data_zj46 _audit_creation_date 2013-10-11 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C37 H35 N Si Ti' _chemical_formula_sum 'C37 H35 N Si Ti' _chemical_formula_weight 569.65 _chemical_melting_point ? _chemical_oxdiff_formula 'C26 H17 N1 Si1 Ti1' 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' _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.2052(3) _cell_length_b 17.3311(5) _cell_length_c 17.0297(6) _cell_angle_alpha 90 _cell_angle_beta 99.069(3) _cell_angle_gamma 90 _cell_volume 2974.35(17) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6452 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 28.9020 _cell_measurement_theta_min 3.7230 _exptl_absorpt_coefficient_mu 0.355 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.86303 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dark green' _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description 'block' _exptl_crystal_F_000 1200 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_unetI/netI 0.0312 _diffrn_reflns_Laue_measured_fraction_full 0.971 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 11341 _diffrn_reflns_point_group_measured_fraction_full 0.971 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 3.100 _diffrn_ambient_temperature 180.15 _diffrn_detector_area_resol_mean 10.3914 _diffrn_measured_fraction_theta_full 0.9919 _diffrn_measured_fraction_theta_max 0.8327 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -75.00 96.00 1.0000 13.8600 omega____ theta____ kappa____ phi______ frames - 10.7017 0.0000 0.0000 171 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0258797000 _diffrn_orient_matrix_UB_12 -0.0258699000 _diffrn_orient_matrix_UB_13 0.0259712000 _diffrn_orient_matrix_UB_21 0.0622730000 _diffrn_orient_matrix_UB_22 -0.0189832000 _diffrn_orient_matrix_UB_23 0.0078280000 _diffrn_orient_matrix_UB_31 0.0201607000 _diffrn_orient_matrix_UB_32 0.0254162000 _diffrn_orient_matrix_UB_33 0.0322820000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4460 _reflns_number_total 5222 _reflns_odcompleteness_completeness 99.19 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 25.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _refine_diff_density_max 0.602 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.048 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 363 _refine_ls_number_reflns 5222 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0386 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+2.0176P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0935 _refine_ls_wR_factor_ref 0.1000 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37) 2.b Secondary CH2 refined with riding coordinates: C25(H25A,H25B), C26(H26A,H26B) 2.c Aromatic/amide H refined with riding coordinates: C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23) 2.d Idealised Me refined as rotating group: C24(H24A,H24B,H24C), C27(H27A,H27B,H27C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.65480(3) 0.34756(2) 0.38230(2) 0.02261(12) Uani 1 1 d . . . . . N1 N 1.14035(16) 0.34181(10) 0.40283(11) 0.0282(4) Uani 1 1 d . . . . . Si1 Si 1.10974(5) 0.25308(3) 0.44530(4) 0.02719(15) Uani 1 1 d . . . . . C1 C 1.04570(19) 0.38709(11) 0.37392(12) 0.0232(4) Uani 1 1 d . . . . . C2 C 0.90174(19) 0.36717(11) 0.36977(12) 0.0214(4) Uani 1 1 d . . . . . C3 C 0.85739(19) 0.31368(11) 0.42811(11) 0.0214(4) Uani 1 1 d . . . . . C4 C 0.93776(19) 0.26012(11) 0.47011(11) 0.0230(4) Uani 1 1 d . . . . . C5 C 1.08033(19) 0.46568(11) 0.34592(11) 0.0224(4) Uani 1 1 d . . . . . C6 C 1.1865(2) 0.47312(12) 0.30474(12) 0.0275(5) Uani 1 1 d . . . . . H6 H 1.2360 0.4288 0.2946 0.033 Uiso 1 1 calc R U . . . C7 C 1.2210(2) 0.54508(13) 0.27814(13) 0.0334(5) Uani 1 1 d . . . . . H7 H 1.2926 0.5495 0.2489 0.040 Uiso 1 1 calc R U . . . C8 C 1.1521(2) 0.60986(13) 0.29404(14) 0.0358(5) Uani 1 1 d . . . . . H8 H 1.1758 0.6589 0.2758 0.043 Uiso 1 1 calc R U . . . C9 C 1.0482(2) 0.60326(13) 0.33674(15) 0.0368(5) Uani 1 1 d . . . . . H9 H 1.0015 0.6480 0.3489 0.044 Uiso 1 1 calc R U . . . C10 C 1.0120(2) 0.53129(12) 0.36186(13) 0.0298(5) Uani 1 1 d . . . . . H10 H 0.9394 0.5270 0.3904 0.036 Uiso 1 1 calc R U . . . C11 C 0.8852(2) 0.20534(12) 0.52409(11) 0.0244(4) Uani 1 1 d . . . . . C12 C 0.7752(2) 0.22341(14) 0.55979(13) 0.0363(5) Uani 1 1 d . . . . . H12 H 0.7373 0.2735 0.5525 0.044 Uiso 1 1 calc R U . . . C13 C 0.7197(3) 0.17020(16) 0.60571(14) 0.0462(6) Uani 1 1 d . . . . . H13 H 0.6443 0.1840 0.6289 0.055 Uiso 1 1 calc R U . . . C14 C 0.7731(3) 0.09746(15) 0.61791(13) 0.0438(6) Uani 1 1 d . . . . . H14 H 0.7333 0.0605 0.6479 0.053 Uiso 1 1 calc R U . . . C15 C 0.8848(3) 0.07895(13) 0.58619(13) 0.0384(6) Uani 1 1 d . . . . . H15 H 0.9239 0.0294 0.5958 0.046 Uiso 1 1 calc R U . . . C16 C 0.9414(2) 0.13194(12) 0.54020(12) 0.0302(5) Uani 1 1 d . . . . . H16 H 1.0192 0.1183 0.5193 0.036 Uiso 1 1 calc R U . . . C17 C 0.79780(19) 0.39339(11) 0.31630(12) 0.0246(4) Uani 1 1 d . . . . . C18 C 0.8014(2) 0.43192(12) 0.24039(13) 0.0287(5) Uani 1 1 d . . . . . C19 C 0.8937(2) 0.41078(13) 0.19192(13) 0.0343(5) Uani 1 1 d . . . . . H19 H 0.9567 0.3716 0.2092 0.041 Uiso 1 1 calc R U . . . C20 C 0.8951(3) 0.44604(15) 0.11880(14) 0.0436(6) Uani 1 1 d . . . . . H20 H 0.9592 0.4311 0.0869 0.052 Uiso 1 1 calc R U . . . C21 C 0.8040(3) 0.50258(16) 0.09243(16) 0.0509(7) Uani 1 1 d . . . . . H21 H 0.8063 0.5276 0.0430 0.061 Uiso 1 1 calc R U . . . C22 C 0.7098(3) 0.52250(16) 0.13807(18) 0.0553(8) Uani 1 1 d . . . . . H22 H 0.6457 0.5607 0.1195 0.066 Uiso 1 1 calc R U . . . C23 C 0.7071(2) 0.48767(15) 0.21071(16) 0.0459(7) Uani 1 1 d . . . . . H23 H 0.6403 0.5018 0.2410 0.055 Uiso 1 1 calc R U . . . C24 C 1.0331(3) 0.18860(18) 0.29023(17) 0.0582(8) Uani 1 1 d . . . . . H24A H 0.9407 0.1894 0.2995 0.087 Uiso 1 1 calc R U . . . H24B H 1.0452 0.1464 0.2538 0.087 Uiso 1 1 calc R U . . . H24C H 1.0543 0.2378 0.2668 0.087 Uiso 1 1 calc R U . . . C25 C 1.1244(2) 0.17661(13) 0.36871(15) 0.0375(5) Uani 1 1 d . . . . . H25A H 1.2172 0.1752 0.3585 0.045 Uiso 1 1 calc R U . . . H25B H 1.1046 0.1258 0.3907 0.045 Uiso 1 1 calc R U . . . C26 C 1.2455(2) 0.23827(14) 0.53121(16) 0.0459(6) Uani 1 1 d . . . . . H26A H 1.2230 0.1930 0.5618 0.055 Uiso 1 1 calc R U . . . H26B H 1.3282 0.2259 0.5102 0.055 Uiso 1 1 calc R U . . . C27 C 1.2720(3) 0.3047(2) 0.58639(16) 0.0632(8) Uani 1 1 d . . . . . H27A H 1.2915 0.3506 0.5566 0.095 Uiso 1 1 calc R U . . . H27B H 1.3483 0.2929 0.6273 0.095 Uiso 1 1 calc R U . . . H27C H 1.1939 0.3145 0.6117 0.095 Uiso 1 1 calc R U . . . C28 C 0.5308(2) 0.46326(13) 0.38634(16) 0.0379(6) Uani 1 1 d . . . . . H28 H 0.4774 0.4893 0.3395 0.046 Uiso 1 1 calc R U . . . C29 C 0.4813(2) 0.41301(13) 0.43862(14) 0.0350(5) Uani 1 1 d . . . . . H29 H 0.3870 0.3956 0.4346 0.042 Uiso 1 1 calc R U . . . C30 C 0.5839(3) 0.39605(17) 0.50066(15) 0.0496(7) Uani 1 1 d . . . . . H30 H 0.5753 0.3652 0.5492 0.060 Uiso 1 1 calc R U . . . C31 C 0.6970(3) 0.43727(18) 0.48746(19) 0.0603(9) Uani 1 1 d . . . . . H31 H 0.7817 0.4418 0.5258 0.072 Uiso 1 1 calc R U . . . C32 C 0.6642(2) 0.47949(14) 0.4174(2) 0.0546(8) Uani 1 1 d . . . . . H32 H 0.7209 0.5195 0.3970 0.065 Uiso 1 1 calc R U . . . C33 C 0.5324(3) 0.29695(14) 0.26352(15) 0.0503(7) Uani 1 1 d . . . . . H33 H 0.5021 0.3264 0.2134 0.060 Uiso 1 1 calc R U . . . C34 C 0.6491(3) 0.25389(16) 0.28060(16) 0.0475(7) Uani 1 1 d . . . . . H34 H 0.7171 0.2475 0.2447 0.057 Uiso 1 1 calc R U . . . C35 C 0.6469(3) 0.21520(13) 0.35007(17) 0.0460(7) Uani 1 1 d . . . . . H35 H 0.7127 0.1754 0.3734 0.055 Uiso 1 1 calc R U . . . C36 C 0.5306(3) 0.23319(15) 0.37732(15) 0.0473(7) Uani 1 1 d . . . . . H36 H 0.4980 0.2084 0.4236 0.057 Uiso 1 1 calc R U . . . C37 C 0.4585(2) 0.28285(15) 0.32377(18) 0.0489(7) Uani 1 1 d . . . . . H37 H 0.3655 0.3005 0.3249 0.059 Uiso 1 1 calc R U . . . 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 0.01639(19) 0.0207(2) 0.0302(2) -0.00513(15) 0.00214(15) 0.00076(14) N1 0.0181(9) 0.0253(9) 0.0405(10) 0.0062(8) 0.0032(7) 0.0011(7) Si1 0.0189(3) 0.0225(3) 0.0394(3) 0.0083(2) 0.0021(2) 0.0024(2) C1 0.0204(10) 0.0218(10) 0.0267(10) 0.0006(8) 0.0016(8) -0.0005(8) C2 0.0186(10) 0.0165(9) 0.0288(10) -0.0001(8) 0.0030(8) 0.0018(8) C3 0.0203(10) 0.0199(10) 0.0240(10) -0.0040(8) 0.0038(8) -0.0007(8) C4 0.0224(10) 0.0225(10) 0.0236(10) -0.0004(8) 0.0020(8) -0.0004(8) C5 0.0186(10) 0.0222(10) 0.0240(10) 0.0034(8) -0.0038(8) -0.0010(8) C6 0.0263(11) 0.0262(11) 0.0301(11) 0.0016(9) 0.0047(9) -0.0005(9) C7 0.0342(12) 0.0338(12) 0.0330(12) 0.0054(10) 0.0079(10) -0.0057(10) C8 0.0391(13) 0.0241(11) 0.0426(13) 0.0095(10) 0.0015(11) -0.0074(10) C9 0.0316(12) 0.0215(11) 0.0554(15) 0.0016(10) 0.0012(11) 0.0029(9) C10 0.0215(11) 0.0274(11) 0.0399(12) -0.0003(10) 0.0032(9) 0.0002(9) C11 0.0269(11) 0.0248(10) 0.0206(10) 0.0001(8) 0.0004(8) -0.0028(9) C12 0.0410(13) 0.0356(13) 0.0342(12) 0.0044(10) 0.0123(10) 0.0014(11) C13 0.0484(15) 0.0560(17) 0.0384(13) 0.0041(12) 0.0195(12) -0.0069(13) C14 0.0589(17) 0.0442(15) 0.0282(12) 0.0092(11) 0.0065(11) -0.0181(13) C15 0.0540(16) 0.0275(12) 0.0310(12) 0.0066(10) -0.0019(11) -0.0068(11) C16 0.0351(12) 0.0288(11) 0.0256(11) 0.0013(9) 0.0012(9) -0.0014(10) C17 0.0206(10) 0.0170(10) 0.0349(11) 0.0009(9) 0.0004(9) -0.0002(8) C18 0.0219(11) 0.0246(11) 0.0359(12) 0.0060(9) -0.0068(9) -0.0067(9) C19 0.0402(13) 0.0288(12) 0.0301(11) 0.0004(10) -0.0058(10) -0.0006(10) C20 0.0524(16) 0.0469(15) 0.0290(12) 0.0027(11) -0.0017(11) -0.0085(12) C21 0.0505(16) 0.0526(16) 0.0435(14) 0.0248(13) -0.0115(13) -0.0152(13) C22 0.0351(14) 0.0530(17) 0.0722(19) 0.0392(15) -0.0085(14) -0.0001(12) C23 0.0271(12) 0.0447(15) 0.0636(16) 0.0262(13) -0.0001(11) 0.0017(11) C24 0.0564(18) 0.0600(18) 0.0566(17) -0.0150(15) 0.0041(14) 0.0211(15) C25 0.0297(12) 0.0299(12) 0.0563(15) 0.0061(11) 0.0176(11) 0.0067(10) C26 0.0319(13) 0.0385(14) 0.0617(16) 0.0147(13) -0.0103(12) 0.0007(11) C27 0.067(2) 0.080(2) 0.0398(15) 0.0035(15) 0.0002(14) 0.0055(17) C28 0.0263(12) 0.0260(11) 0.0626(16) -0.0060(11) 0.0106(11) 0.0082(9) C29 0.0262(12) 0.0354(12) 0.0444(13) -0.0139(11) 0.0088(10) 0.0076(10) C30 0.0474(16) 0.0661(18) 0.0353(13) -0.0192(13) 0.0065(12) 0.0259(14) C31 0.0334(15) 0.0648(19) 0.076(2) -0.0532(18) -0.0106(14) 0.0165(14) C32 0.0274(13) 0.0282(13) 0.111(3) -0.0321(15) 0.0187(15) 0.0002(11) C33 0.0688(19) 0.0347(14) 0.0376(14) 0.0020(11) -0.0219(13) -0.0219(13) C34 0.0393(15) 0.0559(17) 0.0509(15) -0.0348(14) 0.0187(12) -0.0206(13) C35 0.0438(15) 0.0223(12) 0.0649(18) -0.0148(12) -0.0131(13) 0.0019(11) C36 0.0576(17) 0.0440(15) 0.0415(14) -0.0070(12) 0.0112(13) -0.0310(14) C37 0.0186(12) 0.0427(15) 0.082(2) -0.0327(15) -0.0017(12) -0.0045(11) _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 C3 2.1724(19) . ? Ti1 C17 2.131(2) . ? Ti1 C28 2.378(2) . ? Ti1 C29 2.424(2) . ? Ti1 C30 2.398(2) . ? Ti1 C31 2.359(2) . ? Ti1 C32 2.361(2) . ? Ti1 C33 2.372(2) . ? Ti1 C34 2.368(2) . ? Ti1 C35 2.357(2) . ? Ti1 C36 2.347(2) . ? Ti1 C37 2.374(2) . ? N1 Si1 1.7484(17) . ? N1 C1 1.281(3) . ? Si1 C4 1.873(2) . ? Si1 C25 1.882(2) . ? Si1 C26 1.867(2) . ? C1 C2 1.500(3) . ? C1 C5 1.504(3) . ? C2 C3 1.481(3) . ? C2 C17 1.363(3) . ? C3 C4 1.364(3) . ? C4 C11 1.479(3) . ? C5 C6 1.386(3) . ? C5 C10 1.383(3) . ? C6 H6 0.9500 . ? C6 C7 1.391(3) . ? C7 H7 0.9500 . ? C7 C8 1.374(3) . ? C8 H8 0.9500 . ? C8 C9 1.382(3) . ? C9 H9 0.9500 . ? C9 C10 1.387(3) . ? C10 H10 0.9500 . ? C11 C12 1.394(3) . ? C11 C16 1.404(3) . ? C12 H12 0.9500 . ? C12 C13 1.387(3) . ? C13 H13 0.9500 . ? C13 C14 1.376(4) . ? C14 H14 0.9500 . ? C14 C15 1.374(4) . ? C15 H15 0.9500 . ? C15 C16 1.390(3) . ? C16 H16 0.9500 . ? C17 C18 1.461(3) . ? C18 C19 1.396(3) . ? C18 C23 1.400(3) . ? C19 H19 0.9500 . ? C19 C20 1.389(3) . ? C20 H20 0.9500 . ? C20 C21 1.377(4) . ? C21 H21 0.9500 . ? C21 C22 1.372(4) . ? C22 H22 0.9500 . ? C22 C23 1.381(4) . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C24 C25 1.518(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26 C27 1.484(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28 1.0000 . ? C28 C29 1.396(3) . ? C28 C32 1.408(3) . ? C29 H29 1.0000 . ? C29 C30 1.397(3) . ? C30 H30 1.0000 . ? C30 C31 1.405(4) . ? C31 H31 1.0000 . ? C31 C32 1.395(4) . ? C32 H32 1.0000 . ? C33 H33 1.0000 . ? C33 C34 1.397(4) . ? C33 C37 1.388(4) . ? C34 H34 1.0000 . ? C34 C35 1.363(4) . ? C35 H35 1.0000 . ? C35 C36 1.377(4) . ? C36 H36 1.0000 . ? C36 C37 1.379(4) . ? C37 H37 1.0000 . ? 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 C3 Ti1 C28 134.28(8) . . ? C3 Ti1 C29 134.23(7) . . ? C3 Ti1 C30 100.90(8) . . ? C3 Ti1 C31 81.72(8) . . ? C3 Ti1 C32 99.94(8) . . ? C3 Ti1 C33 123.35(9) . . ? C3 Ti1 C34 89.41(9) . . ? C3 Ti1 C35 79.41(8) . . ? C3 Ti1 C36 105.23(9) . . ? C3 Ti1 C37 135.69(8) . . ? C17 Ti1 C3 66.30(7) . . ? C17 Ti1 C28 96.47(8) . . ? C17 Ti1 C29 129.64(8) . . ? C17 Ti1 C30 129.43(10) . . ? C17 Ti1 C31 95.54(10) . . ? C17 Ti1 C32 76.64(9) . . ? C17 Ti1 C33 90.02(9) . . ? C17 Ti1 C34 79.02(8) . . ? C17 Ti1 C35 103.94(9) . . ? C17 Ti1 C36 134.95(9) . . ? C17 Ti1 C37 123.88(9) . . ? C28 Ti1 C29 33.78(8) . . ? C28 Ti1 C30 56.48(9) . . ? C30 Ti1 C29 33.66(8) . . ? C31 Ti1 C28 57.09(9) . . ? C31 Ti1 C29 56.55(8) . . ? C31 Ti1 C30 34.35(10) . . ? C31 Ti1 C32 34.36(11) . . ? C31 Ti1 C33 154.12(10) . . ? C31 Ti1 C34 170.92(9) . . ? C31 Ti1 C37 132.14(10) . . ? C32 Ti1 C28 34.57(8) . . ? C32 Ti1 C29 56.62(8) . . ? C32 Ti1 C30 56.87(11) . . ? C32 Ti1 C33 124.67(11) . . ? C32 Ti1 C34 147.60(12) . . ? C32 Ti1 C37 124.16(9) . . ? C33 Ti1 C28 97.21(10) . . ? C33 Ti1 C29 101.02(10) . . ? C33 Ti1 C30 131.17(11) . . ? C33 Ti1 C37 34.01(10) . . ? C34 Ti1 C28 130.35(10) . . ? C34 Ti1 C29 132.44(8) . . ? C34 Ti1 C30 151.53(10) . . ? C34 Ti1 C33 34.27(10) . . ? C34 Ti1 C37 56.44(9) . . ? C35 Ti1 C28 145.97(9) . . ? C35 Ti1 C29 123.18(9) . . ? C35 Ti1 C30 122.21(11) . . ? C35 Ti1 C31 144.44(12) . . ? C35 Ti1 C32 178.80(11) . . ? C35 Ti1 C33 56.46(9) . . ? C35 Ti1 C34 33.53(10) . . ? C35 Ti1 C37 56.43(9) . . ? C36 Ti1 C28 115.24(9) . . ? C36 Ti1 C29 89.17(9) . . ? C36 Ti1 C30 95.37(10) . . ? C36 Ti1 C31 128.09(11) . . ? C36 Ti1 C32 145.78(10) . . ? C36 Ti1 C33 56.50(9) . . ? C36 Ti1 C34 56.20(9) . . ? C36 Ti1 C35 34.04(9) . . ? C36 Ti1 C37 33.97(10) . . ? C37 Ti1 C28 89.59(8) . . ? C37 Ti1 C29 76.49(8) . . ? C37 Ti1 C30 99.90(10) . . ? C1 N1 Si1 121.65(14) . . ? N1 Si1 C4 105.72(9) . . ? N1 Si1 C25 107.09(10) . . ? N1 Si1 C26 106.62(10) . . ? C4 Si1 C25 112.45(10) . . ? C26 Si1 C4 116.00(11) . . ? C26 Si1 C25 108.42(11) . . ? N1 C1 C2 123.41(18) . . ? N1 C1 C5 118.43(17) . . ? C2 C1 C5 118.10(16) . . ? C1 C2 Ti1 170.68(14) . . ? C3 C2 Ti1 57.13(10) . . ? C3 C2 C1 120.88(16) . . ? C17 C2 Ti1 55.43(11) . . ? C17 C2 C1 127.46(18) . . ? C17 C2 C3 111.66(17) . . ? C2 C3 Ti1 87.95(11) . . ? C4 C3 Ti1 146.27(15) . . ? C4 C3 C2 123.76(18) . . ? C3 C4 Si1 115.68(15) . . ? C3 C4 C11 121.05(18) . . ? C11 C4 Si1 122.85(14) . . ? C6 C5 C1 119.09(18) . . ? C10 C5 C1 122.11(18) . . ? C10 C5 C6 118.77(19) . . ? C5 C6 H6 119.8 . . ? C5 C6 C7 120.4(2) . . ? C7 C6 H6 119.8 . . ? C6 C7 H7 119.9 . . ? C8 C7 C6 120.3(2) . . ? C8 C7 H7 119.9 . . ? C7 C8 H8 120.2 . . ? C7 C8 C9 119.7(2) . . ? C9 C8 H8 120.2 . . ? C8 C9 H9 120.0 . . ? C8 C9 C10 120.0(2) . . ? C10 C9 H9 120.0 . . ? C5 C10 C9 120.8(2) . . ? C5 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C12 C11 C4 121.48(19) . . ? C12 C11 C16 116.75(19) . . ? C16 C11 C4 121.74(19) . . ? C11 C12 H12 119.2 . . ? C13 C12 C11 121.7(2) . . ? C13 C12 H12 119.2 . . ? C12 C13 H13 119.8 . . ? C14 C13 C12 120.5(2) . . ? C14 C13 H13 119.8 . . ? C13 C14 H14 120.4 . . ? C15 C14 C13 119.2(2) . . ? C15 C14 H14 120.4 . . ? C14 C15 H15 119.6 . . ? C14 C15 C16 120.7(2) . . ? C16 C15 H15 119.6 . . ? C11 C16 H16 119.5 . . ? C15 C16 C11 121.0(2) . . ? C15 C16 H16 119.5 . . ? C2 C17 Ti1 92.80(13) . . ? C2 C17 C18 128.22(19) . . ? C18 C17 Ti1 138.76(14) . . ? C19 C18 C17 121.12(19) . . ? C19 C18 C23 117.2(2) . . ? C23 C18 C17 121.6(2) . . ? C18 C19 H19 119.4 . . ? C20 C19 C18 121.2(2) . . ? C20 C19 H19 119.4 . . ? C19 C20 H20 119.9 . . ? C21 C20 C19 120.2(3) . . ? C21 C20 H20 119.9 . . ? C20 C21 H21 120.3 . . ? C22 C21 C20 119.5(2) . . ? C22 C21 H21 120.3 . . ? C21 C22 H22 119.6 . . ? C21 C22 C23 120.8(2) . . ? C23 C22 H22 119.6 . . ? C18 C23 H23 119.5 . . ? C22 C23 C18 121.0(3) . . ? C22 C23 H23 119.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? Si1 C25 H25A 108.7 . . ? Si1 C25 H25B 108.7 . . ? C24 C25 Si1 114.14(17) . . ? C24 C25 H25A 108.7 . . ? C24 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? Si1 C26 H26A 108.4 . . ? Si1 C26 H26B 108.4 . . ? H26A C26 H26B 107.5 . . ? C27 C26 Si1 115.35(19) . . ? C27 C26 H26A 108.4 . . ? C27 C26 H26B 108.4 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Ti1 C28 H28 125.7 . . ? C29 C28 Ti1 74.94(13) . . ? C29 C28 H28 125.7 . . ? C29 C28 C32 108.1(2) . . ? C32 C28 Ti1 72.08(13) . . ? C32 C28 H28 125.7 . . ? Ti1 C29 H29 125.9 . . ? C28 C29 Ti1 71.28(12) . . ? C28 C29 H29 125.9 . . ? C28 C29 C30 108.1(2) . . ? C30 C29 Ti1 72.15(13) . . ? C30 C29 H29 125.9 . . ? Ti1 C30 H30 125.8 . . ? C29 C30 Ti1 74.19(13) . . ? C29 C30 H30 125.8 . . ? C29 C30 C31 108.0(3) . . ? C31 C30 Ti1 71.31(14) . . ? C31 C30 H30 125.8 . . ? Ti1 C31 H31 125.6 . . ? C30 C31 Ti1 74.34(14) . . ? C30 C31 H31 125.6 . . ? C32 C31 Ti1 72.90(14) . . ? C32 C31 C30 108.1(2) . . ? C32 C31 H31 125.6 . . ? Ti1 C32 H32 125.9 . . ? C28 C32 Ti1 73.35(13) . . ? C28 C32 H32 125.9 . . ? C31 C32 Ti1 72.74(15) . . ? C31 C32 C28 107.7(3) . . ? C31 C32 H32 125.9 . . ? Ti1 C33 H33 126.1 . . ? C34 C33 Ti1 72.72(13) . . ? C34 C33 H33 126.1 . . ? C37 C33 Ti1 73.09(14) . . ? C37 C33 H33 126.1 . . ? C37 C33 C34 107.3(2) . . ? Ti1 C34 H34 125.7 . . ? C33 C34 Ti1 73.01(14) . . ? C33 C34 H34 125.7 . . ? C35 C34 Ti1 72.79(14) . . ? C35 C34 C33 108.3(2) . . ? C35 C34 H34 125.7 . . ? Ti1 C35 H35 125.6 . . ? C34 C35 Ti1 73.67(14) . . ? C34 C35 H35 125.6 . . ? C34 C35 C36 108.3(2) . . ? C36 C35 Ti1 72.58(14) . . ? C36 C35 H35 125.6 . . ? Ti1 C36 H36 125.5 . . ? C35 C36 Ti1 73.38(14) . . ? C35 C36 H36 125.5 . . ? C35 C36 C37 108.5(2) . . ? C37 C36 Ti1 74.10(14) . . ? C37 C36 H36 125.5 . . ? Ti1 C37 H37 126.0 . . ? C33 C37 Ti1 72.90(13) . . ? C33 C37 H37 126.0 . . ? C36 C37 Ti1 71.93(13) . . ? C36 C37 C33 107.6(2) . . ? C36 C37 H37 126.0 . . ? _shelx_estimated_absorpt_T_max 0.965 _shelx_estimated_absorpt_T_min 0.932 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelxl_version_number 2013-3 #===end data_zhaoj _audit_creation_date 2012-10-29 _audit_creation_method ; Olex2 1.2 (compiled 2012.05.09 svn.r2324, GUI svn.r4230) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C35 H31 N Si Ti' _chemical_formula_sum 'C35 H31 N Si Ti' _chemical_formula_weight 541.60 _chemical_melting_point ? _chemical_oxdiff_formula C35H40NTiSi 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' _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 15.9762(8) _cell_length_b 11.2754(4) _cell_length_c 17.1936(9) _cell_angle_alpha 90.00 _cell_angle_beta 115.916(6) _cell_angle_gamma 90.00 _cell_volume 2785.8(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9991 _cell_measurement_temperature 99.98(11) _cell_measurement_theta_max 30.2688 _cell_measurement_theta_min 2.9009 _exptl_absorpt_coefficient_mu 0.375 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.64773 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'red' _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'block' _exptl_crystal_F_000 1136 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_unetI/netI 0.0362 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 23411 _diffrn_reflns_theta_full 25.02 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_min 2.91 _diffrn_ambient_temperature 99.98(11) _diffrn_detector_area_resol_mean 10.3914 _diffrn_measured_fraction_theta_full 0.9982 _diffrn_measured_fraction_theta_max 0.9822 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 1.00 86.00 1.0000 2.6000 omega____ theta____ kappa____ phi______ frames - 13.6191 77.0000 120.0000 85 #__ type_ start__ end____ width___ exp.time_ 2 omega -65.00 47.00 1.0000 2.6000 omega____ theta____ kappa____ phi______ frames - 13.6191 -77.0000 30.0000 112 #__ type_ start__ end____ width___ exp.time_ 3 omega 2.00 39.00 1.0000 2.6000 omega____ theta____ kappa____ phi______ frames - 13.6191 -38.0000 -120.0000 37 #__ type_ start__ end____ width___ exp.time_ 4 omega 34.00 100.00 1.0000 2.6000 omega____ theta____ kappa____ phi______ frames - 13.6191 -178.0000 30.0000 66 #__ type_ start__ end____ width___ exp.time_ 5 omega 1.00 29.00 1.0000 2.6000 omega____ theta____ kappa____ phi______ frames - 13.6191 38.0000 -90.0000 28 #__ type_ start__ end____ width___ exp.time_ 6 omega 47.00 89.00 1.0000 2.6000 omega____ theta____ kappa____ phi______ frames - 13.6191 38.0000 -90.0000 42 #__ type_ start__ end____ width___ exp.time_ 7 omega -18.00 20.00 1.0000 2.6000 omega____ theta____ kappa____ phi______ frames - -14.4003 -85.0000 163.0000 38 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0196563000 _diffrn_orient_matrix_UB_12 0.0079482000 _diffrn_orient_matrix_UB_13 -0.0295126000 _diffrn_orient_matrix_UB_21 0.0399582000 _diffrn_orient_matrix_UB_22 -0.0323793000 _diffrn_orient_matrix_UB_23 0.0279351000 _diffrn_orient_matrix_UB_31 -0.0213186000 _diffrn_orient_matrix_UB_32 -0.0532970000 _diffrn_orient_matrix_UB_33 -0.0213227000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'SuperNova (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4198 _reflns_number_total 4911 _reflns_odcompleteness_completeness 99.82 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 27.42 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'J. Appl. Cryst. (2007) 40, 786-790' _refine_diff_density_max 0.390 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.050 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 345 _refine_ls_number_reflns 4911 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0366 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+1.4439P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0913 _refine_ls_wR_factor_ref 0.0977 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap 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 0.30967(2) 0.97126(3) 0.61539(2) 0.02129(12) Uani 1 1 d . . . N1 N 0.20929(11) 0.84800(14) 0.31685(10) 0.0217(4) Uani 1 1 d . . . Si1 Si 0.23202(4) 0.99928(5) 0.31481(3) 0.01914(14) Uani 1 1 d . . . C1 C 0.17773(15) 1.0697(2) 0.61368(16) 0.0379(6) Uani 1 1 d . . . H1 H 0.1179 1.0315 0.6054 0.045 Uiso 1 1 calc R . . C2 C 0.19605(19) 1.1222(2) 0.54930(16) 0.0461(7) Uani 1 1 d . . . H2 H 0.1517 1.1261 0.4866 0.055 Uiso 1 1 calc R . . C3 C 0.28238(19) 1.1783(2) 0.58761(17) 0.0434(6) Uani 1 1 d . . . H3 H 0.3100 1.2297 0.5574 0.052 Uiso 1 1 calc R . . C4 C 0.31865(16) 1.1607(2) 0.67695(16) 0.0356(5) Uani 1 1 d . . . H4 H 0.3761 1.1985 0.7218 0.043 Uiso 1 1 calc R . . C5 C 0.25362(15) 1.0934(2) 0.69284(14) 0.0322(5) Uani 1 1 d . . . H5 H 0.2571 1.0754 0.7511 0.039 Uiso 1 1 calc R . . C6 C 0.36821(16) 0.8489(2) 0.74027(14) 0.0390(6) Uani 1 1 d . . . H6 H 0.3346 0.8278 0.7756 0.047 Uiso 1 1 calc R . . C7 C 0.43269(16) 0.9400(2) 0.75813(14) 0.0408(6) Uani 1 1 d . . . H7 H 0.4521 0.9968 0.8076 0.049 Uiso 1 1 calc R . . C8 C 0.47110(15) 0.9321(2) 0.69950(14) 0.0385(6) Uani 1 1 d . . . H8 H 0.5235 0.9816 0.7005 0.046 Uiso 1 1 calc R . . C9 C 0.43226(15) 0.8335(2) 0.64626(14) 0.0362(6) Uani 1 1 d . . . H9 H 0.4527 0.7999 0.6035 0.043 Uiso 1 1 calc R . . C10 C 0.36904(15) 0.7814(2) 0.67187(14) 0.0364(6) Uani 1 1 d . . . H10 H 0.3363 0.7041 0.6505 0.044 Uiso 1 1 calc R . . C11 C 0.20587(13) 0.85511(17) 0.52889(12) 0.0208(4) Uani 1 1 d . . . C12 C 0.23792(12) 0.87063(16) 0.46795(12) 0.0189(4) Uani 1 1 d . . . C13 C 0.30529(13) 0.96978(16) 0.48907(12) 0.0184(4) Uani 1 1 d . . . C14 C 0.31799(12) 1.03441(16) 0.42817(12) 0.0185(4) Uani 1 1 d . . . C15 C 0.21386(12) 0.80047(17) 0.38637(12) 0.0193(4) Uani 1 1 d . . . C16 C 0.12162(14) 1.0820(2) 0.28756(13) 0.0299(5) Uani 1 1 d . . . H16A H 0.0742 1.0554 0.2312 0.045 Uiso 1 1 calc R . . H16B H 0.1326 1.1671 0.2851 0.045 Uiso 1 1 calc R . . H16C H 0.1001 1.0669 0.3320 0.045 Uiso 1 1 calc R . . C17 C 0.27141(15) 1.02227(19) 0.22894(13) 0.0277(5) Uani 1 1 d . . . H17A H 0.3240 0.9696 0.2393 0.041 Uiso 1 1 calc R . . H17B H 0.2908 1.1049 0.2299 0.041 Uiso 1 1 calc R . . H17C H 0.2202 1.0044 0.1724 0.041 Uiso 1 1 calc R . . C18 C 0.12697(13) 0.78405(16) 0.52283(12) 0.0209(4) Uani 1 1 d . . . C19 C 0.12435(14) 0.73745(19) 0.59735(13) 0.0273(5) Uani 1 1 d . . . H19 H 0.1746 0.7524 0.6523 0.033 Uiso 1 1 calc R . . C20 C 0.04972(15) 0.67008(19) 0.59218(14) 0.0319(5) Uani 1 1 d . . . H20 H 0.0497 0.6381 0.6433 0.038 Uiso 1 1 calc R . . C21 C -0.02494(15) 0.64893(19) 0.51297(15) 0.0314(5) Uani 1 1 d . . . H21 H -0.0753 0.6007 0.5093 0.038 Uiso 1 1 calc R . . C22 C -0.02566(14) 0.69850(19) 0.43916(14) 0.0295(5) Uani 1 1 d . . . H22 H -0.0778 0.6866 0.3849 0.035 Uiso 1 1 calc R . . C23 C 0.04888(13) 0.76525(18) 0.44379(13) 0.0250(4) Uani 1 1 d . . . H23 H 0.0472 0.7990 0.3925 0.030 Uiso 1 1 calc R . . C24 C 0.38314(12) 1.13533(17) 0.45252(12) 0.0189(4) Uani 1 1 d . . . C25 C 0.36099(13) 1.24029(17) 0.40480(13) 0.0224(4) Uani 1 1 d . . . H25 H 0.3049 1.2448 0.3530 0.027 Uiso 1 1 calc R . . C26 C 0.41923(14) 1.33802(18) 0.43149(14) 0.0279(5) Uani 1 1 d . . . H26 H 0.4015 1.4097 0.3993 0.033 Uiso 1 1 calc R . . C27 C 0.50296(14) 1.33186(19) 0.50468(14) 0.0305(5) Uani 1 1 d . . . H27 H 0.5430 1.3989 0.5228 0.037 Uiso 1 1 calc R . . C28 C 0.52811(14) 1.22735(19) 0.55144(14) 0.0296(5) Uani 1 1 d . . . H28 H 0.5863 1.2219 0.6011 0.035 Uiso 1 1 calc R . . C29 C 0.46888(13) 1.13096(18) 0.52616(12) 0.0233(4) Uani 1 1 d . . . H29 H 0.4866 1.0601 0.5594 0.028 Uiso 1 1 calc R . . C30 C 0.20088(12) 0.66957(17) 0.38832(13) 0.0215(4) Uani 1 1 d . . . C31 C 0.25030(14) 0.60363(18) 0.46244(14) 0.0280(5) Uani 1 1 d . . . H31 H 0.2931 0.6423 0.5134 0.034 Uiso 1 1 calc R . . C32 C 0.23815(16) 0.48204(19) 0.46316(16) 0.0356(5) Uani 1 1 d . . . H32 H 0.2726 0.4379 0.5144 0.043 Uiso 1 1 calc R . . C33 C 0.17612(16) 0.42519(19) 0.38959(16) 0.0350(6) Uani 1 1 d . . . H33 H 0.1672 0.3420 0.3902 0.042 Uiso 1 1 calc R . . C34 C 0.12695(15) 0.48933(19) 0.31491(16) 0.0324(5) Uani 1 1 d . . . H34 H 0.0842 0.4500 0.2642 0.039 Uiso 1 1 calc R . . C35 C 0.13962(14) 0.61088(19) 0.31347(14) 0.0268(5) Uani 1 1 d . . . H35 H 0.1066 0.6542 0.2615 0.032 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 0.0255(2) 0.0217(2) 0.0164(2) -0.00092(14) 0.00890(16) 0.00209(14) N1 0.0250(8) 0.0214(9) 0.0189(8) -0.0001(7) 0.0097(7) -0.0055(7) Si1 0.0218(3) 0.0189(3) 0.0153(3) 0.0006(2) 0.0068(2) -0.0029(2) C1 0.0311(12) 0.0341(13) 0.0477(15) -0.0101(11) 0.0165(11) 0.0086(10) C2 0.0616(16) 0.0379(15) 0.0302(13) -0.0033(11) 0.0121(12) 0.0302(13) C3 0.0751(18) 0.0202(12) 0.0537(16) 0.0038(11) 0.0455(15) 0.0137(12) C4 0.0444(13) 0.0250(12) 0.0430(14) -0.0126(10) 0.0244(11) -0.0037(10) C5 0.0406(12) 0.0315(12) 0.0310(12) -0.0083(10) 0.0217(11) 0.0020(10) C6 0.0400(13) 0.0541(16) 0.0231(11) 0.0168(11) 0.0137(10) 0.0118(11) C7 0.0393(13) 0.0541(16) 0.0175(11) -0.0034(11) 0.0017(10) 0.0072(12) C8 0.0224(11) 0.0535(16) 0.0296(12) 0.0099(11) 0.0023(10) 0.0027(10) C9 0.0347(12) 0.0468(15) 0.0234(11) 0.0055(10) 0.0094(10) 0.0199(11) C10 0.0386(13) 0.0301(13) 0.0279(12) 0.0098(10) 0.0027(10) 0.0105(10) C11 0.0255(10) 0.0164(10) 0.0190(10) 0.0037(8) 0.0083(8) 0.0056(8) C12 0.0217(9) 0.0151(10) 0.0176(9) 0.0024(8) 0.0065(8) 0.0016(7) C13 0.0210(9) 0.0160(10) 0.0170(9) 0.0002(7) 0.0070(8) 0.0031(7) C14 0.0207(9) 0.0151(10) 0.0190(10) -0.0014(8) 0.0078(8) 0.0002(7) C15 0.0167(9) 0.0193(10) 0.0212(10) 0.0002(8) 0.0077(8) -0.0014(7) C16 0.0271(11) 0.0328(12) 0.0238(11) -0.0012(9) 0.0056(9) 0.0016(9) C17 0.0370(12) 0.0254(11) 0.0233(11) -0.0025(9) 0.0157(10) -0.0084(9) C18 0.0272(10) 0.0146(10) 0.0236(10) 0.0025(8) 0.0135(9) 0.0053(8) C19 0.0313(11) 0.0283(12) 0.0248(11) 0.0044(9) 0.0145(9) 0.0022(9) C20 0.0377(12) 0.0293(12) 0.0351(12) 0.0097(10) 0.0219(11) 0.0030(9) C21 0.0321(11) 0.0241(11) 0.0457(14) -0.0011(10) 0.0242(11) -0.0012(9) C22 0.0240(10) 0.0330(12) 0.0332(12) -0.0070(10) 0.0139(9) -0.0002(9) C23 0.0273(10) 0.0270(11) 0.0234(10) 0.0017(9) 0.0135(9) 0.0047(8) C24 0.0225(9) 0.0180(10) 0.0184(10) -0.0032(8) 0.0109(8) 0.0008(7) C25 0.0276(10) 0.0204(10) 0.0216(10) -0.0020(8) 0.0129(9) -0.0013(8) C26 0.0391(12) 0.0172(11) 0.0328(12) -0.0021(9) 0.0207(10) -0.0030(9) C27 0.0347(12) 0.0219(11) 0.0379(13) -0.0144(9) 0.0187(11) -0.0109(9) C28 0.0268(11) 0.0285(12) 0.0288(11) -0.0137(9) 0.0078(9) -0.0035(9) C29 0.0263(10) 0.0194(10) 0.0221(10) -0.0052(8) 0.0087(9) 0.0008(8) C30 0.0233(10) 0.0189(10) 0.0286(11) -0.0015(8) 0.0172(9) -0.0018(8) C31 0.0332(11) 0.0193(11) 0.0349(12) 0.0013(9) 0.0178(10) 0.0013(9) C32 0.0452(13) 0.0223(12) 0.0475(15) 0.0071(10) 0.0280(12) 0.0056(10) C33 0.0470(13) 0.0141(11) 0.0620(16) -0.0038(11) 0.0405(13) -0.0026(9) C34 0.0350(12) 0.0250(12) 0.0465(14) -0.0148(10) 0.0264(11) -0.0114(9) C35 0.0307(11) 0.0247(11) 0.0308(11) -0.0052(9) 0.0187(10) -0.0049(9) _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 C1 2.371(2) . ? Ti1 C2 2.383(2) . ? Ti1 C3 2.385(2) . ? Ti1 C4 2.360(2) . ? Ti1 C5 2.348(2) . ? Ti1 C6 2.374(2) . ? Ti1 C7 2.407(2) . ? Ti1 C8 2.383(2) . ? Ti1 C9 2.371(2) . ? Ti1 C10 2.371(2) . ? Ti1 C11 2.126(2) . ? Ti1 C13 2.1423(19) . ? N1 Si1 1.7475(17) . ? N1 C15 1.283(2) . ? Si1 C14 1.8714(19) . ? Si1 C16 1.865(2) . ? Si1 C17 1.859(2) . ? C1 H1 1.0000 . ? C1 C2 1.395(4) . ? C1 C5 1.397(3) . ? C2 H2 1.0000 . ? C2 C3 1.393(4) . ? C3 H3 1.0000 . ? C3 C4 1.399(3) . ? C4 H4 1.0000 . ? C4 C5 1.407(3) . ? C5 H5 1.0000 . ? C6 H6 1.0000 . ? C6 C7 1.391(4) . ? C6 C10 1.405(3) . ? C7 H7 1.0000 . ? C7 C8 1.393(3) . ? C8 H8 1.0000 . ? C8 C9 1.400(3) . ? C9 H9 1.0000 . ? C9 C10 1.396(3) . ? C10 H10 1.0000 . ? C11 C12 1.364(3) . ? C11 C18 1.458(3) . ? C12 C13 1.483(3) . ? C12 C15 1.507(3) . ? C13 C14 1.362(3) . ? C14 C24 1.474(3) . ? C15 C30 1.493(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.402(3) . ? C18 C23 1.402(3) . ? C19 H19 0.9500 . ? C19 C20 1.383(3) . ? C20 H20 0.9500 . ? C20 C21 1.384(3) . ? C21 H21 0.9500 . ? C21 C22 1.382(3) . ? C22 H22 0.9500 . ? C22 C23 1.381(3) . ? C23 H23 0.9500 . ? C24 C25 1.395(3) . ? C24 C29 1.402(3) . ? C25 H25 0.9500 . ? C25 C26 1.385(3) . ? C26 H26 0.9500 . ? C26 C27 1.381(3) . ? C27 H27 0.9500 . ? C27 C28 1.383(3) . ? C28 H28 0.9500 . ? C28 C29 1.381(3) . ? C29 H29 0.9500 . ? C30 C31 1.386(3) . ? C30 C35 1.397(3) . ? C31 H31 0.9500 . ? C31 C32 1.385(3) . ? C32 H32 0.9500 . ? C32 C33 1.377(3) . ? C33 H33 0.9500 . ? C33 C34 1.381(3) . ? C34 H34 0.9500 . ? C34 C35 1.387(3) . ? C35 H35 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 C1 Ti1 C2 34.12(9) . . ? C1 Ti1 C3 57.01(9) . . ? C1 Ti1 C6 106.26(9) . . ? C1 Ti1 C7 113.99(8) . . ? C1 Ti1 C8 144.58(9) . . ? C1 Ti1 C9 162.24(9) . . ? C2 Ti1 C3 33.98(9) . . ? C2 Ti1 C7 134.68(9) . . ? C3 Ti1 C7 110.12(9) . . ? C4 Ti1 C1 57.42(8) . . ? C4 Ti1 C2 56.75(8) . . ? C4 Ti1 C3 34.28(8) . . ? C4 Ti1 C6 101.41(9) . . ? C4 Ti1 C7 79.22(9) . . ? C4 Ti1 C8 93.34(9) . . ? C4 Ti1 C9 127.60(8) . . ? C4 Ti1 C10 134.30(8) . . ? C5 Ti1 C1 34.43(8) . . ? C5 Ti1 C2 56.76(8) . . ? C5 Ti1 C3 57.17(8) . . ? C5 Ti1 C4 34.77(8) . . ? C5 Ti1 C6 85.70(8) . . ? C5 Ti1 C7 81.46(8) . . ? C5 Ti1 C8 110.15(8) . . ? C5 Ti1 C9 137.70(8) . . ? C5 Ti1 C10 118.72(8) . . ? C6 Ti1 C2 139.76(9) . . ? C6 Ti1 C3 135.70(9) . . ? C6 Ti1 C7 33.81(8) . . ? C6 Ti1 C8 56.57(8) . . ? C8 Ti1 C2 144.94(10) . . ? C8 Ti1 C3 110.96(9) . . ? C8 Ti1 C7 33.82(8) . . ? C9 Ti1 C2 163.15(9) . . ? C9 Ti1 C3 138.33(9) . . ? C9 Ti1 C6 57.06(8) . . ? C9 Ti1 C7 56.58(8) . . ? C9 Ti1 C8 34.27(8) . . ? C10 Ti1 C1 128.47(9) . . ? C10 Ti1 C2 157.70(10) . . ? C10 Ti1 C3 166.28(9) . . ? C10 Ti1 C6 34.46(8) . . ? C10 Ti1 C7 56.48(8) . . ? C10 Ti1 C8 56.68(8) . . ? C10 Ti1 C9 34.23(8) . . ? C11 Ti1 C1 82.08(8) . . ? C11 Ti1 C2 84.71(8) . . ? C11 Ti1 C3 116.39(9) . . ? C11 Ti1 C4 138.34(8) . . ? C11 Ti1 C5 112.56(8) . . ? C11 Ti1 C6 98.80(8) . . ? C11 Ti1 C7 131.49(8) . . ? C11 Ti1 C8 128.07(8) . . ? C11 Ti1 C9 93.93(8) . . ? C11 Ti1 C10 77.32(7) . . ? C11 Ti1 C13 67.43(7) . . ? C13 Ti1 C1 110.86(8) . . ? C13 Ti1 C2 80.89(8) . . ? C13 Ti1 C3 83.25(8) . . ? C13 Ti1 C4 115.49(8) . . ? C13 Ti1 C5 136.72(8) . . ? C13 Ti1 C6 137.55(8) . . ? C13 Ti1 C7 133.06(8) . . ? C13 Ti1 C8 99.26(8) . . ? C13 Ti1 C9 83.09(7) . . ? C13 Ti1 C10 103.78(8) . . ? C15 N1 Si1 119.93(14) . . ? N1 Si1 C14 104.48(8) . . ? N1 Si1 C16 108.12(9) . . ? N1 Si1 C17 107.31(9) . . ? C16 Si1 C14 109.81(9) . . ? C17 Si1 C14 116.66(9) . . ? C17 Si1 C16 110.00(10) . . ? Ti1 C1 H1 126.1 . . ? C2 C1 Ti1 73.43(13) . . ? C2 C1 H1 126.1 . . ? C2 C1 C5 107.3(2) . . ? C5 C1 Ti1 71.88(12) . . ? C5 C1 H1 126.1 . . ? Ti1 C2 H2 125.4 . . ? C1 C2 Ti1 72.45(13) . . ? C1 C2 H2 125.4 . . ? C3 C2 Ti1 73.06(13) . . ? C3 C2 C1 109.0(2) . . ? C3 C2 H2 125.4 . . ? Ti1 C3 H3 126.0 . . ? C2 C3 Ti1 72.96(13) . . ? C2 C3 H3 126.0 . . ? C2 C3 C4 107.7(2) . . ? C4 C3 Ti1 71.90(13) . . ? C4 C3 H3 126.0 . . ? Ti1 C4 H4 125.9 . . ? C3 C4 Ti1 73.81(13) . . ? C3 C4 H4 125.9 . . ? C3 C4 C5 107.7(2) . . ? C5 C4 Ti1 72.13(12) . . ? C5 C4 H4 125.9 . . ? Ti1 C5 H5 125.6 . . ? C1 C5 Ti1 73.69(12) . . ? C1 C5 C4 108.3(2) . . ? C1 C5 H5 125.6 . . ? C4 C5 Ti1 73.10(12) . . ? C4 C5 H5 125.6 . . ? Ti1 C6 H6 125.7 . . ? C7 C6 Ti1 74.41(13) . . ? C7 C6 H6 125.7 . . ? C7 C6 C10 107.9(2) . . ? C10 C6 Ti1 72.65(12) . . ? C10 C6 H6 125.7 . . ? Ti1 C7 H7 125.8 . . ? C6 C7 Ti1 71.77(12) . . ? C6 C7 H7 125.8 . . ? C6 C7 C8 108.1(2) . . ? C8 C7 Ti1 72.14(12) . . ? C8 C7 H7 125.8 . . ? Ti1 C8 H8 125.6 . . ? C7 C8 Ti1 74.05(13) . . ? C7 C8 H8 125.6 . . ? C7 C8 C9 108.3(2) . . ? C9 C8 Ti1 72.40(12) . . ? C9 C8 H8 125.6 . . ? Ti1 C9 H9 125.9 . . ? C8 C9 Ti1 73.33(13) . . ? C8 C9 H9 125.9 . . ? C10 C9 Ti1 72.87(12) . . ? C10 C9 C8 107.6(2) . . ? C10 C9 H9 125.9 . . ? Ti1 C10 H10 125.8 . . ? C6 C10 Ti1 72.89(13) . . ? C6 C10 H10 125.8 . . ? C9 C10 Ti1 72.90(13) . . ? C9 C10 C6 108.0(2) . . ? C9 C10 H10 125.8 . . ? C12 C11 Ti1 91.05(12) . . ? C12 C11 C18 128.22(17) . . ? C18 C11 Ti1 140.70(14) . . ? C11 C12 C13 112.63(17) . . ? C11 C12 C15 128.27(17) . . ? C13 C12 C15 119.10(16) . . ? C12 C13 Ti1 87.29(11) . . ? C14 C13 Ti1 145.65(14) . . ? C14 C13 C12 123.46(17) . . ? C13 C14 Si1 113.54(14) . . ? C13 C14 C24 121.25(17) . . ? C24 C14 Si1 124.40(14) . . ? N1 C15 C12 122.40(17) . . ? N1 C15 C30 118.83(17) . . ? C30 C15 C12 118.66(16) . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si1 C17 H17A 109.5 . . ? Si1 C17 H17B 109.5 . . ? Si1 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C11 120.70(17) . . ? C23 C18 C11 121.83(17) . . ? C23 C18 C19 117.36(18) . . ? C18 C19 H19 119.5 . . ? C20 C19 C18 121.1(2) . . ? C20 C19 H19 119.5 . . ? C19 C20 H20 119.8 . . ? C19 C20 C21 120.4(2) . . ? C21 C20 H20 119.8 . . ? C20 C21 H21 120.3 . . ? C22 C21 C20 119.45(19) . . ? C22 C21 H21 120.3 . . ? C21 C22 H22 119.8 . . ? C23 C22 C21 120.4(2) . . ? C23 C22 H22 119.8 . . ? C18 C23 H23 119.4 . . ? C22 C23 C18 121.18(19) . . ? C22 C23 H23 119.4 . . ? C25 C24 C14 121.46(17) . . ? C25 C24 C29 117.23(17) . . ? C29 C24 C14 121.29(17) . . ? C24 C25 H25 119.4 . . ? C26 C25 C24 121.29(18) . . ? C26 C25 H25 119.4 . . ? C25 C26 H26 119.8 . . ? C27 C26 C25 120.33(19) . . ? C27 C26 H26 119.8 . . ? C26 C27 H27 120.3 . . ? C26 C27 C28 119.48(19) . . ? C28 C27 H27 120.3 . . ? C27 C28 H28 119.9 . . ? C29 C28 C27 120.17(19) . . ? C29 C28 H28 119.9 . . ? C24 C29 H29 119.3 . . ? C28 C29 C24 121.42(19) . . ? C28 C29 H29 119.3 . . ? C31 C30 C15 121.48(17) . . ? C31 C30 C35 118.77(19) . . ? C35 C30 C15 119.73(18) . . ? C30 C31 H31 119.6 . . ? C32 C31 C30 120.9(2) . . ? C32 C31 H31 119.6 . . ? C31 C32 H32 120.0 . . ? C33 C32 C31 120.0(2) . . ? C33 C32 H32 120.0 . . ? C32 C33 H33 120.0 . . ? C32 C33 C34 119.9(2) . . ? C34 C33 H33 120.0 . . ? C33 C34 H34 119.8 . . ? C33 C34 C35 120.4(2) . . ? C35 C34 H34 119.8 . . ? C30 C35 H35 120.0 . . ? C34 C35 C30 120.0(2) . . ? C34 C35 H35 120.0 . . ? #===end data_13sep06b _audit_creation_date 2013-11-21 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C45 H35 N Si Ti, C4 H4 O' _chemical_formula_sum 'C49 H43 N O Si Ti' _chemical_formula_weight 737.83 _chemical_melting_point ? _chemical_oxdiff_formula 'C46 H17 N1 Si1 Ti1' 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'monoclinic' _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_operation_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 16.2653(6) _cell_length_b 19.3916(6) _cell_length_c 24.7760(8) _cell_angle_alpha 90 _cell_angle_beta 104.915(3) _cell_angle_gamma 90 _cell_volume 7551.3(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 7532 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 29.1200 _cell_measurement_theta_min 3.3210 _exptl_absorpt_coefficient_mu 0.298 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.94514 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour '' _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description '' _exptl_crystal_F_000 3104 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_unetI/netI 0.0334 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 14417 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.019 _diffrn_reflns_theta_min 3.275 _diffrn_ambient_temperature 180.15 _diffrn_detector_area_resol_mean 10.3914 _diffrn_measured_fraction_theta_full 0.9923 _diffrn_measured_fraction_theta_max 0.8206 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 35.00 99.00 1.0000 13.0000 omega____ theta____ kappa____ phi______ frames - 10.7017 178.0000 -90.0000 64 #__ type_ start__ end____ width___ exp.time_ 2 omega -60.00 36.00 1.0000 13.0000 omega____ theta____ kappa____ phi______ frames - 10.7017 -57.0000 60.0000 96 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0389917000 _diffrn_orient_matrix_UB_12 0.0184292000 _diffrn_orient_matrix_UB_13 0.0071018000 _diffrn_orient_matrix_UB_21 -0.0054069000 _diffrn_orient_matrix_UB_22 0.0086510000 _diffrn_orient_matrix_UB_23 -0.0285048000 _diffrn_orient_matrix_UB_31 -0.0221227000 _diffrn_orient_matrix_UB_32 0.0303881000 _diffrn_orient_matrix_UB_33 0.0038191000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6208 _reflns_number_total 7392 _reflns_odcompleteness_completeness 99.23 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 25.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790' _refine_diff_density_max 0.692 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.056 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 487 _refine_ls_number_reflns 7392 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0469 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+16.5480P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1209 _refine_ls_wR_factor_ref 0.1291 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Restrained distances O1-C48 1.48 with sigma of 0.01 O1-C49 1.48 with sigma of 0.01 O1A-C48 1.48 with sigma of 0.01 O1A-C48 1.48 with sigma of 0.01 3. Others Fixed Sof: O1(0.5) O1A(0.5) 4.a Ternary CH refined with riding coordinates: C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45) 4.b Secondary CH2 refined with riding coordinates: C46(H46A,H46B), C47(H47A,H47B) 4.c Aromatic/amide H refined with riding coordinates: C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.76032(2) 0.83555(2) 0.75600(2) 0.01927(12) Uani 1 1 d . . . . . N1 N 0.76735(12) 0.59110(9) 0.70620(7) 0.0238(4) Uani 1 1 d . . . . . O1 O 0.3212(7) 0.5855(4) 0.4950(3) 0.141(4) Uani 0.5 1 d D . P A 1 Si1 Si 0.69113(4) 0.62258(3) 0.64845(2) 0.02150(15) Uani 1 1 d . . . . . C1 C 0.80306(14) 0.62781(11) 0.74897(9) 0.0215(4) Uani 1 1 d . . . . . C2 C 0.79335(13) 0.70412(11) 0.75150(8) 0.0203(4) Uani 1 1 d . . . . . C3 C 0.84081(14) 0.75027(11) 0.78827(8) 0.0212(4) Uani 1 1 d . . . . . C4 C 0.72501(13) 0.74086(11) 0.71052(9) 0.0204(4) Uani 1 1 d . . . . . C5 C 0.67473(13) 0.71502(11) 0.66259(9) 0.0208(4) Uani 1 1 d . . . . . C6 C 0.85344(15) 0.59052(11) 0.79965(9) 0.0255(5) Uani 1 1 d . . . . . C7 C 0.91388(16) 0.54184(12) 0.79503(11) 0.0341(6) Uani 1 1 d . . . . . H7 H 0.9246 0.5333 0.7597 0.041 Uiso 1 1 calc R U . . . C8 C 0.95866(18) 0.50566(14) 0.84161(13) 0.0473(8) Uani 1 1 d . . . . . H8 H 1.0010 0.4733 0.8383 0.057 Uiso 1 1 calc R U . . . C9 C 0.9421(2) 0.51645(15) 0.89232(13) 0.0520(9) Uani 1 1 d . . . . . H9 H 0.9720 0.4909 0.9240 0.062 Uiso 1 1 calc R U . . . C10 C 0.8823(2) 0.56406(15) 0.89753(11) 0.0466(7) Uani 1 1 d . . . . . H10 H 0.8712 0.5714 0.9329 0.056 Uiso 1 1 calc R U . . . C11 C 0.83776(17) 0.60171(13) 0.85134(10) 0.0333(6) Uani 1 1 d . . . . . H11 H 0.7968 0.6349 0.8553 0.040 Uiso 1 1 calc R U . . . C12 C 0.92285(14) 0.74303(11) 0.82955(9) 0.0226(5) Uani 1 1 d . . . . . C13 C 0.98839(15) 0.70362(13) 0.81852(10) 0.0288(5) Uani 1 1 d . . . . . H13 H 0.9779 0.6783 0.7846 0.035 Uiso 1 1 calc R U . . . C14 C 1.06798(16) 0.70034(14) 0.85537(11) 0.0362(6) Uani 1 1 d . . . . . H14 H 1.1116 0.6736 0.8464 0.043 Uiso 1 1 calc R U . . . C15 C 1.08418(17) 0.73559(15) 0.90493(11) 0.0401(6) Uani 1 1 d . . . . . H15 H 1.1385 0.7327 0.9308 0.048 Uiso 1 1 calc R U . . . C16 C 1.02092(19) 0.77523(15) 0.91691(11) 0.0442(7) Uani 1 1 d . . . . . H16 H 1.0317 0.7996 0.9513 0.053 Uiso 1 1 calc R U . . . C17 C 0.94152(17) 0.77996(14) 0.87923(10) 0.0362(6) Uani 1 1 d . . . . . H17 H 0.8993 0.8089 0.8876 0.043 Uiso 1 1 calc R U . . . C18 C 0.72793(14) 0.60269(11) 0.58423(9) 0.0244(5) Uani 1 1 d . . . . . C19 C 0.67906(16) 0.62279(13) 0.53158(10) 0.0306(5) Uani 1 1 d . . . . . H19 H 0.6276 0.6474 0.5287 0.037 Uiso 1 1 calc R U . . . C20 C 0.70387(17) 0.60767(14) 0.48341(10) 0.0353(6) Uani 1 1 d . . . . . H20 H 0.6701 0.6227 0.4481 0.042 Uiso 1 1 calc R U . . . C21 C 0.77700(18) 0.57117(15) 0.48658(11) 0.0414(6) Uani 1 1 d . . . . . H21 H 0.7941 0.5606 0.4536 0.050 Uiso 1 1 calc R U . . . C22 C 0.82575(19) 0.54987(17) 0.53806(12) 0.0475(7) Uani 1 1 d . . . . . H22 H 0.8765 0.5244 0.5404 0.057 Uiso 1 1 calc R U . . . C23 C 0.80148(16) 0.56521(14) 0.58637(10) 0.0347(6) Uani 1 1 d . . . . . H23 H 0.8356 0.5499 0.6214 0.042 Uiso 1 1 calc R U . . . C24 C 0.59141(15) 0.57172(12) 0.64287(9) 0.0272(5) Uani 1 1 d . . . . . C25 C 0.53727(18) 0.58660(14) 0.67634(11) 0.0391(6) Uani 1 1 d . . . . . H25 H 0.5505 0.6241 0.7018 0.047 Uiso 1 1 calc R U . . . C26 C 0.46428(19) 0.54821(17) 0.67361(12) 0.0482(7) Uani 1 1 d . . . . . H26 H 0.4283 0.5597 0.6970 0.058 Uiso 1 1 calc R U . . . C27 C 0.44378(18) 0.49374(16) 0.63723(12) 0.0453(7) Uani 1 1 d . . . . . H27 H 0.3937 0.4676 0.6352 0.054 Uiso 1 1 calc R U . . . C28 C 0.49641(19) 0.47739(15) 0.60383(12) 0.0459(7) Uani 1 1 d . . . . . H28 H 0.4828 0.4397 0.5786 0.055 Uiso 1 1 calc R U . . . C29 C 0.56961(17) 0.51575(13) 0.60674(11) 0.0361(6) Uani 1 1 d . . . . . H29 H 0.6056 0.5035 0.5836 0.043 Uiso 1 1 calc R U . . . C30 C 0.60905(14) 0.75987(11) 0.62558(9) 0.0222(4) Uani 1 1 d . . . . . C31 C 0.53652(15) 0.77991(13) 0.64150(10) 0.0293(5) Uani 1 1 d . . . . . H31 H 0.5284 0.7641 0.6760 0.035 Uiso 1 1 calc R U . . . C32 C 0.47574(16) 0.82264(14) 0.60789(11) 0.0353(6) Uani 1 1 d . . . . . H32 H 0.4269 0.8360 0.6197 0.042 Uiso 1 1 calc R U . . . C33 C 0.48618(16) 0.84573(13) 0.55730(10) 0.0348(6) Uani 1 1 d . . . . . H33 H 0.4446 0.8747 0.5342 0.042 Uiso 1 1 calc R U . . . C34 C 0.55761(17) 0.82637(13) 0.54065(10) 0.0331(6) Uani 1 1 d . . . . . H34 H 0.5653 0.8422 0.5060 0.040 Uiso 1 1 calc R U . . . C35 C 0.61809(15) 0.78382(12) 0.57440(9) 0.0279(5) Uani 1 1 d . . . . . H35 H 0.6668 0.7707 0.5623 0.033 Uiso 1 1 calc R U . . . C36 C 0.80080(16) 0.85752(13) 0.67305(10) 0.0306(5) Uani 1 1 d . . . . . H36 H 0.7851 0.8290 0.6383 0.037 Uiso 1 1 calc R U . . . C37 C 0.87599(15) 0.85213(12) 0.71533(11) 0.0301(5) Uani 1 1 d . . . . . H37 H 0.9230 0.8185 0.7164 0.036 Uiso 1 1 calc R U . . . C38 C 0.87812(17) 0.90628(13) 0.75262(10) 0.0346(6) Uani 1 1 d . . . . . H38 H 0.9269 0.9179 0.7851 0.041 Uiso 1 1 calc R U . . . C39 C 0.80518(18) 0.94577(13) 0.73341(12) 0.0384(6) Uani 1 1 d . . . . . H39 H 0.7928 0.9907 0.7495 0.046 Uiso 1 1 calc R U . . . C40 C 0.75633(16) 0.91524(14) 0.68444(11) 0.0366(6) Uani 1 1 d . . . . . H40 H 0.7038 0.9352 0.6590 0.044 Uiso 1 1 calc R U . . . C41 C 0.64524(16) 0.79788(14) 0.79064(11) 0.0337(6) Uani 1 1 d . . . . . H41 H 0.6112 0.7549 0.7792 0.040 Uiso 1 1 calc R U . . . C42 C 0.71641(17) 0.80469(13) 0.83692(10) 0.0330(6) Uani 1 1 d . . . . . H42 H 0.7417 0.7673 0.8639 0.040 Uiso 1 1 calc R U . . . C43 C 0.73918(16) 0.87483(13) 0.84202(10) 0.0318(5) Uani 1 1 d . . . . . H43 H 0.7838 0.8957 0.8733 0.038 Uiso 1 1 calc R U . . . C44 C 0.68129(16) 0.91163(13) 0.80010(10) 0.0317(5) Uani 1 1 d . . . . . H44 H 0.6782 0.9629 0.7961 0.038 Uiso 1 1 calc R U . . . C45 C 0.62424(15) 0.86433(14) 0.76791(10) 0.0327(6) Uani 1 1 d . . . . . H45 H 0.5729 0.8762 0.7373 0.039 Uiso 1 1 calc R U . . . C46 C 0.4042(4) 0.6695(4) 0.5234(3) 0.147(3) Uani 1 1 d . . . . . H46A H 0.4216 0.7161 0.5144 0.176 Uiso 1 1 calc R U . . . H46B H 0.4557 0.6449 0.5448 0.176 Uiso 1 1 calc R U . . . C47 C 0.3435(4) 0.6758(4) 0.5580(3) 0.133(2) Uani 1 1 d . . . . . H47A H 0.3718 0.6665 0.5978 0.160 Uiso 1 1 calc R U . . . H47B H 0.3184 0.7226 0.5548 0.160 Uiso 1 1 calc R U . . . C48 C 0.3695(3) 0.6344(2) 0.47485(17) 0.0683(12) Uani 1 1 d D . . . . C49 C 0.2808(4) 0.6259(4) 0.5366(2) 0.150(3) Uani 1 1 d D . . . . O1A O 0.2842(6) 0.6476(13) 0.4826(6) 0.47(2) Uani 0.5 1 d D . P A 2 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 0.0214(2) 0.0169(2) 0.0194(2) -0.00102(15) 0.00499(15) -0.00049(15) N1 0.0274(10) 0.0189(9) 0.0228(9) 0.0001(7) 0.0023(8) -0.0031(8) O1 0.278(12) 0.111(6) 0.055(4) -0.021(4) 0.081(6) -0.094(7) Si1 0.0243(3) 0.0188(3) 0.0191(3) -0.0008(2) 0.0013(2) -0.0045(2) C1 0.0218(11) 0.0205(11) 0.0214(10) 0.0003(9) 0.0042(8) -0.0020(9) C2 0.0219(11) 0.0195(10) 0.0190(10) 0.0005(8) 0.0042(8) -0.0010(8) C3 0.0260(11) 0.0191(10) 0.0187(10) 0.0006(8) 0.0058(8) -0.0015(9) C4 0.0199(10) 0.0204(10) 0.0210(10) 0.0011(8) 0.0058(8) -0.0026(8) C5 0.0205(10) 0.0201(10) 0.0205(10) 0.0014(8) 0.0029(8) -0.0034(8) C6 0.0274(12) 0.0177(10) 0.0267(11) 0.0021(9) -0.0017(9) -0.0061(9) C7 0.0300(13) 0.0247(12) 0.0412(14) 0.0000(11) -0.0026(11) -0.0013(10) C8 0.0357(15) 0.0272(13) 0.064(2) 0.0067(13) -0.0140(13) 0.0009(12) C9 0.0540(18) 0.0351(15) 0.0468(17) 0.0189(13) -0.0235(14) -0.0103(14) C10 0.0605(19) 0.0424(16) 0.0277(13) 0.0099(12) -0.0053(12) -0.0172(15) C11 0.0405(14) 0.0293(13) 0.0269(12) 0.0043(10) 0.0031(10) -0.0081(11) C12 0.0261(11) 0.0174(10) 0.0218(10) 0.0023(9) 0.0016(9) -0.0040(9) C13 0.0285(12) 0.0304(12) 0.0276(11) -0.0004(10) 0.0073(9) -0.0035(10) C14 0.0269(13) 0.0405(15) 0.0403(14) 0.0078(12) 0.0072(11) 0.0011(11) C15 0.0308(14) 0.0436(15) 0.0361(14) 0.0098(12) -0.0091(11) -0.0045(12) C16 0.0463(16) 0.0458(16) 0.0285(13) -0.0092(12) -0.0118(11) 0.0026(13) C17 0.0387(14) 0.0336(13) 0.0296(13) -0.0083(11) -0.0037(10) 0.0063(11) C18 0.0270(12) 0.0212(11) 0.0232(11) -0.0022(9) 0.0032(9) -0.0061(9) C19 0.0329(13) 0.0317(13) 0.0253(11) -0.0007(10) 0.0041(10) 0.0001(10) C20 0.0441(15) 0.0366(14) 0.0227(12) 0.0000(10) 0.0040(10) -0.0052(12) C21 0.0471(16) 0.0492(17) 0.0318(13) -0.0050(12) 0.0172(12) -0.0048(13) C22 0.0374(15) 0.062(2) 0.0448(16) -0.0044(14) 0.0140(12) 0.0113(14) C23 0.0328(13) 0.0382(14) 0.0298(12) -0.0003(11) 0.0024(10) 0.0041(11) C24 0.0290(12) 0.0247(11) 0.0244(11) 0.0037(9) 0.0009(9) -0.0067(10) C25 0.0446(16) 0.0401(15) 0.0346(14) -0.0063(12) 0.0138(12) -0.0169(12) C26 0.0451(17) 0.0598(19) 0.0442(15) 0.0018(14) 0.0199(13) -0.0189(15) C27 0.0404(15) 0.0482(17) 0.0435(15) 0.0073(13) 0.0042(12) -0.0227(13) C28 0.0470(17) 0.0365(15) 0.0483(16) -0.0075(13) 0.0018(13) -0.0205(13) C29 0.0371(14) 0.0297(13) 0.0396(14) -0.0059(11) 0.0062(11) -0.0114(11) C30 0.0229(11) 0.0203(10) 0.0204(10) -0.0019(9) 0.0002(8) -0.0053(9) C31 0.0273(12) 0.0339(13) 0.0250(11) 0.0016(10) 0.0038(9) -0.0013(10) C32 0.0262(12) 0.0410(14) 0.0362(13) -0.0021(11) 0.0035(10) 0.0038(11) C33 0.0310(13) 0.0338(13) 0.0320(13) 0.0032(11) -0.0058(10) 0.0027(11) C34 0.0374(14) 0.0333(13) 0.0248(12) 0.0056(10) 0.0010(10) -0.0038(11) C35 0.0273(12) 0.0283(12) 0.0273(11) 0.0018(10) 0.0058(9) -0.0020(10) C36 0.0400(14) 0.0312(13) 0.0240(11) -0.0019(10) 0.0143(10) -0.0122(11) C37 0.0279(12) 0.0230(11) 0.0441(14) 0.0076(10) 0.0180(11) 0.0004(10) C38 0.0356(14) 0.0359(14) 0.0309(12) -0.0005(11) 0.0062(10) -0.0167(11) C39 0.0550(17) 0.0173(11) 0.0533(16) -0.0021(11) 0.0327(14) -0.0037(11) C40 0.0310(13) 0.0388(14) 0.0408(14) 0.0210(12) 0.0109(11) 0.0054(11) C41 0.0343(13) 0.0350(14) 0.0384(13) -0.0062(11) 0.0213(11) -0.0062(11) C42 0.0432(15) 0.0348(13) 0.0261(12) 0.0025(10) 0.0181(11) 0.0036(11) C43 0.0363(13) 0.0363(14) 0.0250(12) -0.0068(10) 0.0120(10) 0.0028(11) C44 0.0356(13) 0.0290(13) 0.0344(13) -0.0043(10) 0.0161(11) 0.0044(10) C45 0.0245(12) 0.0416(14) 0.0337(13) -0.0028(11) 0.0106(10) 0.0062(11) C46 0.088(4) 0.203(7) 0.156(6) -0.119(5) 0.044(4) -0.044(4) C47 0.153(6) 0.135(5) 0.124(5) -0.071(4) 0.057(4) -0.047(4) C48 0.098(3) 0.066(2) 0.0425(19) -0.0118(17) 0.022(2) -0.040(2) C49 0.117(5) 0.245(8) 0.084(4) 0.009(5) 0.017(3) -0.107(5) O1A 0.76(6) 0.35(3) 0.132(13) 0.042(16) -0.19(2) -0.09(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 C3 2.133(2) . ? Ti1 C4 2.154(2) . ? Ti1 C36 2.353(2) . ? Ti1 C37 2.374(2) . ? Ti1 C38 2.375(2) . ? Ti1 C39 2.372(2) . ? Ti1 C40 2.340(2) . ? Ti1 C41 2.366(2) . ? Ti1 C42 2.372(2) . ? Ti1 C43 2.370(2) . ? Ti1 C44 2.397(2) . ? Ti1 C45 2.374(2) . ? N1 Si1 1.7446(19) . ? N1 C1 1.285(3) . ? O1 C48 1.403(6) . ? O1 C49 1.567(8) . ? Si1 C5 1.859(2) . ? Si1 C18 1.879(2) . ? Si1 C24 1.873(2) . ? C1 C2 1.491(3) . ? C1 C6 1.497(3) . ? C2 C3 1.366(3) . ? C2 C4 1.481(3) . ? C3 C12 1.464(3) . ? C4 C5 1.353(3) . ? C5 C30 1.495(3) . ? C6 C7 1.389(3) . ? C6 C11 1.386(3) . ? C7 H7 0.9500 . ? C7 C8 1.387(4) . ? C8 H8 0.9500 . ? C8 C9 1.367(5) . ? C9 H9 0.9500 . ? C9 C10 1.371(5) . ? C10 H10 0.9500 . ? C10 C11 1.393(4) . ? C11 H11 0.9500 . ? C12 C13 1.395(3) . ? C12 C17 1.389(3) . ? C13 H13 0.9500 . ? C13 C14 1.380(3) . ? C14 H14 0.9500 . ? C14 C15 1.371(4) . ? C15 H15 0.9500 . ? C15 C16 1.377(4) . ? C16 H16 0.9500 . ? C16 C17 1.388(4) . ? C17 H17 0.9500 . ? C18 C19 1.397(3) . ? C18 C23 1.389(3) . ? C19 H19 0.9500 . ? C19 C20 1.386(3) . ? C20 H20 0.9500 . ? C20 C21 1.369(4) . ? C21 H21 0.9500 . ? C21 C22 1.380(4) . ? C22 H22 0.9500 . ? C22 C23 1.386(4) . ? C23 H23 0.9500 . ? C24 C25 1.387(4) . ? C24 C29 1.393(3) . ? C25 H25 0.9500 . ? C25 C26 1.388(4) . ? C26 H26 0.9500 . ? C26 C27 1.373(4) . ? C27 H27 0.9500 . ? C27 C28 1.372(4) . ? C28 H28 0.9500 . ? C28 C29 1.390(4) . ? C29 H29 0.9500 . ? C30 C31 1.392(3) . ? C30 C35 1.393(3) . ? C31 H31 0.9500 . ? C31 C32 1.391(3) . ? C32 H32 0.9500 . ? C32 C33 1.382(4) . ? C33 H33 0.9500 . ? C33 C34 1.381(4) . ? C34 H34 0.9500 . ? C34 C35 1.387(3) . ? C35 H35 0.9500 . ? C36 H36 1.0000 . ? C36 C37 1.395(4) . ? C36 C40 1.400(4) . ? C37 H37 1.0000 . ? C37 C38 1.393(4) . ? C38 H38 1.0000 . ? C38 C39 1.389(4) . ? C39 H39 1.0000 . ? C39 C40 1.399(4) . ? C40 H40 1.0000 . ? C41 H41 1.0000 . ? C41 C42 1.410(4) . ? C41 C45 1.412(4) . ? C42 H42 1.0000 . ? C42 C43 1.407(4) . ? C43 H43 1.0000 . ? C43 C44 1.404(4) . ? C44 H44 1.0000 . ? C44 C45 1.399(4) . ? C45 H45 1.0000 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C46 C47 1.469(8) . ? C46 C48 1.372(6) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C47 C49 1.408(7) . ? C48 O1A 1.472(7) . ? C49 O1A 1.417(16) . ? 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 C3 Ti1 C4 65.81(8) . . ? C3 Ti1 C36 100.66(9) . . ? C3 Ti1 C37 77.70(8) . . ? C3 Ti1 C38 92.18(9) . . ? C3 Ti1 C39 126.21(9) . . ? C3 Ti1 C40 133.68(9) . . ? C3 Ti1 C41 95.23(9) . . ? C3 Ti1 C42 77.11(8) . . ? C3 Ti1 C43 97.43(8) . . ? C3 Ti1 C44 130.98(8) . . ? C3 Ti1 C45 129.63(9) . . ? C4 Ti1 C36 78.13(8) . . ? C4 Ti1 C37 91.56(8) . . ? C4 Ti1 C38 125.65(9) . . ? C4 Ti1 C39 134.57(9) . . ? C4 Ti1 C40 102.41(9) . . ? C4 Ti1 C41 78.30(8) . . ? C4 Ti1 C42 97.43(8) . . ? C4 Ti1 C43 131.58(9) . . ? C4 Ti1 C44 131.39(9) . . ? C4 Ti1 C45 97.69(9) . . ? C36 Ti1 C37 34.32(9) . . ? C36 Ti1 C38 56.97(9) . . ? C36 Ti1 C39 57.20(9) . . ? C36 Ti1 C41 142.93(9) . . ? C36 Ti1 C42 175.56(9) . . ? C36 Ti1 C43 149.91(9) . . ? C36 Ti1 C44 126.17(9) . . ? C36 Ti1 C45 123.06(9) . . ? C37 Ti1 C38 34.12(9) . . ? C37 Ti1 C44 133.37(9) . . ? C37 Ti1 C45 152.54(9) . . ? C38 Ti1 C44 101.11(9) . . ? C39 Ti1 C37 56.78(8) . . ? C39 Ti1 C38 34.03(10) . . ? C39 Ti1 C42 127.22(9) . . ? C39 Ti1 C43 92.71(9) . . ? C39 Ti1 C44 77.68(9) . . ? C39 Ti1 C45 99.84(9) . . ? C40 Ti1 C36 34.72(9) . . ? C40 Ti1 C37 57.28(9) . . ? C40 Ti1 C38 57.13(9) . . ? C40 Ti1 C39 34.54(10) . . ? C40 Ti1 C41 127.46(9) . . ? C40 Ti1 C42 148.36(9) . . ? C40 Ti1 C43 119.13(9) . . ? C40 Ti1 C44 91.45(9) . . ? C40 Ti1 C45 95.39(9) . . ? C41 Ti1 C37 169.44(9) . . ? C41 Ti1 C38 155.72(9) . . ? C41 Ti1 C39 133.15(9) . . ? C41 Ti1 C42 34.63(9) . . ? C41 Ti1 C43 57.44(9) . . ? C41 Ti1 C44 57.16(9) . . ? C41 Ti1 C45 34.67(9) . . ? C42 Ti1 C37 146.83(9) . . ? C42 Ti1 C38 126.63(9) . . ? C42 Ti1 C44 57.08(9) . . ? C42 Ti1 C45 57.38(9) . . ? C43 Ti1 C37 130.73(9) . . ? C43 Ti1 C38 98.69(9) . . ? C43 Ti1 C42 34.52(9) . . ? C43 Ti1 C44 34.25(9) . . ? C43 Ti1 C45 57.11(9) . . ? C45 Ti1 C38 130.93(10) . . ? C45 Ti1 C44 34.11(9) . . ? C1 N1 Si1 123.89(16) . . ? C48 O1 C49 105.3(5) . . ? N1 Si1 C5 106.80(9) . . ? N1 Si1 C18 107.98(10) . . ? N1 Si1 C24 107.18(10) . . ? C5 Si1 C18 116.75(10) . . ? C5 Si1 C24 111.00(11) . . ? C24 Si1 C18 106.74(10) . . ? N1 C1 C2 123.67(19) . . ? N1 C1 C6 117.25(19) . . ? C2 C1 C6 119.01(18) . . ? C1 C2 Ti1 174.19(15) . . ? C3 C2 Ti1 54.50(12) . . ? C3 C2 C1 129.1(2) . . ? C3 C2 C4 109.74(19) . . ? C4 C2 Ti1 55.51(11) . . ? C4 C2 C1 121.16(18) . . ? C2 C3 Ti1 94.08(14) . . ? C2 C3 C12 131.3(2) . . ? C12 C3 Ti1 134.21(15) . . ? C2 C4 Ti1 89.97(13) . . ? C5 C4 Ti1 142.62(17) . . ? C5 C4 C2 126.9(2) . . ? C4 C5 Si1 116.04(16) . . ? C4 C5 C30 119.88(19) . . ? C30 C5 Si1 124.06(15) . . ? C7 C6 C1 120.4(2) . . ? C11 C6 C1 120.6(2) . . ? C11 C6 C7 119.0(2) . . ? C6 C7 H7 119.8 . . ? C8 C7 C6 120.5(3) . . ? C8 C7 H7 119.8 . . ? C7 C8 H8 119.9 . . ? C9 C8 C7 120.1(3) . . ? C9 C8 H8 119.9 . . ? C8 C9 H9 119.9 . . ? C8 C9 C10 120.1(2) . . ? C10 C9 H9 119.9 . . ? C9 C10 H10 119.8 . . ? C9 C10 C11 120.5(3) . . ? C11 C10 H10 119.8 . . ? C6 C11 C10 119.8(3) . . ? C6 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C13 C12 C3 121.4(2) . . ? C17 C12 C3 121.5(2) . . ? C17 C12 C13 116.9(2) . . ? C12 C13 H13 119.0 . . ? C14 C13 C12 122.0(2) . . ? C14 C13 H13 119.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 C13 120.1(3) . . ? C15 C14 H14 120.0 . . ? C14 C15 H15 120.3 . . ? C14 C15 C16 119.3(2) . . ? C16 C15 H15 120.3 . . ? C15 C16 H16 119.7 . . ? C15 C16 C17 120.6(2) . . ? C17 C16 H16 119.7 . . ? C12 C17 H17 119.5 . . ? C16 C17 C12 121.0(2) . . ? C16 C17 H17 119.5 . . ? C19 C18 Si1 120.32(18) . . ? C23 C18 Si1 122.29(17) . . ? C23 C18 C19 117.3(2) . . ? C18 C19 H19 119.2 . . ? C20 C19 C18 121.6(2) . . ? C20 C19 H19 119.2 . . ? C19 C20 H20 120.0 . . ? C21 C20 C19 120.1(2) . . ? C21 C20 H20 120.0 . . ? C20 C21 H21 120.3 . . ? C20 C21 C22 119.5(2) . . ? C22 C21 H21 120.3 . . ? C21 C22 H22 119.7 . . ? C21 C22 C23 120.7(3) . . ? C23 C22 H22 119.7 . . ? C18 C23 H23 119.6 . . ? C22 C23 C18 120.9(2) . . ? C22 C23 H23 119.6 . . ? C25 C24 Si1 121.16(18) . . ? C25 C24 C29 116.8(2) . . ? C29 C24 Si1 122.01(19) . . ? C24 C25 H25 119.1 . . ? C24 C25 C26 121.7(3) . . ? C26 C25 H25 119.1 . . ? C25 C26 H26 119.8 . . ? C27 C26 C25 120.3(3) . . ? C27 C26 H26 119.8 . . ? C26 C27 H27 120.3 . . ? C26 C27 C28 119.3(3) . . ? C28 C27 H27 120.3 . . ? C27 C28 H28 119.9 . . ? C27 C28 C29 120.3(3) . . ? C29 C28 H28 119.9 . . ? C24 C29 H29 119.2 . . ? C28 C29 C24 121.5(3) . . ? C28 C29 H29 119.2 . . ? C31 C30 C5 120.84(19) . . ? C35 C30 C5 121.7(2) . . ? C35 C30 C31 117.4(2) . . ? C30 C31 H31 119.3 . . ? C32 C31 C30 121.4(2) . . ? C32 C31 H31 119.3 . . ? C31 C32 H32 119.9 . . ? C33 C32 C31 120.1(2) . . ? C33 C32 H32 119.9 . . ? C32 C33 H33 120.3 . . ? C34 C33 C32 119.5(2) . . ? C34 C33 H33 120.3 . . ? C33 C34 H34 119.9 . . ? C33 C34 C35 120.1(2) . . ? C35 C34 H34 119.9 . . ? C30 C35 H35 119.3 . . ? C34 C35 C30 121.5(2) . . ? C34 C35 H35 119.3 . . ? Ti1 C36 H36 125.8 . . ? C37 C36 Ti1 73.66(13) . . ? C37 C36 H36 125.8 . . ? C37 C36 C40 107.9(2) . . ? C40 C36 Ti1 72.15(13) . . ? C40 C36 H36 125.8 . . ? Ti1 C37 H37 125.8 . . ? C36 C37 Ti1 72.03(13) . . ? C36 C37 H37 125.8 . . ? C38 C37 Ti1 73.01(14) . . ? C38 C37 C36 108.0(2) . . ? C38 C37 H37 125.8 . . ? Ti1 C38 H38 125.6 . . ? C37 C38 Ti1 72.87(14) . . ? C37 C38 H38 125.6 . . ? C39 C38 Ti1 72.83(14) . . ? C39 C38 C37 108.4(2) . . ? C39 C38 H38 125.6 . . ? Ti1 C39 H39 125.9 . . ? C38 C39 Ti1 73.13(14) . . ? C38 C39 H39 125.9 . . ? C38 C39 C40 108.0(2) . . ? C40 C39 Ti1 71.51(14) . . ? C40 C39 H39 125.9 . . ? Ti1 C40 H40 125.8 . . ? C36 C40 Ti1 73.14(14) . . ? C36 C40 H40 125.8 . . ? C39 C40 Ti1 73.95(14) . . ? C39 C40 C36 107.8(2) . . ? C39 C40 H40 125.8 . . ? Ti1 C41 H41 126.0 . . ? C42 C41 Ti1 72.89(14) . . ? C42 C41 H41 126.0 . . ? C42 C41 C45 107.6(2) . . ? C45 C41 Ti1 72.94(14) . . ? C45 C41 H41 126.0 . . ? Ti1 C42 H42 125.9 . . ? C41 C42 Ti1 72.48(13) . . ? C41 C42 H42 125.9 . . ? C43 C42 Ti1 72.68(13) . . ? C43 C42 C41 107.8(2) . . ? C43 C42 H42 125.9 . . ? Ti1 C43 H43 125.6 . . ? C42 C43 Ti1 72.80(13) . . ? C42 C43 H43 125.6 . . ? C44 C43 Ti1 73.92(13) . . ? C44 C43 C42 108.3(2) . . ? C44 C43 H43 125.6 . . ? Ti1 C44 H44 125.9 . . ? C43 C44 Ti1 71.83(13) . . ? C43 C44 H44 125.9 . . ? C45 C44 Ti1 72.03(13) . . ? C45 C44 C43 108.0(2) . . ? C45 C44 H44 125.9 . . ? Ti1 C45 H45 125.6 . . ? C41 C45 Ti1 72.39(14) . . ? C41 C45 H45 125.6 . . ? C44 C45 Ti1 73.86(14) . . ? C44 C45 C41 108.3(2) . . ? C44 C45 H45 125.6 . . ? H46A C46 H46B 108.0 . . ? C47 C46 H46A 109.3 . . ? C47 C46 H46B 109.3 . . ? C48 C46 H46A 109.3 . . ? C48 C46 H46B 109.3 . . ? C48 C46 C47 111.5(5) . . ? C46 C47 H47A 110.8 . . ? C46 C47 H47B 110.8 . . ? H47A C47 H47B 108.9 . . ? C49 C47 C46 104.6(5) . . ? C49 C47 H47A 110.8 . . ? C49 C47 H47B 110.8 . . ? C46 C48 O1 99.4(5) . . ? C46 C48 O1A 89.3(8) . . ? C47 C49 O1 101.9(5) . . ? C47 C49 O1A 87.2(10) . . ? C49 O1A C48 109.8(9) . . ? _shelx_estimated_absorpt_T_max 0.971 _shelx_estimated_absorpt_T_min 0.943 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelxl_version_number 2013-3