 0.0375(8) Uani 1 1 d . . . C38 C 0.20377(15) 1.0949(2) 0.12139(16) 0.0258(6) Uani 1 1 d . . . Si39 Si 0.27140(4) 1.16081(6) 0.08086(4) 0.02481(18) Uani 1 1 d . . . C40 C 0.2274(2) 1.2708(3) 0.0039(2) 0.0398(8) Uani 1 1 d . . . C41 C 0.3151(2) 1.0478(3) 0.0353(2) 0.0404(8) Uani 1 1 d . . . C42 C 0.34564(16) 1.2368(3) 0.15865(18) 0.0321(7) Uani 1 1 d . . . H43 H 0.2669(10) 1.2645(17) 0.3096(11) 0.009(6) Uiso 1 1 d . . . H44 H 0.4937(11) 0.7316(18) 0.3246(12) 0.017(6) Uiso 1 1 d . . . H45 H 0.5050(12) 0.6720(19) 0.4513(12) 0.023(7) Uiso 1 1 d . . . H46 H 0.4336(12) 0.7667(18) 0.5166(13) 0.018(6) Uiso 1 1 d . . . H47 H 0.3087(11) 0.9958(18) 0.4501(12) 0.012(6) Uiso 1 1 d . . . H48 H 0.2373(13) 0.827(2) 0.4345(15) 0.038(8) Uiso 1 1 d . . . H49 H 0.2453(14) 0.888(2) 0.5092(15) 0.042(9) Uiso 1 1 d . . . H50 H 0.2983(13) 0.785(2) 0.5103(15) 0.036(8) Uiso 1 1 d . . . H51 H 0.4062(12) 0.918(2) 0.5839(13) 0.022(7) Uiso 1 1 d . . . H52 H 0.4182(14) 1.037(2) 0.5496(14) 0.041(8) Uiso 1 1 d . . . H53 H 0.3499(12) 1.027(2) 0.5786(13) 0.025(7) Uiso 1 1 d . . . H54 H 0.3733(11) 0.9530(17) 0.2121(12) 0.011(6) Uiso 1 1 d . . . H55 H 0.4932(14) 1.015(2) 0.2642(15) 0.038(9) Uiso 1 1 d . . . H56 H 0.5222(14) 0.893(2) 0.2455(15) 0.044(9) Uiso 1 1 d . . . H57 H 0.4796(13) 0.979(2) 0.1802(14) 0.035(8) Uiso 1 1 d . . . H58 H 0.3949(13) 0.818(2) 0.1241(15) 0.040(8) Uiso 1 1 d . . . H59 H 0.4328(14) 0.729(2) 0.1935(15) 0.046(9) Uiso 1 1 d . . . H60 H 0.3491(14) 0.756(2) 0.1728(15) 0.041(9) Uiso 1 1 d . . . H61 H 0.4306(14) 1.125(2) 0.3500(15) 0.049(9) Uiso 1 1 d . . . H63 H 0.3944(13) 1.244(2) 0.3631(14) 0.032(8) Uiso 1 1 d . . . H65 H 0.1444(16) 1.322(3) 0.3002(18) 0.066(11) Uiso 1 1 d . . . H66 H 0.0814(19) 1.241(3) 0.2659(19) 0.083(13) Uiso 1 1 d . . . H67 H 0.0835(18) 0.830(3) 0.2694(18) 0.071(13) Uiso 1 1 d . . . H68 H 0.1042(14) 0.856(2) 0.3523(15) 0.039(9) Uiso 1 1 d . . . H69 H 0.0216(14) 0.847(2) 0.3046(13) 0.031(7) Uiso 1 1 d . . . H70 H 0.0261(13) 0.975(2) 0.1730(14) 0.035(8) Uiso 1 1 d . . . H71 H 0.0104(13) 1.109(2) 0.1974(14) 0.040(8) Uiso 1 1 d . . . H72 H -0.0345(13) 1.003(2) 0.2087(13) 0.035(8) Uiso 1 1 d . . . H73 H 0.0409(14) 1.160(2) 0.3394(15) 0.050(9) Uiso 1 1 d . . . H74 H 0.0770(14) 1.055(2) 0.3968(16) 0.039(9) Uiso 1 1 d . . . H75 H -0.0050(14) 1.033(2) 0.3441(14) 0.045(8) Uiso 1 1 d . . . H76 H 0.1841(10) 0.9808(17) 0.3178(11) 0.004(5) Uiso 1 1 d . . . H77 H 0.0569(12) 0.6130(19) 0.0020(13) 0.023(7) Uiso 1 1 d . . . H78 H 0.1107(11) 0.4349(18) 0.0619(12) 0.013(6) Uiso 1 1 d . . . H79 H 0.2065(11) 0.4453(18) 0.1796(12) 0.020(6) Uiso 1 1 d . . . H80 H 0.2855(12) 0.704(2) 0.2777(14) 0.028(7) Uiso 1 1 d . . . H81 H 0.1850(15) 0.678(2) 0.3261(15) 0.047(9) Uiso 1 1 d . . . H82 H 0.2627(15) 0.628(2) 0.3812(17) 0.054(10) Uiso 1 1 d . . . H83 H 0.2031(13) 0.540(2) 0.3288(14) 0.036(8) Uiso 1 1 d . . . H84 H 0.3120(12) 0.465(2) 0.2863(13) 0.022(7) Uiso 1 1 d . . . H85 H 0.3473(16) 0.546(2) 0.2404(17) 0.059(11) Uiso 1 1 d . . . H86 H 0.3655(14) 0.557(2) 0.3327(15) 0.044(9) Uiso 1 1 d . . . H87 H 0.0870(12) 0.8926(19) 0.0737(13) 0.017(7) Uiso 1 1 d . . . H88 H 0.1003(12) 0.9445(19) -0.0405(13) 0.023(7) Uiso 1 1 d . . . H89 H 0.1729(14) 0.873(2) 0.0048(15) 0.044(9) Uiso 1 1 d . . . H90 H 0.1141(13) 0.810(2) -0.0570(14) 0.032(7) Uiso 1 1 d . . . H91 H -0.0146(14) 0.762(2) -0.0398(15) 0.044(9) Uiso 1 1 d . . . H92 H -0.0270(12) 0.7963(19) 0.0330(13) 0.017(7) Uiso 1 1 d . . . H93 H -0.0278(13) 0.904(2) -0.0246(14) 0.042(8) Uiso 1 1 d . . . H94 H 0.1797(14) 1.163(2) 0.1414(15) 0.053(9) Uiso 1 1 d . . . H95 H 0.1673(13) 1.058(2) 0.0816(14) 0.029(7) Uiso 1 1 d . . . H96 H 0.2148(15) 1.335(2) 0.0272(16) 0.045(10) Uiso 1 1 d . . . H97 H 0.1867(15) 1.231(2) -0.0339(16) 0.046(9) Uiso 1 1 d . . . H98 H 0.2613(15) 1.294(2) -0.0219(16) 0.048(9) Uiso 1 1 d . . . H99 H 0.2819(17) 1.014(3) -0.0015(18) 0.070(13) Uiso 1 1 d . . . H100 H 0.3471(15) 1.085(2) 0.0120(16) 0.046(9) Uiso 1 1 d . . . H101 H 0.344(2) 0.996(3) 0.063(2) 0.099(16) Uiso 1 1 d . . . H102 H 0.3785(14) 1.277(2) 0.1376(15) 0.046(9) Uiso 1 1 d . . . H103 H 0.3266(14) 1.296(2) 0.1877(14) 0.040(8) Uiso 1 1 d . . . H104 H 0.3784(13) 1.177(2) 0.1965(15) 0.042(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0175(2) 0.0205(2) 0.0160(2) -0.0004(2) 0.00409(19) -0.0006(2) N2 0.0200(10) 0.0190(11) 0.0151(11) -0.0015(9) 0.0051(9) 0.0002(9) C3 0.0245(14) 0.0222(13) 0.0103(13) 0.0013(11) 0.0042(11) -0.0023(11) C4 0.0237(14) 0.0170(13) 0.0190(14) -0.0014(11) 0.0075(12) -0.0036(11) C5 0.0230(13) 0.0228(14) 0.0125(13) -0.0023(11) 0.0045(11) 0.0018(11) C6 0.0191(13) 0.0233(14) 0.0173(14) 0.0026(11) 0.0045(11) 0.0023(11) C7 0.0168(13) 0.0156(12) 0.0191(14) -0.0014(10) 0.0025(11) -0.0008(10) C8 0.0172(12) 0.0208(13) 0.0189(14) -0.0045(11) 0.0019(11) -0.0023(11) C9 0.0184(14) 0.0257(15) 0.0295(17) -0.0048(13) 0.0068(13) 0.0037(12) C10 0.0203(14) 0.0244(15) 0.0306(17) 0.0052(13) 0.0011(13) 0.0050(12) C11 0.0247(14) 0.0272(15) 0.0209(16) 0.0023(12) 0.0027(13) -0.0016(12) C12 0.0187(13) 0.0210(13) 0.0174(14) -0.0022(11) 0.0011(11) -0.0036(11) C13 0.0278(15) 0.0224(15) 0.0219(16) 0.0040(12) 0.0065(13) 0.0049(12) C14 0.0263(16) 0.0383(19) 0.0275(18) -0.0023(15) 0.0094(15) 0.0010(15) C15 0.0395(18) 0.0308(17) 0.0212(16) -0.0005(14) 0.0074(14) -0.0002(15) C16 0.0224(14) 0.0232(14) 0.0215(15) -0.0012(12) 0.0071(12) 0.0037(12) C17 0.048(2) 0.0355(19) 0.0294(19) -0.0064(15) 0.0160(17) -0.0031(17) C18 0.0326(18) 0.043(2) 0.036(2) 0.0042(17) 0.0142(16) -0.0044(16) C19 0.0218(15) 0.0253(16) 0.0297(18) -0.0033(14) 0.0037(14) -0.0062(13) C20 0.0286(17) 0.0241(16) 0.040(2) 0.0027(15) 0.0111(16) 0.0039(13) C21 0.0183(13) 0.0344(16) 0.0182(14) -0.0001(12) 0.0050(11) -0.0015(12) C22 0.0221(17) 0.045(2) 0.056(3) 0.015(2) 0.0049(18) -0.0079(15) C23 0.0227(16) 0.046(2) 0.0303(18) 0.0008(16) 0.0033(14) -0.0007(15) C24 0.0299(19) 0.074(3) 0.031(2) -0.0086(19) 0.0141(17) -0.0119(19) N25 0.0191(10) 0.0218(11) 0.0140(11) -0.0008(9) 0.0034(9) -0.0018(9) C26 0.0202(13) 0.0221(14) 0.0185(14) -0.0015(11) 0.0083(11) -0.0031(11) C27 0.0175(13) 0.0227(13) 0.0197(14) -0.0011(11) 0.0082(11) -0.0010(11) C28 0.0197(14) 0.0309(16) 0.0170(15) -0.0065(12) 0.0047(12) -0.0040(12) C29 0.0264(14) 0.0203(14) 0.0283(16) -0.0095(13) 0.0121(12) -0.0070(12) C30 0.0272(14) 0.0206(14) 0.0286(16) 0.0012(13) 0.0120(13) 0.0000(12) C31 0.0229(14) 0.0241(14) 0.0204(15) -0.0025(11) 0.0076(12) -0.0037(11) C32 0.0348(16) 0.0140(13) 0.0258(16) 0.0017(12) 0.0031(13) -0.0028(12) C33 0.055(2) 0.049(2) 0.0200(19) 0.0002(16) 0.0041(17) -0.0004(19) C34 0.0334(18) 0.0274(18) 0.041(2) 0.0025(16) -0.0054(17) 0.0014(14) C35 0.0235(14) 0.0216(14) 0.0201(15) -0.0053(12) 0.0026(12) -0.0012(12) C36 0.0431(19) 0.0303(17) 0.0213(17) -0.0007(14) 0.0119(15) 0.0046(15) C37 0.0282(16) 0.038(2) 0.039(2) 0.0004(17) -0.0003(15) 0.0001(15) C38 0.0283(15) 0.0255(15) 0.0219(16) -0.0008(12) 0.0056(13) -0.0065(13) Si39 0.0255(4) 0.0270(4) 0.0221(4) 0.0030(3) 0.0078(3) -0.0017(3) C40 0.039(2) 0.047(2) 0.035(2) 0.0096(17) 0.0124(17) -0.0019(17) C41 0.041(2) 0.050(2) 0.034(2) -0.0022(18) 0.0170(18) 0.0044(18) C42 0.0284(17) 0.0342(18) 0.0346(19) 0.0012(15) 0.0112(15) -0.0054(14) _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 N25 1.7251(19) . ? Ti1 N2 2.0319(18) . ? Ti1 C38 2.130(3) . ? Ti1 C6 2.260(2) . ? Ti1 C5 2.563(2) . ? Ti1 C3 2.671(2) . ? Ti1 C4 2.704(2) . ? Ti1 H76 2.098(19) . ? N2 C3 1.350(3) . ? N2 C7 1.436(3) . ? C3 C4 1.393(3) . ? C3 C19 1.502(3) . ? C4 C5 1.440(3) . ? C4 H43 0.998(19) . ? C5 C6 1.381(3) . ? C5 C20 1.511(3) . ? C6 C21 1.528(3) . ? C6 H76 0.943(19) . ? C7 C8 1.392(3) . ? C7 C12 1.416(3) . ? C8 C9 1.391(3) . ? C8 C16 1.522(3) . ? C9 C10 1.376(4) . ? C9 H44 0.97(2) . ? C10 C11 1.386(4) . ? C10 H45 0.99(2) . ? C11 C12 1.397(3) . ? C11 H46 0.96(2) . ? C12 C13 1.512(3) . ? C13 C14 1.515(4) . ? C13 C15 1.527(4) . ? C13 H47 0.86(2) . ? C14 H48 0.99(3) . ? C14 H49 0.90(3) . ? C14 H50 0.94(2) . ? C15 H51 0.96(2) . ? C15 H52 0.96(3) . ? C15 H53 0.98(2) . ? C16 C17 1.518(4) . ? C16 C18 1.522(4) . ? C16 H54 0.970(19) . ? C17 H58 1.02(3) . ? C17 H59 0.99(3) . ? C17 H60 0.90(3) . ? C18 H55 0.90(3) . ? C18 H56 0.98(2) . ? C18 H57 0.98(2) . ? C19 H62 0.94(3) . ? C19 H61 0.98(3) . ? C19 H63 0.96(2) . ? C20 H64 0.88(4) . ? C20 H65 0.91(3) . ? C20 H66 0.91(3) . ? C21 C22 1.524(4) . ? C21 C23 1.531(4) . ? C21 C24 1.531(4) . ? C22 H67 0.90(3) . ? C22 H68 0.90(3) . ? C22 H69 0.99(2) . ? C23 H70 0.95(2) . ? C23 H71 0.98(2) . ? C23 H72 0.96(2) . ? C24 H73 1.06(3) . ? C24 H74 0.87(3) . ? C24 H75 1.02(3) . ? N25 C26 1.398(3) . ? C26 C31 1.422(3) . ? C26 C27 1.425(3) . ? C27 C28 1.388(3) . ? C27 C35 1.510(3) . ? C28 C29 1.389(3) . ? C28 H77 0.92(2) . ? C29 C30 1.380(3) . ? C29 H78 0.98(2) . ? C30 C31 1.387(3) . ? C30 H79 1.00(2) . ? C31 C32 1.517(3) . ? C32 C34 1.526(4) . ? C32 C33 1.529(4) . ? C32 H80 0.91(2) . ? C33 H81 1.05(3) . ? C33 H82 0.94(3) . ? C33 H83 0.97(2) . ? C34 H84 0.93(2) . ? C34 H85 0.95(3) . ? C34 H86 1.00(3) . ? C35 C36 1.526(4) . ? C35 C37 1.526(4) . ? C35 H87 0.89(2) . ? C36 H88 0.96(2) . ? C36 H89 0.98(2) . ? C36 H90 0.97(2) . ? C37 H91 0.96(3) . ? C37 H92 0.93(2) . ? C37 H93 1.04(2) . ? C38 Si39 1.837(3) . ? C38 H94 1.02(3) . ? C38 H95 0.93(2) . ? Si39 C42 1.862(3) . ? Si39 C41 1.863(3) . ? Si39 C40 1.865(3) . ? C40 H96 0.91(3) . ? C40 H97 0.97(3) . ? C40 H98 0.95(3) . ? C41 H99 0.85(3) . ? C41 H100 0.94(3) . ? C41 H101 0.85(4) . ? C42 H102 0.95(3) . ? C42 H103 0.99(3) . ? C42 H104 1.02(2) . ? 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 N25 Ti1 N2 112.09(8) . . ? N25 Ti1 C38 107.91(10) . . ? N2 Ti1 C38 122.03(9) . . ? N25 Ti1 C6 109.12(9) . . ? N2 Ti1 C6 91.18(8) . . ? C38 Ti1 C6 113.24(10) . . ? N25 Ti1 C5 141.16(8) . . ? N2 Ti1 C5 82.60(7) . . ? C38 Ti1 C5 91.52(10) . . ? C6 Ti1 C5 32.51(8) . . ? N25 Ti1 C3 141.62(8) . . ? N2 Ti1 C3 29.58(7) . . ? C38 Ti1 C3 101.98(9) . . ? C6 Ti1 C3 79.42(8) . . ? C5 Ti1 C3 58.96(7) . . ? N25 Ti1 C4 163.22(8) . . ? N2 Ti1 C4 58.41(7) . . ? C38 Ti1 C4 88.67(9) . . ? C6 Ti1 C4 60.06(8) . . ? C5 Ti1 C4 31.59(7) . . ? C3 Ti1 C4 30.02(7) . . ? N25 Ti1 H76 99.0(5) . . ? N2 Ti1 H76 73.9(5) . . ? C38 Ti1 H76 137.4(5) . . ? C6 Ti1 H76 24.6(5) . . ? C5 Ti1 H76 48.9(5) . . ? C3 Ti1 H76 73.0(5) . . ? C4 Ti1 H76 65.7(5) . . ? C3 N2 C7 120.90(19) . . ? C3 N2 Ti1 102.46(15) . . ? C7 N2 Ti1 136.27(15) . . ? N2 C3 C4 120.7(2) . . ? N2 C3 C19 120.1(2) . . ? C4 C3 C19 119.1(2) . . ? N2 C3 Ti1 47.96(11) . . ? C4 C3 Ti1 76.30(14) . . ? C19 C3 Ti1 154.61(19) . . ? C3 C4 C5 131.0(2) . . ? C3 C4 Ti1 73.68(14) . . ? C5 C4 Ti1 68.77(13) . . ? C3 C4 H43 114.4(11) . . ? C5 C4 H43 114.6(11) . . ? Ti1 C4 H43 143.2(12) . . ? C6 C5 C4 126.0(2) . . ? C6 C5 C20 121.3(2) . . ? C4 C5 C20 112.6(2) . . ? C6 C5 Ti1 61.60(13) . . ? C4 C5 Ti1 79.64(14) . . ? C20 C5 Ti1 134.63(19) . . ? C5 C6 C21 129.2(2) . . ? C5 C6 Ti1 85.89(15) . . ? C21 C6 Ti1 130.73(17) . . ? C5 C6 H76 115.0(12) . . ? C21 C6 H76 111.6(12) . . ? Ti1 C6 H76 68.0(12) . . ? C8 C7 C12 121.7(2) . . ? C8 C7 N2 120.2(2) . . ? C12 C7 N2 118.0(2) . . ? C9 C8 C7 118.3(2) . . ? C9 C8 C16 119.1(2) . . ? C7 C8 C16 122.6(2) . . ? C10 C9 C8 121.6(2) . . ? C10 C9 H44 119.5(13) . . ? C8 C9 H44 118.9(13) . . ? C9 C10 C11 119.5(2) . . ? C9 C10 H45 120.4(13) . . ? C11 C10 H45 120.0(13) . . ? C10 C11 C12 121.6(3) . . ? C10 C11 H46 118.3(13) . . ? C12 C11 H46 119.9(14) . . ? C11 C12 C7 117.3(2) . . ? C11 C12 C13 119.0(2) . . ? C7 C12 C13 123.7(2) . . ? C12 C13 C14 111.5(2) . . ? C12 C13 C15 112.5(2) . . ? C14 C13 C15 110.9(2) . . ? C12 C13 H47 109.4(14) . . ? C14 C13 H47 105.7(14) . . ? C15 C13 H47 106.4(14) . . ? C13 C14 H48 114.0(14) . . ? C13 C14 H49 111.2(17) . . ? H48 C14 H49 103(2) . . ? C13 C14 H50 107.5(15) . . ? H48 C14 H50 108(2) . . ? H49 C14 H50 113(2) . . ? C13 C15 H51 108.0(14) . . ? C13 C15 H52 112.6(15) . . ? H51 C15 H52 106.3(19) . . ? C13 C15 H53 110.1(13) . . ? H51 C15 H53 113.3(19) . . ? H52 C15 H53 106(2) . . ? C17 C16 C8 112.3(2) . . ? C17 C16 C18 110.2(3) . . ? C8 C16 C18 111.1(2) . . ? C17 C16 H54 108.4(12) . . ? C8 C16 H54 110.6(12) . . ? C18 C16 H54 104.0(12) . . ? C16 C17 H58 108.3(14) . . ? C16 C17 H59 110.1(15) . . ? H58 C17 H59 105(2) . . ? C16 C17 H60 111.8(18) . . ? H58 C17 H60 112(2) . . ? H59 C17 H60 109(2) . . ? C16 C18 H55 111.2(17) . . ? C16 C18 H56 108.8(15) . . ? H55 C18 H56 113(2) . . ? C16 C18 H57 111.4(14) . . ? H55 C18 H57 108(2) . . ? H56 C18 H57 105(2) . . ? C3 C19 H62 109.8(17) . . ? C3 C19 H61 110.1(15) . . ? H62 C19 H61 109(2) . . ? C3 C19 H63 113.6(14) . . ? H62 C19 H63 106(2) . . ? H61 C19 H63 108(2) . . ? C5 C20 H64 108(3) . . ? C5 C20 H65 114.7(19) . . ? H64 C20 H65 98(3) . . ? C5 C20 H66 112(2) . . ? H64 C20 H66 116(3) . . ? H65 C20 H66 109(3) . . ? C22 C21 C6 107.1(2) . . ? C22 C21 C23 107.4(3) . . ? C6 C21 C23 112.4(2) . . ? C22 C21 C24 108.6(3) . . ? C6 C21 C24 111.3(2) . . ? C23 C21 C24 109.8(2) . . ? C21 C22 H67 112(2) . . ? C21 C22 H68 110.5(17) . . ? H67 C22 H68 109(3) . . ? C21 C22 H69 109.2(14) . . ? H67 C22 H69 107(2) . . ? H68 C22 H69 108(2) . . ? C21 C23 H70 108.7(15) . . ? C21 C23 H71 110.0(15) . . ? H70 C23 H71 116(2) . . ? C21 C23 H72 110.3(14) . . ? H70 C23 H72 106(2) . . ? H71 C23 H72 105(2) . . ? C21 C24 H73 110.8(15) . . ? C21 C24 H74 110.3(18) . . ? H73 C24 H74 111(2) . . ? C21 C24 H75 103.1(15) . . ? H73 C24 H75 110(2) . . ? H74 C24 H75 112(2) . . ? C26 N25 Ti1 174.34(17) . . ? N25 C26 C31 121.1(2) . . ? N25 C26 C27 119.9(2) . . ? C31 C26 C27 119.0(2) . . ? C28 C27 C26 119.2(2) . . ? C28 C27 C35 120.0(2) . . ? C26 C27 C35 120.8(2) . . ? C27 C28 C29 121.6(2) . . ? C27 C28 H77 117.0(14) . . ? C29 C28 H77 121.2(14) . . ? C30 C29 C28 119.0(2) . . ? C30 C29 H78 120.1(12) . . ? C28 C29 H78 120.9(12) . . ? C29 C30 C31 122.1(2) . . ? C29 C30 H79 117.5(12) . . ? C31 C30 H79 120.5(12) . . ? C30 C31 C26 119.1(2) . . ? C30 C31 C32 120.2(2) . . ? C26 C31 C32 120.6(2) . . ? C31 C32 C34 114.0(2) . . ? C31 C32 C33 109.0(2) . . ? C34 C32 C33 110.8(3) . . ? C31 C32 H80 108.1(15) . . ? C34 C32 H80 108.5(15) . . ? C33 C32 H80 106.1(16) . . ? C32 C33 H81 111.9(15) . . ? C32 C33 H82 108.5(17) . . ? H81 C33 H82 107(2) . . ? C32 C33 H83 112.1(15) . . ? H81 C33 H83 105(2) . . ? H82 C33 H83 112(2) . . ? C32 C34 H84 112.7(14) . . ? C32 C34 H85 110.5(17) . . ? H84 C34 H85 110(2) . . ? C32 C34 H86 107.8(14) . . ? H84 C34 H86 104(2) . . ? H85 C34 H86 112(2) . . ? C27 C35 C36 109.7(2) . . ? C27 C35 C37 113.9(2) . . ? C36 C35 C37 110.4(2) . . ? C27 C35 H87 107.5(14) . . ? C36 C35 H87 106.5(15) . . ? C37 C35 H87 108.6(14) . . ? C35 C36 H88 109.4(14) . . ? C35 C36 H89 113.8(16) . . ? H88 C36 H89 109(2) . . ? C35 C36 H90 112.0(15) . . ? H88 C36 H90 111.9(19) . . ? H89 C36 H90 100(2) . . ? C35 C37 H91 110.8(16) . . ? C35 C37 H92 109.6(14) . . ? H91 C37 H92 103(2) . . ? C35 C37 H93 111.8(13) . . ? H91 C37 H93 112(2) . . ? H92 C37 H93 109.3(19) . . ? Si39 C38 Ti1 130.92(15) . . ? Si39 C38 H94 106.7(15) . . ? Ti1 C38 H94 95.6(15) . . ? Si39 C38 H95 108.4(15) . . ? Ti1 C38 H95 104.9(15) . . ? H94 C38 H95 108(2) . . ? C38 Si39 C42 109.88(14) . . ? C38 Si39 C41 111.68(15) . . ? C42 Si39 C41 108.74(17) . . ? C38 Si39 C40 111.87(14) . . ? C42 Si39 C40 108.12(16) . . ? C41 Si39 C40 106.40(18) . . ? Si39 C40 H96 107.9(18) . . ? Si39 C40 H97 106.7(16) . . ? H96 C40 H97 116(2) . . ? Si39 C40 H98 110.5(16) . . ? H96 C40 H98 109(2) . . ? H97 C40 H98 107(2) . . ? Si39 C41 H99 110(2) . . ? Si39 C41 H100 109.9(17) . . ? H99 C41 H100 105(3) . . ? Si39 C41 H101 120(3) . . ? H99 C41 H101 110(3) . . ? H100 C41 H101 101(3) . . ? Si39 C42 H102 110.6(16) . . ? Si39 C42 H103 113.7(15) . . ? H102 C42 H103 107(2) . . ? Si39 C42 H104 110.8(14) . . ? H102 C42 H104 105(2) . . ? H103 C42 H104 110(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 N25 Ti1 N2 C3 -177.12(14) . . . . ? C38 Ti1 N2 C3 52.69(18) . . . . ? C6 Ti1 N2 C3 -65.89(15) . . . . ? C5 Ti1 N2 C3 -34.46(14) . . . . ? C4 Ti1 N2 C3 -12.67(14) . . . . ? N25 Ti1 N2 C7 10.2(2) . . . . ? C38 Ti1 N2 C7 -120.0(2) . . . . ? C6 Ti1 N2 C7 121.4(2) . . . . ? C5 Ti1 N2 C7 152.8(2) . . . . ? C3 Ti1 N2 C7 -172.7(3) . . . . ? C4 Ti1 N2 C7 174.6(2) . . . . ? C7 N2 C3 C4 -160.9(2) . . . . ? Ti1 N2 C3 C4 25.0(3) . . . . ? C7 N2 C3 C19 22.1(3) . . . . ? Ti1 N2 C3 C19 -152.0(2) . . . . ? C7 N2 C3 Ti1 174.1(2) . . . . ? N25 Ti1 C3 N2 4.3(2) . . . . ? C38 Ti1 C3 N2 -136.43(16) . . . . ? C6 Ti1 C3 N2 111.82(15) . . . . ? C5 Ti1 C3 N2 139.09(17) . . . . ? C4 Ti1 C3 N2 158.1(2) . . . . ? N25 Ti1 C3 C4 -153.78(15) . . . . ? N2 Ti1 C3 C4 -158.1(2) . . . . ? C38 Ti1 C3 C4 65.49(16) . . . . ? C6 Ti1 C3 C4 -46.26(15) . . . . ? C5 Ti1 C3 C4 -18.99(14) . . . . ? N25 Ti1 C3 C19 75.5(4) . . . . ? N2 Ti1 C3 C19 71.2(4) . . . . ? C38 Ti1 C3 C19 -65.3(4) . . . . ? C6 Ti1 C3 C19 -177.0(4) . . . . ? C5 Ti1 C3 C19 -149.7(4) . . . . ? C4 Ti1 C3 C19 -130.8(5) . . . . ? N2 C3 C4 C5 22.3(4) . . . . ? C19 C3 C4 C5 -160.7(3) . . . . ? Ti1 C3 C4 C5 41.1(3) . . . . ? N2 C3 C4 Ti1 -18.81(19) . . . . ? C19 C3 C4 Ti1 158.2(2) . . . . ? N25 Ti1 C4 C3 71.8(3) . . . . ? N2 Ti1 C4 C3 12.49(13) . . . . ? C38 Ti1 C4 C3 -117.08(16) . . . . ? C6 Ti1 C4 C3 124.96(16) . . . . ? C5 Ti1 C4 C3 147.8(2) . . . . ? N25 Ti1 C4 C5 -76.0(3) . . . . ? N2 Ti1 C4 C5 -135.35(16) . . . . ? C38 Ti1 C4 C5 95.08(15) . . . . ? C6 Ti1 C4 C5 -22.88(14) . . . . ? C3 Ti1 C4 C5 -147.8(2) . . . . ? C3 C4 C5 C6 0.5(4) . . . . ? Ti1 C4 C5 C6 43.0(2) . . . . ? C3 C4 C5 C20 -176.8(3) . . . . ? Ti1 C4 C5 C20 -134.2(2) . . . . ? C3 C4 C5 Ti1 -42.6(3) . . . . ? N25 Ti1 C5 C6 12.3(2) . . . . ? N2 Ti1 C5 C6 -104.03(15) . . . . ? C38 Ti1 C5 C6 133.86(16) . . . . ? C3 Ti1 C5 C6 -123.06(16) . . . . ? C4 Ti1 C5 C6 -141.2(2) . . . . ? N25 Ti1 C5 C4 153.46(15) . . . . ? N2 Ti1 C5 C4 37.13(14) . . . . ? C38 Ti1 C5 C4 -84.98(15) . . . . ? C6 Ti1 C5 C4 141.2(2) . . . . ? C3 Ti1 C5 C4 18.11(13) . . . . ? N25 Ti1 C5 C20 -94.9(3) . . . . ? N2 Ti1 C5 C20 148.8(3) . . . . ? C38 Ti1 C5 C20 26.7(3) . . . . ? C6 Ti1 C5 C20 -107.2(3) . . . . ? C3 Ti1 C5 C20 129.7(3) . . . . ? C4 Ti1 C5 C20 111.6(3) . . . . ? C4 C5 C6 C21 168.5(2) . . . . ? C20 C5 C6 C21 -14.5(4) . . . . ? Ti1 C5 C6 C21 -141.8(3) . . . . ? C4 C5 C6 Ti1 -49.7(3) . . . . ? C20 C5 C6 Ti1 127.3(2) . . . . ? N25 Ti1 C6 C5 -171.87(14) . . . . ? N2 Ti1 C6 C5 74.21(15) . . . . ? C38 Ti1 C6 C5 -51.67(17) . . . . ? C3 Ti1 C6 C5 46.93(14) . . . . ? C4 Ti1 C6 C5 22.28(13) . . . . ? N25 Ti1 C6 C21 -31.1(2) . . . . ? N2 Ti1 C6 C21 -145.0(2) . . . . ? C38 Ti1 C6 C21 89.1(2) . . . . ? C5 Ti1 C6 C21 140.8(3) . . . . ? C3 Ti1 C6 C21 -172.3(2) . . . . ? C4 Ti1 C6 C21 163.0(2) . . . . ? C3 N2 C7 C8 -111.3(3) . . . . ? Ti1 N2 C7 C8 60.4(3) . . . . ? C3 N2 C7 C12 72.4(3) . . . . ? Ti1 N2 C7 C12 -115.9(2) . . . . ? C12 C7 C8 C9 2.3(3) . . . . ? N2 C7 C8 C9 -173.9(2) . . . . ? C12 C7 C8 C16 -176.0(2) . . . . ? N2 C7 C8 C16 7.8(3) . . . . ? C7 C8 C9 C10 -0.7(4) . . . . ? C16 C8 C9 C10 177.6(2) . . . . ? C8 C9 C10 C11 -1.3(4) . . . . ? C9 C10 C11 C12 1.8(4) . . . . ? C10 C11 C12 C7 -0.3(4) . . . . ? C10 C11 C12 C13 178.9(2) . . . . ? C8 C7 C12 C11 -1.8(3) . . . . ? N2 C7 C12 C11 174.5(2) . . . . ? C8 C7 C12 C13 179.1(2) . . . . ? N2 C7 C12 C13 -4.7(3) . . . . ? C11 C12 C13 C14 -73.2(3) . . . . ? C7 C12 C13 C14 106.0(3) . . . . ? C11 C12 C13 C15 52.2(3) . . . . ? C7 C12 C13 C15 -128.7(3) . . . . ? C9 C8 C16 C17 58.2(3) . . . . ? C7 C8 C16 C17 -123.5(3) . . . . ? C9 C8 C16 C18 -65.6(3) . . . . ? C7 C8 C16 C18 112.6(3) . . . . ? C5 C6 C21 C22 -171.0(3) . . . . ? Ti1 C6 C21 C22 63.5(3) . . . . ? C5 C6 C21 C23 71.2(4) . . . . ? Ti1 C6 C21 C23 -54.2(3) . . . . ? C5 C6 C21 C24 -52.4(4) . . . . ? Ti1 C6 C21 C24 -177.9(2) . . . . ? N2 Ti1 N25 C26 -163.6(17) . . . . ? C38 Ti1 N25 C26 -26.5(18) . . . . ? C6 Ti1 N25 C26 96.9(17) . . . . ? C5 Ti1 N25 C26 90.0(17) . . . . ? C3 Ti1 N25 C26 -165.9(17) . . . . ? C4 Ti1 N25 C26 144.1(16) . . . . ? Ti1 N25 C26 C31 172.3(16) . . . . ? Ti1 N25 C26 C27 -7.6(19) . . . . ? N25 C26 C27 C28 179.3(2) . . . . ? C31 C26 C27 C28 -0.6(3) . . . . ? N25 C26 C27 C35 2.7(3) . . . . ? C31 C26 C27 C35 -177.2(2) . . . . ? C26 C27 C28 C29 -0.3(4) . . . . ? C35 C27 C28 C29 176.5(2) . . . . ? C27 C28 C29 C30 0.0(4) . . . . ? C28 C29 C30 C31 1.1(4) . . . . ? C29 C30 C31 C26 -1.9(4) . . . . ? C29 C30 C31 C32 175.1(2) . . . . ? N25 C26 C31 C30 -178.3(2) . . . . ? C27 C26 C31 C30 1.6(3) . . . . ? N25 C26 C31 C32 4.7(3) . . . . ? C27 C26 C31 C32 -175.4(2) . . . . ? C30 C31 C32 C34 39.4(4) . . . . ? C26 C31 C32 C34 -143.6(3) . . . . ? C30 C31 C32 C33 -85.0(3) . . . . ? C26 C31 C32 C33 92.0(3) . . . . ? C28 C27 C35 C36 -84.4(3) . . . . ? C26 C27 C35 C36 92.3(3) . . . . ? C28 C27 C35 C37 40.0(3) . . . . ? C26 C27 C35 C37 -143.4(3) . . . . ? N25 Ti1 C38 Si39 -104.0(2) . . . . ? N2 Ti1 C38 Si39 27.9(2) . . . . ? C6 Ti1 C38 Si39 135.06(18) . . . . ? C5 Ti1 C38 Si39 110.1(2) . . . . ? C3 Ti1 C38 Si39 51.6(2) . . . . ? C4 Ti1 C38 Si39 78.7(2) . . . . ? Ti1 C38 Si39 C42 -49.8(2) . . . . ? Ti1 C38 Si39 C41 71.0(2) . . . . ? Ti1 C38 Si39 C40 -169.89(19) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.323 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.057