# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1160 data_greg16 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H35 B F15 N Si Ti' _chemical_formula_weight 877.47 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2430(10) _cell_length_b 11.3760(10) _cell_length_c 16.419(2) _cell_angle_alpha 78.670(10) _cell_angle_beta 79.450(10) _cell_angle_gamma 84.850(10) _cell_volume 1841.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method ? _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 0.372 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9281 _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8284 _reflns_number_observed 6974 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+1.1019P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8282 _refine_ls_number_parameters 654 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_obs 0.0410 _refine_ls_wR_factor_all 0.1170 _refine_ls_wR_factor_obs 0.1092 _refine_ls_goodness_of_fit_all 1.057 _refine_ls_goodness_of_fit_obs 1.085 _refine_ls_restrained_S_all 1.059 _refine_ls_restrained_S_obs 1.085 _refine_ls_shift/esd_max -0.060 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ti1 Ti 0.56807(3) 0.84230(3) 0.30099(2) 0.02171(9) Uani 1 d . . B1 B 0.7763(2) 0.5779(2) 0.19025(13) 0.0226(4) Uani 1 d . . Si1 Si 0.32794(5) 0.79627(5) 0.41715(4) 0.03043(13) Uani 1 d . . N1 N 0.3837(2) 0.80076(15) 0.30842(10) 0.0262(3) Uani 1 d . . F1 F 0.65247(12) 0.72702(12) 0.05840(8) 0.0358(3) Uani 1 d . . F2 F 0.7652(2) 0.88541(15) -0.06929(10) 0.0571(4) Uani 1 d . . F3 F 1.0334(2) 0.9068(2) -0.09792(10) 0.0654(5) Uani 1 d . . F4 F 1.18504(15) 0.7590(2) 0.00327(10) 0.0562(4) Uani 1 d . . F5 F 1.07554(12) 0.59876(14) 0.13117(9) 0.0417(3) Uani 1 d . . F6 F 0.73558(14) 0.48908(12) 0.03333(8) 0.0375(3) Uani 1 d . . F7 F 0.5322(2) 0.37065(13) 0.02089(9) 0.0480(4) Uani 1 d . . F8 F 0.3326(2) 0.31598(14) 0.15479(12) 0.0554(4) Uani 1 d . . F9 F 0.35169(14) 0.37404(13) 0.30497(10) 0.0475(4) Uani 1 d . . F10 F 0.56179(14) 0.48139(12) 0.32214(8) 0.0381(3) Uani 1 d . . F11 F 0.9019(2) 0.35793(14) 0.14578(9) 0.0505(4) Uani 1 d . . F12 F 1.0519(2) 0.19390(13) 0.23168(11) 0.0556(4) Uani 1 d . . F13 F 1.11462(14) 0.22917(13) 0.37854(10) 0.0489(4) Uani 1 d . . F14 F 1.0249(2) 0.4343(2) 0.43596(9) 0.0500(4) Uani 1 d . . F15 F 0.87234(14) 0.59783(12) 0.35340(8) 0.0390(3) Uani 1 d . . C1 C 0.6978(2) 0.6921(2) 0.23719(12) 0.0229(4) Uani 1 d . . C2 C 0.7721(2) 0.8029(2) 0.22537(13) 0.0272(4) Uani 1 d . . C3 C 0.7313(2) 0.9170(2) 0.18878(14) 0.0346(5) Uani 1 d . . C4 C 0.6019(2) 0.9538(2) 0.17206(15) 0.0375(5) Uani 1 d . . C5 C 0.5654(4) 1.0819(3) 0.1352(2) 0.0556(7) Uani 1 d . . H5A H 0.4693(45) 1.0980(39) 0.1419(26) 0.094(13) Uiso 1 d . . H5B H 0.5848(39) 1.0865(36) 0.0739(26) 0.083(12) Uiso 1 d . . H5C H 0.6218(39) 1.1414(36) 0.1551(24) 0.080(11) Uiso 1 d . . C6 C 0.6036(2) 0.8084(2) 0.43953(13) 0.0289(4) Uani 1 d . . C7 C 0.7042(2) 0.8873(2) 0.39939(14) 0.0323(4) Uani 1 d . . C8 C 0.6417(2) 0.9989(2) 0.3657(2) 0.0365(5) Uani 1 d . . C9 C 0.5034(2) 0.9880(2) 0.38457(14) 0.0334(4) Uani 1 d . . C10 C 0.4766(2) 0.8690(2) 0.43029(13) 0.0289(4) Uani 1 d . . C11 C 0.6283(3) 0.6833(2) 0.48704(15) 0.0380(5) Uani 1 d . . H11A H 0.6094(32) 0.6124(31) 0.4627(20) 0.060(9) Uiso 1 d . . H11B H 0.5686(39) 0.6665(35) 0.5409(25) 0.082(11) Uiso 1 d . . H11C H 0.7156(43) 0.6690(37) 0.4935(25) 0.089(13) Uiso 1 d . . C12 C 0.8496(2) 0.8666(3) 0.4018(2) 0.0439(6) Uani 1 d . . H12A H 0.8728(33) 0.8965(31) 0.4493(22) 0.065(9) Uiso 1 d . . H12B H 0.9000(35) 0.9055(31) 0.3500(22) 0.063(9) Uiso 1 d . . H12C H 0.8805(34) 0.7815(33) 0.4096(21) 0.066(10) Uiso 1 d . . C13 C 0.7108(4) 1.1115(3) 0.3258(2) 0.0536(7) Uani 1 d . . H13A H 0.7946(41) 1.0953(35) 0.2996(24) 0.077(12) Uiso 1 d . . H13B H 0.7192(41) 1.1548(38) 0.3623(26) 0.086(13) Uiso 1 d . . H13C H 0.6688(40) 1.1598(36) 0.2816(25) 0.082(12) Uiso 1 d . . C14 C 0.4029(3) 1.0863(2) 0.3605(2) 0.0482(6) Uani 1 d . . H14A H 0.3598(41) 1.1218(37) 0.4091(27) 0.091(13) Uiso 1 d . . H14B H 0.3483(38) 1.0587(35) 0.3252(24) 0.079(11) Uiso 1 d . . H14C H 0.4413(42) 1.1410(40) 0.3193(27) 0.089(13) Uiso 1 d . . C15 C 0.1699(3) 0.8813(3) 0.4513(2) 0.0530(7) Uani 1 d . . H15A H 0.1699(50) 0.8922(47) 0.5107(34) 0.130(18) Uiso 1 d . . H15B H 0.1043(50) 0.8353(44) 0.4468(30) 0.114(17) Uiso 1 d . . H15C H 0.1630(30) 0.9557(29) 0.4130(19) 0.048(8) Uiso 1 d . . C16 C 0.3151(3) 0.6405(3) 0.4811(2) 0.0470(6) Uani 1 d . . H16A H 0.2282(38) 0.6143(32) 0.4826(22) 0.071(10) Uiso 1 d . . H16B H 0.3222(32) 0.6409(29) 0.5356(22) 0.059(9) Uiso 1 d . . H16C H 0.3856(39) 0.5859(34) 0.4554(23) 0.076(11) Uiso 1 d . . C17 C 0.2920(2) 0.7748(2) 0.25315(14) 0.0322(4) Uani 1 d . . C18 C 0.2103(3) 0.8911(3) 0.2275(2) 0.0535(7) Uani 1 d . . H18A H 0.1578(34) 0.8768(30) 0.1874(21) 0.065(9) Uiso 1 d . . H18B H 0.2747(35) 0.9544(32) 0.1981(22) 0.067(10) Uiso 1 d . . H18C H 0.1566(38) 0.9179(35) 0.2840(25) 0.082(12) Uiso 1 d . . C19 C 0.1982(3) 0.6779(3) 0.3012(2) 0.0493(6) Uani 1 d . . H19A H 0.1349(31) 0.6624(27) 0.2638(19) 0.053(8) Uiso 1 d . . H19B H 0.1446(30) 0.7011(26) 0.3526(19) 0.049(8) Uiso 1 d . . H19C H 0.2507(32) 0.6052(30) 0.3207(20) 0.056(9) Uiso 1 d . . C20 C 0.3653(2) 0.7316(3) 0.1742(2) 0.0414(5) Uani 1 d . . H20A H 0.3055(29) 0.7102(26) 0.1447(18) 0.045(7) Uiso 1 d . . H20B H 0.4267(31) 0.6574(28) 0.1877(19) 0.054(8) Uiso 1 d . . H20C H 0.4114(31) 0.8062(29) 0.1374(19) 0.053(8) Uiso 1 d . . C21 C 0.8569(2) 0.6520(2) 0.10164(12) 0.0255(4) Uani 1 d . . C22 C 0.7862(2) 0.7286(2) 0.04602(13) 0.0298(4) Uani 1 d . . C23 C 0.8417(2) 0.8130(2) -0.02054(14) 0.0383(5) Uani 1 d . . C24 C 0.9765(3) 0.8238(2) -0.03448(15) 0.0427(6) Uani 1 d . . C25 C 1.0524(2) 0.7495(2) 0.01694(14) 0.0386(5) Uani 1 d . . C26 C 0.9928(2) 0.6656(2) 0.08285(13) 0.0306(4) Uani 1 d . . C27 C 0.6581(2) 0.4969(2) 0.17762(12) 0.0252(4) Uani 1 d . . C28 C 0.6440(2) 0.4628(2) 0.10308(13) 0.0292(4) Uani 1 d . . C29 C 0.5386(2) 0.4010(2) 0.09461(14) 0.0344(5) Uani 1 d . . C30 C 0.4384(2) 0.3723(2) 0.1622(2) 0.0382(5) Uani 1 d . . C31 C 0.4485(2) 0.4010(2) 0.23778(15) 0.0347(5) Uani 1 d . . C32 C 0.5580(2) 0.4590(2) 0.24459(13) 0.0290(4) Uani 1 d . . C33 C 0.8746(2) 0.4855(2) 0.24576(12) 0.0247(4) Uani 1 d . . C34 C 0.9269(2) 0.3801(2) 0.21901(13) 0.0324(4) Uani 1 d . . C35 C 1.0063(2) 0.2942(2) 0.2615(2) 0.0363(5) Uani 1 d . . C36 C 1.0388(2) 0.3119(2) 0.33526(14) 0.0339(5) Uani 1 d . . C37 C 0.9930(2) 0.4152(2) 0.36440(13) 0.0321(4) Uani 1 d . . C38 C 0.9124(2) 0.4983(2) 0.31979(13) 0.0275(4) Uani 1 d . . H1A H 0.6691(25) 0.6649(22) 0.2945(16) 0.032(6) Uiso 1 d . . H1B H 0.6239(26) 0.7056(22) 0.2148(15) 0.031(6) Uiso 1 d . . H2 H 0.8510(26) 0.7950(23) 0.2477(16) 0.035(6) Uiso 1 d . . H3 H 0.7882(31) 0.9834(29) 0.1860(19) 0.057(9) Uiso 1 d . . H4 H 0.5500(27) 0.8955(25) 0.1539(17) 0.041(7) Uiso 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 0.0190(2) 0.0179(2) 0.0275(2) -0.00312(12) -0.00274(12) -0.00161(11) B1 0.0224(9) 0.0222(9) 0.0229(9) -0.0034(7) -0.0036(8) -0.0010(7) Si1 0.0220(3) 0.0352(3) 0.0321(3) -0.0057(2) -0.0001(2) -0.0014(2) N1 0.0214(7) 0.0254(8) 0.0302(8) -0.0019(6) -0.0038(6) -0.0003(6) F1 0.0297(6) 0.0385(7) 0.0351(6) 0.0042(5) -0.0070(5) -0.0016(5) F2 0.0606(10) 0.0539(9) 0.0464(8) 0.0218(7) -0.0134(7) -0.0079(8) F3 0.0677(11) 0.0669(11) 0.0498(9) 0.0181(8) 0.0043(8) -0.0338(9) F4 0.0336(7) 0.0759(11) 0.0545(9) -0.0044(8) 0.0063(6) -0.0232(7) F5 0.0246(6) 0.0574(9) 0.0403(7) -0.0019(6) -0.0047(5) -0.0041(6) F6 0.0467(8) 0.0391(7) 0.0272(6) -0.0090(5) -0.0028(5) -0.0068(6) F7 0.0651(10) 0.0413(8) 0.0482(8) -0.0140(6) -0.0293(7) -0.0061(7) F8 0.0450(8) 0.0438(8) 0.0848(12) -0.0101(8) -0.0249(8) -0.0172(7) F9 0.0382(7) 0.0381(7) 0.0585(9) 0.0022(6) 0.0057(6) -0.0150(6) F10 0.0463(7) 0.0390(7) 0.0269(6) -0.0023(5) 0.0014(5) -0.0150(6) F11 0.0605(9) 0.0536(9) 0.0466(8) -0.0301(7) -0.0234(7) 0.0240(7) F12 0.0608(10) 0.0373(8) 0.0730(11) -0.0232(7) -0.0207(8) 0.0225(7) F13 0.0405(8) 0.0462(8) 0.0525(8) 0.0078(7) -0.0146(6) 0.0137(6) F14 0.0498(8) 0.0677(10) 0.0366(7) -0.0137(7) -0.0212(6) 0.0134(7) F15 0.0428(7) 0.0405(7) 0.0400(7) -0.0198(6) -0.0166(6) 0.0111(6) C1 0.0195(8) 0.0231(9) 0.0248(9) -0.0031(7) -0.0020(7) -0.0013(7) C2 0.0215(9) 0.0273(9) 0.0322(10) -0.0081(8) 0.0014(8) -0.0041(7) C3 0.0333(11) 0.0290(10) 0.0364(11) -0.0016(8) 0.0068(9) -0.0101(9) C4 0.0389(12) 0.0286(10) 0.0400(12) 0.0026(9) -0.0015(9) -0.0055(9) C5 0.063(2) 0.0354(13) 0.058(2) 0.0136(12) -0.0085(14) 0.0009(12) C6 0.0283(10) 0.0308(10) 0.0291(10) -0.0098(8) -0.0057(8) 0.0019(8) C7 0.0292(10) 0.0331(10) 0.0390(11) -0.0126(9) -0.0100(8) -0.0026(8) C8 0.0395(12) 0.0266(10) 0.0466(12) -0.0120(9) -0.0079(10) -0.0056(9) C9 0.0359(11) 0.0252(10) 0.0413(11) -0.0130(8) -0.0070(9) 0.0020(8) C10 0.0264(9) 0.0306(10) 0.0301(10) -0.0097(8) -0.0030(8) 0.0020(8) C11 0.0401(13) 0.0371(12) 0.0333(11) -0.0016(9) -0.0070(10) 0.0070(10) C12 0.0286(11) 0.054(2) 0.056(2) -0.0241(13) -0.0106(11) -0.0017(10) C13 0.062(2) 0.0339(13) 0.068(2) -0.0102(13) -0.010(2) -0.0190(13) C14 0.056(2) 0.0288(12) 0.059(2) -0.0111(12) -0.0112(13) 0.0124(11) C15 0.0282(12) 0.077(2) 0.057(2) -0.029(2) -0.0030(11) 0.0108(13) C16 0.0479(15) 0.0498(15) 0.0377(13) 0.0097(11) -0.0040(11) -0.0183(12) C17 0.0243(9) 0.0366(11) 0.0362(11) -0.0034(9) -0.0095(8) -0.0032(8) C18 0.0464(15) 0.057(2) 0.059(2) -0.0055(14) -0.0278(14) 0.0148(13) C19 0.0396(13) 0.063(2) 0.0478(14) -0.0062(13) -0.0083(12) -0.0251(13) C20 0.0328(11) 0.056(2) 0.0401(12) -0.0152(11) -0.0111(10) -0.0050(11) C21 0.0269(9) 0.0265(9) 0.0231(8) -0.0060(7) -0.0015(7) -0.0038(7) C22 0.0300(10) 0.0307(10) 0.0271(9) -0.0028(8) -0.0019(8) -0.0051(8) C23 0.0464(13) 0.0346(11) 0.0303(10) 0.0030(9) -0.0052(9) -0.0058(10) C24 0.0497(14) 0.0414(13) 0.0317(11) 0.0027(9) 0.0046(10) -0.0194(11) C25 0.0318(11) 0.0478(13) 0.0351(11) -0.0091(10) 0.0049(9) -0.0149(10) C26 0.0296(10) 0.0349(11) 0.0274(9) -0.0074(8) -0.0011(8) -0.0052(8) C27 0.0263(9) 0.0215(8) 0.0278(9) -0.0023(7) -0.0070(7) -0.0003(7) C28 0.0346(10) 0.0237(9) 0.0293(10) -0.0023(7) -0.0093(8) -0.0002(8) C29 0.0447(12) 0.0250(10) 0.0381(11) -0.0050(8) -0.0204(10) -0.0012(9) C30 0.0357(11) 0.0248(10) 0.0571(14) -0.0018(9) -0.0194(10) -0.0066(8) C31 0.0321(11) 0.0239(9) 0.0447(12) 0.0022(9) -0.0042(9) -0.0061(8) C32 0.0323(10) 0.0242(9) 0.0292(9) 0.0001(7) -0.0057(8) -0.0043(8) C33 0.0217(9) 0.0256(9) 0.0252(9) -0.0025(7) -0.0025(7) -0.0001(7) C34 0.0322(10) 0.0333(11) 0.0331(10) -0.0098(8) -0.0073(8) 0.0033(8) C35 0.0320(11) 0.0297(10) 0.0460(12) -0.0091(9) -0.0053(9) 0.0072(8) C36 0.0240(9) 0.0346(11) 0.0374(11) 0.0049(9) -0.0055(8) 0.0044(8) C37 0.0258(10) 0.0417(12) 0.0276(9) -0.0026(8) -0.0065(8) 0.0002(8) C38 0.0231(9) 0.0286(10) 0.0297(9) -0.0060(8) -0.0018(7) 0.0010(7) _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 N1 1.964(2) . ? Ti1 C10 2.225(2) . ? Ti1 C4 2.228(2) . ? Ti1 C2 2.282(2) . ? Ti1 C6 2.321(2) . ? Ti1 C3 2.329(2) . ? Ti1 C9 2.331(2) . ? Ti1 C1 2.360(2) . ? Ti1 C7 2.469(2) . ? Ti1 C8 2.479(2) . ? Ti1 Si1 2.8430(7) . ? Ti1 H1A 2.20(2) . ? B1 C21 1.647(3) . ? B1 C33 1.649(3) . ? B1 C27 1.650(3) . ? B1 C1 1.705(3) . ? Si1 N1 1.764(2) . ? Si1 C10 1.862(2) . ? Si1 C15 1.863(3) . ? Si1 C16 1.876(3) . ? N1 C17 1.504(3) . ? F1 C22 1.349(2) . ? F2 C23 1.337(3) . ? F3 C24 1.344(3) . ? F4 C25 1.346(3) . ? F5 C26 1.349(3) . ? F6 C28 1.343(2) . ? F7 C29 1.336(3) . ? F8 C30 1.342(2) . ? F9 C31 1.347(3) . ? F10 C32 1.355(2) . ? F11 C34 1.348(2) . ? F12 C35 1.341(3) . ? F13 C36 1.342(2) . ? F14 C37 1.338(2) . ? F15 C38 1.355(2) . ? C1 C2 1.493(3) . ? C1 H1A 0.93(3) . ? C1 H1B 0.89(3) . ? C2 C3 1.382(3) . ? C2 H2 0.94(3) . ? C3 C4 1.412(3) . ? C3 H3 0.98(3) . ? C4 C5 1.506(3) . ? C4 H4 1.01(3) . ? C5 H5A 0.98(4) . ? C5 H5B 0.98(4) . ? C5 H5C 1.06(4) . ? C6 C7 1.410(3) . ? C6 C10 1.435(3) . ? C6 C11 1.506(3) . ? C7 C8 1.427(3) . ? C7 C12 1.494(3) . ? C8 C9 1.405(3) . ? C8 C13 1.495(3) . ? C9 C10 1.436(3) . ? C9 C14 1.495(3) . ? C11 H11A 1.02(3) . ? C11 H11B 0.97(4) . ? C11 H11C 0.92(4) . ? C12 H12A 0.98(4) . ? C12 H12B 0.96(4) . ? C12 H12C 0.98(4) . ? C13 H13A 0.91(4) . ? C13 H13B 0.87(4) . ? C13 H13C 0.96(4) . ? C14 H14A 0.98(4) . ? C14 H14B 0.98(4) . ? C14 H14C 0.88(4) . ? C15 H15A 1.01(5) . ? C15 H15B 0.91(5) . ? C15 H15C 0.95(3) . ? C16 H16A 0.96(4) . ? C16 H16B 0.91(3) . ? C16 H16C 1.00(4) . ? C17 C20 1.520(3) . ? C17 C19 1.526(3) . ? C17 C18 1.530(3) . ? C18 H18A 0.97(3) . ? C18 H18B 1.01(4) . ? C18 H18C 1.07(4) . ? C19 H19A 1.02(3) . ? C19 H19B 0.99(3) . ? C19 H19C 0.98(3) . ? C20 H20A 0.92(3) . ? C20 H20B 1.02(3) . ? C20 H20C 1.04(3) . ? C21 C26 1.386(3) . ? C21 C22 1.390(3) . ? C22 C23 1.377(3) . ? C23 C24 1.371(4) . ? C24 C25 1.369(4) . ? C25 C26 1.383(3) . ? C27 C32 1.388(3) . ? C27 C28 1.390(3) . ? C28 C29 1.381(3) . ? C29 C30 1.375(3) . ? C30 C31 1.368(3) . ? C31 C32 1.383(3) . ? C33 C38 1.378(3) . ? C33 C34 1.387(3) . ? C34 C35 1.379(3) . ? C35 C36 1.369(3) . ? C36 C37 1.367(3) . ? C37 C38 1.386(3) . ? 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 N1 Ti1 C10 77.75(7) . . ? N1 Ti1 C4 100.21(8) . . ? C10 Ti1 C4 137.06(8) . . ? N1 Ti1 C2 137.75(7) . . ? C10 Ti1 C2 139.64(8) . . ? C4 Ti1 C2 66.89(8) . . ? N1 Ti1 C6 104.94(7) . . ? C10 Ti1 C6 36.72(7) . . ? C4 Ti1 C6 148.67(8) . . ? C2 Ti1 C6 104.16(7) . . ? N1 Ti1 C3 133.22(8) . . ? C10 Ti1 C3 141.13(8) . . ? C4 Ti1 C3 36.02(9) . . ? C2 Ti1 C3 34.85(8) . . ? C6 Ti1 C3 121.80(8) . . ? N1 Ti1 C9 92.43(8) . . ? C10 Ti1 C9 36.65(8) . . ? C4 Ti1 C9 101.77(9) . . ? C2 Ti1 C9 128.93(8) . . ? C6 Ti1 C9 59.20(7) . . ? C3 Ti1 C9 108.89(8) . . ? N1 Ti1 C1 104.34(7) . . ? C10 Ti1 C1 137.75(7) . . ? C4 Ti1 C1 84.81(8) . . ? C2 Ti1 C1 37.46(6) . . ? C6 Ti1 C1 106.35(7) . . ? C3 Ti1 C1 66.19(7) . . ? C9 Ti1 C1 160.71(7) . . ? N1 Ti1 C7 136.02(7) . . ? C10 Ti1 C7 58.75(7) . . ? C4 Ti1 C7 115.41(8) . . ? C2 Ti1 C7 82.32(7) . . ? C6 Ti1 C7 34.06(7) . . ? C3 Ti1 C7 89.19(8) . . ? C9 Ti1 C7 56.97(8) . . ? C1 Ti1 C7 103.79(7) . . ? N1 Ti1 C8 126.21(8) . . ? C10 Ti1 C8 58.57(8) . . ? C4 Ti1 C8 92.96(9) . . ? C2 Ti1 C8 95.37(8) . . ? C6 Ti1 C8 57.01(8) . . ? C3 Ti1 C8 82.57(8) . . ? C9 Ti1 C8 33.80(8) . . ? C1 Ti1 C8 128.80(7) . . ? C7 Ti1 C8 33.52(7) . . ? N1 Ti1 Si1 37.77(5) . . ? C10 Ti1 Si1 40.88(6) . . ? C4 Ti1 Si1 130.13(7) . . ? C2 Ti1 Si1 158.17(5) . . ? C6 Ti1 Si1 68.32(5) . . ? C3 Ti1 Si1 165.69(6) . . ? C9 Ti1 Si1 66.19(6) . . ? C1 Ti1 Si1 122.99(5) . . ? C7 Ti1 Si1 98.27(5) . . ? C8 Ti1 Si1 96.91(6) . . ? N1 Ti1 H1A 99.3(7) . . ? C10 Ti1 H1A 114.6(7) . . ? C4 Ti1 H1A 108.0(7) . . ? C2 Ti1 H1A 53.2(7) . . ? C6 Ti1 H1A 86.2(7) . . ? C3 Ti1 H1A 86.4(7) . . ? C9 Ti1 H1A 145.3(7) . . ? C1 Ti1 H1A 23.2(7) . . ? C7 Ti1 H1A 93.6(7) . . ? C8 Ti1 H1A 125.6(7) . . ? Si1 Ti1 H1A 105.1(7) . . ? C21 B1 C33 113.0(2) . . ? C21 B1 C27 114.2(2) . . ? C33 B1 C27 106.47(15) . . ? C21 B1 C1 101.65(14) . . ? C33 B1 C1 115.2(2) . . ? C27 B1 C1 106.34(15) . . ? N1 Si1 C10 93.26(9) . . ? N1 Si1 C15 118.72(12) . . ? C10 Si1 C15 112.14(13) . . ? N1 Si1 C16 114.00(12) . . ? C10 Si1 C16 112.01(11) . . ? C15 Si1 C16 106.4(2) . . ? N1 Si1 Ti1 42.99(5) . . ? C10 Si1 Ti1 51.44(6) . . ? C15 Si1 Ti1 137.31(12) . . ? C16 Si1 Ti1 116.27(10) . . ? C17 N1 Si1 120.73(13) . . ? C17 N1 Ti1 140.02(13) . . ? Si1 N1 Ti1 99.24(8) . . ? C2 C1 B1 116.9(2) . . ? C2 C1 Ti1 68.45(10) . . ? B1 C1 Ti1 174.01(13) . . ? C2 C1 H1A 109.5(16) . . ? B1 C1 H1A 110.7(15) . . ? Ti1 C1 H1A 68.5(15) . . ? C2 C1 H1B 112.4(16) . . ? B1 C1 H1B 101.5(16) . . ? Ti1 C1 H1B 73.3(16) . . ? H1A C1 H1B 104.9(22) . . ? C3 C2 C1 125.9(2) . . ? C3 C2 Ti1 74.40(12) . . ? C1 C2 Ti1 74.08(10) . . ? C3 C2 H2 117.1(16) . . ? C1 C2 H2 116.9(16) . . ? Ti1 C2 H2 123.2(15) . . ? C2 C3 C4 125.8(2) . . ? C2 C3 Ti1 70.75(11) . . ? C4 C3 Ti1 68.12(12) . . ? C2 C3 H3 118.2(18) . . ? C4 C3 H3 114.4(18) . . ? Ti1 C3 H3 126.7(18) . . ? C3 C4 C5 121.9(2) . . ? C3 C4 Ti1 75.86(13) . . ? C5 C4 Ti1 134.6(2) . . ? C3 C4 H4 118.5(16) . . ? C5 C4 H4 111.8(16) . . ? Ti1 C4 H4 87.7(15) . . ? C4 C5 H5A 111.8(25) . . ? C4 C5 H5B 105.3(23) . . ? H5A C5 H5B 99.0(32) . . ? C4 C5 H5C 110.2(20) . . ? H5A C5 H5C 117.6(33) . . ? H5B C5 H5C 112.0(31) . . ? C7 C6 C10 108.7(2) . . ? C7 C6 C11 124.5(2) . . ? C10 C6 C11 126.7(2) . . ? C7 C6 Ti1 78.70(12) . . ? C10 C6 Ti1 67.99(11) . . ? C11 C6 Ti1 121.44(15) . . ? C6 C7 C8 108.0(2) . . ? C6 C7 C12 126.8(2) . . ? C8 C7 C12 124.6(2) . . ? C6 C7 Ti1 67.24(11) . . ? C8 C7 Ti1 73.65(12) . . ? C12 C7 Ti1 131.4(2) . . ? C9 C8 C7 108.0(2) . . ? C9 C8 C13 125.9(2) . . ? C7 C8 C13 125.7(2) . . ? C9 C8 Ti1 67.29(12) . . ? C7 C8 Ti1 72.83(12) . . ? C13 C8 Ti1 130.5(2) . . ? C8 C9 C10 108.9(2) . . ? C8 C9 C14 124.4(2) . . ? C10 C9 C14 126.7(2) . . ? C8 C9 Ti1 78.91(13) . . ? C10 C9 Ti1 67.67(11) . . ? C14 C9 Ti1 119.9(2) . . ? C6 C10 C9 106.3(2) . . ? C6 C10 Si1 125.0(2) . . ? C9 C10 Si1 119.5(2) . . ? C6 C10 Ti1 75.29(12) . . ? C9 C10 Ti1 75.67(12) . . ? Si1 C10 Ti1 87.68(8) . . ? C6 C11 H11A 118.7(18) . . ? C6 C11 H11B 112.3(23) . . ? H11A C11 H11B 98.4(28) . . ? C6 C11 H11C 111.3(26) . . ? H11A C11 H11C 103.7(31) . . ? H11B C11 H11C 111.5(33) . . ? C7 C12 H12A 111.0(20) . . ? C7 C12 H12B 110.2(20) . . ? H12A C12 H12B 109.8(28) . . ? C7 C12 H12C 113.7(20) . . ? H12A C12 H12C 105.3(27) . . ? H12B C12 H12C 106.6(28) . . ? C8 C13 H13A 111.5(25) . . ? C8 C13 H13B 112.5(27) . . ? H13A C13 H13B 105.8(36) . . ? C8 C13 H13C 113.1(24) . . ? H13A C13 H13C 103.9(33) . . ? H13B C13 H13C 109.5(35) . . ? C9 C14 H14A 111.4(24) . . ? C9 C14 H14B 108.7(22) . . ? H14A C14 H14B 119.9(33) . . ? C9 C14 H14C 109.5(27) . . ? H14A C14 H14C 111.4(35) . . ? H14B C14 H14C 94.4(33) . . ? Si1 C15 H15A 107.3(29) . . ? Si1 C15 H15B 105.0(31) . . ? H15A C15 H15B 113.5(41) . . ? Si1 C15 H15C 109.9(18) . . ? H15A C15 H15C 113.0(34) . . ? H15B C15 H15C 107.9(34) . . ? Si1 C16 H16A 108.6(21) . . ? Si1 C16 H16B 110.3(21) . . ? H16A C16 H16B 106.2(29) . . ? Si1 C16 H16C 109.4(21) . . ? H16A C16 H16C 111.1(30) . . ? H16B C16 H16C 111.1(29) . . ? N1 C17 C20 113.1(2) . . ? N1 C17 C19 110.6(2) . . ? C20 C17 C19 107.4(2) . . ? N1 C17 C18 107.4(2) . . ? C20 C17 C18 109.1(2) . . ? C19 C17 C18 109.2(2) . . ? C17 C18 H18A 107.5(20) . . ? C17 C18 H18B 107.6(20) . . ? H18A C18 H18B 108.4(27) . . ? C17 C18 H18C 107.7(21) . . ? H18A C18 H18C 116.6(29) . . ? H18B C18 H18C 108.6(29) . . ? C17 C19 H19A 110.1(17) . . ? C17 C19 H19B 112.0(17) . . ? H19A C19 H19B 108.2(24) . . ? C17 C19 H19C 109.2(19) . . ? H19A C19 H19C 111.8(25) . . ? H19B C19 H19C 105.6(25) . . ? C17 C20 H20A 110.2(18) . . ? C17 C20 H20B 112.4(17) . . ? H20A C20 H20B 106.3(24) . . ? C17 C20 H20C 104.9(17) . . ? H20A C20 H20C 107.4(24) . . ? H20B C20 H20C 115.5(24) . . ? C26 C21 C22 113.4(2) . . ? C26 C21 B1 125.7(2) . . ? C22 C21 B1 119.6(2) . . ? F1 C22 C23 115.5(2) . . ? F1 C22 C21 119.5(2) . . ? C23 C22 C21 124.9(2) . . ? F2 C23 C24 120.5(2) . . ? F2 C23 C22 120.7(2) . . ? C24 C23 C22 118.8(2) . . ? F3 C24 C25 120.4(2) . . ? F3 C24 C23 120.2(2) . . ? C25 C24 C23 119.3(2) . . ? F4 C25 C24 119.7(2) . . ? F4 C25 C26 120.3(2) . . ? C24 C25 C26 120.0(2) . . ? F5 C26 C25 115.6(2) . . ? F5 C26 C21 120.9(2) . . ? C25 C26 C21 123.5(2) . . ? C32 C27 C28 113.4(2) . . ? C32 C27 B1 120.3(2) . . ? C28 C27 B1 126.2(2) . . ? F6 C28 C29 115.5(2) . . ? F6 C28 C27 120.5(2) . . ? C29 C28 C27 123.9(2) . . ? F7 C29 C30 119.8(2) . . ? F7 C29 C28 120.5(2) . . ? C30 C29 C28 119.8(2) . . ? F8 C30 C31 120.1(2) . . ? F8 C30 C29 120.9(2) . . ? C31 C30 C29 118.9(2) . . ? F9 C31 C30 120.2(2) . . ? F9 C31 C32 120.2(2) . . ? C30 C31 C32 119.6(2) . . ? F10 C32 C31 115.8(2) . . ? F10 C32 C27 120.0(2) . . ? C31 C32 C27 124.2(2) . . ? C38 C33 C34 113.0(2) . . ? C38 C33 B1 127.5(2) . . ? C34 C33 B1 119.4(2) . . ? F11 C34 C35 115.9(2) . . ? F11 C34 C33 119.4(2) . . ? C35 C34 C33 124.7(2) . . ? F12 C35 C36 119.7(2) . . ? F12 C35 C34 121.0(2) . . ? C36 C35 C34 119.3(2) . . ? F13 C36 C37 120.3(2) . . ? F13 C36 C35 120.6(2) . . ? C37 C36 C35 119.1(2) . . ? F14 C37 C36 119.8(2) . . ? F14 C37 C38 120.8(2) . . ? C36 C37 C38 119.4(2) . . ? F15 C38 C33 120.4(2) . . ? F15 C38 C37 115.1(2) . . ? C33 C38 C37 124.5(2) . . ? _refine_diff_density_max 1.014 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.056 data_greg21 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C45 H43 Al F15 N Si Ti' _chemical_formula_weight 985.77 _chemical_melting_point ? _chemical_compound_source ? 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' 'F' 'F' 0.0171 0.0103 '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' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_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 10.879(3) _cell_length_b 38.665(6) _cell_length_c 11.069(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.19(2) _cell_angle_gamma 90.00 _cell_volume 4448.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method ? _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.336 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12132 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10205 _reflns_number_observed 6604 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+3.3726P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0007(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10199 _refine_ls_number_parameters 718 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1004 _refine_ls_R_factor_obs 0.0536 _refine_ls_wR_factor_all 0.1365 _refine_ls_wR_factor_obs 0.1116 _refine_ls_goodness_of_fit_all 1.046 _refine_ls_goodness_of_fit_obs 1.092 _refine_ls_restrained_S_all 1.055 _refine_ls_restrained_S_obs 1.092 _refine_ls_shift/esd_max -0.008 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ti1 Ti 0.70999(5) 0.122601(13) 0.74211(5) 0.02420(13) Uani 1 d . . Al1 Al 1.10834(8) 0.11305(2) 0.98531(8) 0.0275(2) Uani 1 d . . Si1 Si 0.58381(8) 0.09682(2) 0.49307(8) 0.0307(2) Uani 1 d . . N1 N 0.6807(2) 0.08044(6) 0.6393(2) 0.0284(5) Uani 1 d . . F1 F 1.0750(2) 0.18704(6) 0.8309(2) 0.0587(6) Uani 1 d . . F2 F 1.2231(2) 0.24354(6) 0.8770(3) 0.0752(8) Uani 1 d . . F3 F 1.4458(2) 0.24430(6) 1.0672(3) 0.0793(8) Uani 1 d . . F4 F 1.5200(2) 0.18709(8) 1.2144(3) 0.0818(8) Uani 1 d . . F5 F 1.3704(2) 0.13039(6) 1.1706(2) 0.0599(6) Uani 1 d . . F6 F 1.1432(2) 0.15480(5) 1.2503(2) 0.0490(5) Uani 1 d . . F7 F 1.0774(2) 0.13746(7) 1.4560(2) 0.0607(6) Uani 1 d . . F8 F 0.9748(2) 0.07415(7) 1.4731(2) 0.0623(6) Uani 1 d . . F9 F 0.9329(2) 0.02900(6) 1.2770(2) 0.0663(7) Uani 1 d . . F10 F 0.9910(2) 0.04695(5) 1.0661(2) 0.0535(6) Uani 1 d . . F11 F 1.2716(2) 0.04545(6) 1.1161(2) 0.0547(6) Uani 1 d . . F12 F 1.3646(2) -0.00739(6) 1.0118(2) 0.0649(7) Uani 1 d . . F13 F 1.3457(2) -0.00681(5) 0.7629(2) 0.0544(6) Uani 1 d . . F14 F 1.2301(2) 0.04731(6) 0.6157(2) 0.0558(6) Uani 1 d . . F15 F 1.1325(2) 0.09991(5) 0.7176(2) 0.0486(5) Uani 1 d . . C1 C 0.9289(3) 0.12024(8) 0.8602(3) 0.0298(7) Uani 1 d . . C2 C 0.8527(3) 0.14188(8) 0.9220(3) 0.0323(7) Uani 1 d . . C3 C 0.7475(3) 0.13132(8) 0.9594(3) 0.0334(7) Uani 1 d . . C4 C 0.6765(3) 0.10075(8) 0.9209(3) 0.0338(7) Uani 1 d . . C5 C 0.5564(4) 0.09378(12) 0.9584(4) 0.0475(9) Uani 1 d . . H5A H 0.5059(35) 0.1176(10) 0.9640(33) 0.048(10) Uiso 1 d . . H5B H 0.4953(39) 0.0799(10) 0.8962(38) 0.057(12) Uiso 1 d . . H5C H 0.5720(36) 0.0824(10) 1.0324(40) 0.054(12) Uiso 1 d . . C6 C 0.5805(3) 0.14121(7) 0.5588(3) 0.0281(6) Uani 1 d . . C7 C 0.5118(3) 0.14862(8) 0.6487(3) 0.0312(7) Uani 1 d . . C8 C 0.5769(3) 0.17514(8) 0.7300(3) 0.0323(7) Uani 1 d . . C9 C 0.6872(3) 0.18486(7) 0.6928(3) 0.0312(7) Uani 1 d . . C10 C 0.6903(3) 0.16417(7) 0.5894(3) 0.0307(7) Uani 1 d . . C11 C 0.3890(3) 0.13225(11) 0.6554(4) 0.0436(8) Uani 1 d . . H11A H 0.3565(37) 0.1439(10) 0.7198(38) 0.059(12) Uiso 1 d . . H11B H 0.4039(38) 0.1071(11) 0.6661(37) 0.060(12) Uiso 1 d . . H11C H 0.3235(52) 0.1336(14) 0.5777(52) 0.104(18) Uiso 1 d . . C12 C 0.5316(4) 0.19301(10) 0.8290(4) 0.0437(9) Uani 1 d . . H12A H 0.6023(43) 0.2020(11) 0.8992(43) 0.074(14) Uiso 1 d . . H12B H 0.4952(40) 0.1763(11) 0.8695(40) 0.065(13) Uiso 1 d . . H12C H 0.4755(37) 0.2100(10) 0.7884(36) 0.054(11) Uiso 1 d . . C13 C 0.7731(4) 0.21453(9) 0.7466(4) 0.0428(9) Uani 1 d . . H13A H 0.7841(43) 0.2183(11) 0.8322(45) 0.074(14) Uiso 1 d . . H13B H 0.7467(41) 0.2350(11) 0.6935(42) 0.072(13) Uiso 1 d . . H13C H 0.8674(43) 0.2118(11) 0.7379(39) 0.070(13) Uiso 1 d . . C14 C 0.7902(4) 0.16701(11) 0.5202(4) 0.0442(9) Uani 1 d . . H14A H 0.7584(52) 0.1750(14) 0.4422(54) 0.105(20) Uiso 1 d . . H14B H 0.8382(43) 0.1463(13) 0.5160(41) 0.077(14) Uiso 1 d . . H14C H 0.8583(45) 0.1818(12) 0.5652(44) 0.080(15) Uiso 1 d . . C15 C 0.6560(4) 0.09639(11) 0.3596(4) 0.0446(9) Uani 1 d . . H15A H 0.6362(44) 0.0751(13) 0.3165(44) 0.083(15) Uiso 1 d . . H15B H 0.7480(40) 0.0999(10) 0.3837(35) 0.053(11) Uiso 1 d . . H15C H 0.6295(41) 0.1143(12) 0.3027(42) 0.067(13) Uiso 1 d . . C16 C 0.4203(4) 0.07750(11) 0.4288(4) 0.0448(9) Uani 1 d . . H16A H 0.4307(45) 0.0554(13) 0.3858(46) 0.090(16) Uiso 1 d . . H16B H 0.3682(45) 0.0942(13) 0.3798(44) 0.082(15) Uiso 1 d . . H16C H 0.3838(45) 0.0722(12) 0.4914(47) 0.080(16) Uiso 1 d . . C17 C 0.7067(3) 0.04242(8) 0.6573(3) 0.0330(7) Uani 1 d . . C18 C 0.5953(4) 0.02626(9) 0.6961(4) 0.0411(8) Uani 1 d . . H18A H 0.5899(35) 0.0362(10) 0.7743(37) 0.051(11) Uiso 1 d . . H18B H 0.6092(33) 0.0022(10) 0.7104(32) 0.041(9) Uiso 1 d . . H18C H 0.5139(40) 0.0292(10) 0.6223(39) 0.063(12) Uiso 1 d . . C19 C 0.8335(4) 0.03506(9) 0.7591(4) 0.0437(9) Uani 1 d . . H19A H 0.8335(30) 0.0417(8) 0.8432(32) 0.032(9) Uiso 1 d . . H19B H 0.9018(36) 0.0465(10) 0.7367(34) 0.048(11) Uiso 1 d . . H19C H 0.8527(31) 0.0090(9) 0.7632(30) 0.040(9) Uiso 1 d . . C20 C 0.7149(4) 0.02543(10) 0.5352(4) 0.0439(9) Uani 1 d . . H20A H 0.6356(39) 0.0283(10) 0.4642(37) 0.057(12) Uiso 1 d . . H20B H 0.7403(36) 0.0014(11) 0.5536(35) 0.055(11) Uiso 1 d . . H20C H 0.7859(41) 0.0352(11) 0.5051(38) 0.066(13) Uiso 1 d . . C21 C 1.2151(3) 0.15630(8) 1.0010(3) 0.0317(7) Uani 1 d . . C22 C 1.1852(3) 0.18593(8) 0.9294(3) 0.0371(7) Uani 1 d . . C23 C 1.2589(4) 0.21547(9) 0.9503(4) 0.0472(9) Uani 1 d . . C24 C 1.3711(4) 0.21577(10) 1.0461(4) 0.0506(10) Uani 1 d . . C25 C 1.4081(3) 0.18721(11) 1.1199(4) 0.0498(9) Uani 1 d . . C26 C 1.3302(3) 0.15822(9) 1.0952(3) 0.0382(7) Uani 1 d . . C27 C 1.0723(3) 0.10137(8) 1.1487(3) 0.0312(7) Uani 1 d . . C28 C 1.0910(3) 0.12277(9) 1.2523(3) 0.0363(7) Uani 1 d . . C29 C 1.0592(3) 0.11460(10) 1.3596(3) 0.0402(8) Uani 1 d . . C30 C 1.0072(3) 0.08268(11) 1.3692(3) 0.0447(9) Uani 1 d . . C31 C 0.9856(3) 0.06012(10) 1.2694(3) 0.0438(8) Uani 1 d . . C32 C 1.0175(3) 0.06984(9) 1.1631(3) 0.0365(7) Uani 1 d . . C33 C 1.1950(3) 0.07458(8) 0.9204(3) 0.0288(6) Uani 1 d . . C34 C 1.2573(3) 0.04669(9) 0.9908(3) 0.0360(7) Uani 1 d . . C35 C 1.3074(3) 0.01944(8) 0.9401(3) 0.0399(8) Uani 1 d . . C36 C 1.2976(3) 0.01956(8) 0.8138(3) 0.0382(8) Uani 1 d . . C37 C 1.2389(3) 0.04671(9) 0.7399(3) 0.0367(7) Uani 1 d . . C38 C 1.1897(3) 0.07333(8) 0.7952(3) 0.0322(7) Uani 1 d . . C39 C 0.8630(4) 0.23130(11) 1.1237(4) 0.0566(10) Uani 1 d . . C40 C 0.7603(4) 0.25358(12) 1.0840(4) 0.0598(11) Uani 1 d . . H40 H 0.6868(4) 0.25024(12) 1.1139(4) 0.072 Uiso 1 d R . C41 C 0.7598(5) 0.28063(13) 1.0019(5) 0.0744(14) Uani 1 d . . H41 H 0.6867(5) 0.29576(13) 0.9765(5) 0.089 Uiso 1 d R . C42 C 0.8621(5) 0.28611(12) 0.9565(5) 0.0753(14) Uani 1 d . . H42 H 0.8618(5) 0.30479(12) 0.8993(5) 0.090 Uiso 1 d R . C43 C 0.9665(5) 0.26386(13) 0.9950(5) 0.0692(13) Uani 1 d . . H43 H 1.0395(5) 0.26756(13) 0.9647(5) 0.083 Uiso 1 d R . C44 C 0.9683(4) 0.23692(12) 1.0755(4) 0.0597(12) Uani 1 d . . H44 H 1.0412(4) 0.22169(12) 1.0989(4) 0.072 Uiso 1 d R . C45 C 0.8676(5) 0.20303(13) 1.2145(5) 0.0785(14) Uani 1 d . . H45A H 0.7890(5) 0.20303(13) 1.2374(5) 0.118 Uiso 1 d R . H45B H 0.8766(5) 0.18132(13) 1.1760(5) 0.118 Uiso 1 d R . H45C H 0.9391(5) 0.20631(13) 1.2889(5) 0.118 Uiso 1 d R . H1A H 0.8998(31) 0.0962(9) 0.8393(30) 0.038(9) Uiso 1 d . . H1B H 0.9422(28) 0.1311(8) 0.7883(29) 0.027(8) Uiso 1 d . . H2 H 0.8793(29) 0.1668(8) 0.9355(29) 0.033(8) Uiso 1 d . . H3 H 0.7096(29) 0.1500(8) 1.0013(28) 0.029(8) Uiso 1 d . . H4 H 0.7262(32) 0.0814(9) 0.9125(32) 0.041(9) Uiso 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 0.0235(2) 0.0213(2) 0.0257(3) 0.0001(2) 0.0040(2) 0.0005(2) Al1 0.0250(4) 0.0273(4) 0.0280(5) 0.0012(4) 0.0045(4) 0.0009(4) Si1 0.0343(5) 0.0283(4) 0.0265(4) -0.0010(3) 0.0045(3) -0.0006(4) N1 0.0289(13) 0.0231(12) 0.0311(13) 0.0005(10) 0.0059(10) 0.0003(10) F1 0.0456(12) 0.0533(13) 0.0665(15) 0.0243(11) 0.0000(11) 0.0012(10) F2 0.075(2) 0.0395(13) 0.123(2) 0.0272(14) 0.047(2) 0.0014(12) F3 0.063(2) 0.0499(14) 0.139(3) -0.030(2) 0.051(2) -0.0302(12) F4 0.0440(13) 0.099(2) 0.087(2) -0.014(2) -0.0043(13) -0.0310(14) F5 0.0379(11) 0.069(2) 0.0601(14) 0.0205(12) -0.0051(10) -0.0034(11) F6 0.0609(13) 0.0402(11) 0.0499(12) -0.0103(9) 0.0227(10) -0.0112(10) F7 0.0617(14) 0.083(2) 0.0412(12) -0.0169(11) 0.0209(10) -0.0095(13) F8 0.0512(13) 0.101(2) 0.0386(12) 0.0121(12) 0.0185(10) -0.0103(13) F9 0.069(2) 0.067(2) 0.067(2) 0.0111(12) 0.0268(12) -0.0270(13) F10 0.0649(14) 0.0478(12) 0.0476(12) -0.0088(10) 0.0164(10) -0.0210(11) F11 0.0723(15) 0.0601(14) 0.0345(11) 0.0130(10) 0.0202(10) 0.0308(12) F12 0.091(2) 0.0485(13) 0.0650(15) 0.0199(11) 0.0383(13) 0.0333(13) F13 0.0656(14) 0.0430(12) 0.0640(14) -0.0135(10) 0.0337(12) 0.0032(10) F14 0.0649(14) 0.072(2) 0.0349(11) -0.0041(10) 0.0217(10) 0.0093(12) F15 0.0580(13) 0.0551(13) 0.0340(10) 0.0148(9) 0.0157(9) 0.0169(10) C1 0.0247(15) 0.027(2) 0.033(2) -0.0015(13) 0.0025(12) -0.0009(13) C2 0.033(2) 0.027(2) 0.032(2) -0.0031(13) 0.0005(13) 0.0008(13) C3 0.037(2) 0.032(2) 0.027(2) -0.0007(13) 0.0038(13) 0.0052(14) C4 0.037(2) 0.031(2) 0.032(2) 0.0006(13) 0.0095(13) 0.0005(14) C5 0.047(2) 0.054(2) 0.046(2) 0.006(2) 0.021(2) -0.004(2) C6 0.029(2) 0.0265(15) 0.0255(15) 0.0060(12) 0.0025(12) 0.0020(12) C7 0.0271(15) 0.029(2) 0.035(2) 0.0036(13) 0.0057(13) 0.0045(12) C8 0.033(2) 0.028(2) 0.034(2) 0.0030(13) 0.0071(13) 0.0086(13) C9 0.031(2) 0.0216(14) 0.038(2) 0.0057(13) 0.0049(13) 0.0035(12) C10 0.031(2) 0.0241(15) 0.036(2) 0.0059(13) 0.0080(13) 0.0033(12) C11 0.031(2) 0.048(2) 0.053(2) -0.001(2) 0.013(2) -0.001(2) C12 0.049(2) 0.039(2) 0.044(2) -0.003(2) 0.015(2) 0.014(2) C13 0.042(2) 0.029(2) 0.050(2) 0.003(2) 0.003(2) -0.0021(15) C14 0.050(2) 0.042(2) 0.047(2) 0.002(2) 0.022(2) -0.003(2) C15 0.056(2) 0.044(2) 0.035(2) 0.001(2) 0.016(2) 0.006(2) C16 0.041(2) 0.044(2) 0.042(2) -0.004(2) 0.000(2) -0.006(2) C17 0.037(2) 0.0253(15) 0.033(2) -0.0003(12) 0.0045(13) 0.0016(13) C18 0.054(2) 0.027(2) 0.040(2) 0.0028(15) 0.012(2) -0.005(2) C19 0.047(2) 0.026(2) 0.049(2) -0.003(2) 0.000(2) 0.009(2) C20 0.060(3) 0.031(2) 0.042(2) -0.007(2) 0.017(2) 0.004(2) C21 0.029(2) 0.031(2) 0.037(2) 0.0003(13) 0.0123(13) -0.0007(13) C22 0.031(2) 0.035(2) 0.047(2) 0.0028(15) 0.0138(15) 0.0010(14) C23 0.047(2) 0.033(2) 0.073(3) 0.006(2) 0.035(2) 0.001(2) C24 0.044(2) 0.040(2) 0.080(3) -0.018(2) 0.036(2) -0.015(2) C25 0.031(2) 0.064(3) 0.053(2) -0.013(2) 0.011(2) -0.012(2) C26 0.030(2) 0.042(2) 0.042(2) 0.002(2) 0.0101(14) -0.0021(14) C27 0.0237(15) 0.039(2) 0.030(2) 0.0039(13) 0.0057(12) 0.0019(13) C28 0.028(2) 0.041(2) 0.039(2) 0.0023(15) 0.0092(13) 0.0047(14) C29 0.034(2) 0.053(2) 0.034(2) -0.006(2) 0.0102(14) 0.002(2) C30 0.031(2) 0.071(3) 0.033(2) 0.009(2) 0.0112(14) -0.001(2) C31 0.032(2) 0.051(2) 0.048(2) 0.012(2) 0.010(2) -0.008(2) C32 0.030(2) 0.042(2) 0.034(2) -0.0006(14) 0.0050(13) -0.0018(14) C33 0.0260(15) 0.0276(15) 0.033(2) -0.0004(12) 0.0085(12) -0.0052(12) C34 0.041(2) 0.040(2) 0.029(2) 0.0035(14) 0.0135(14) 0.0040(15) C35 0.046(2) 0.031(2) 0.046(2) 0.0100(15) 0.018(2) 0.0051(15) C36 0.035(2) 0.034(2) 0.049(2) -0.009(2) 0.019(2) -0.0042(14) C37 0.040(2) 0.043(2) 0.031(2) -0.0056(14) 0.0160(14) -0.0060(15) C38 0.030(2) 0.034(2) 0.033(2) 0.0034(13) 0.0090(13) -0.0015(13) C39 0.058(3) 0.051(2) 0.055(2) -0.019(2) 0.008(2) -0.007(2) C40 0.040(2) 0.069(3) 0.067(3) -0.026(2) 0.011(2) 0.000(2) C41 0.067(3) 0.058(3) 0.084(4) -0.022(3) 0.000(3) 0.005(2) C42 0.087(4) 0.054(3) 0.079(3) -0.027(2) 0.016(3) -0.023(3) C43 0.062(3) 0.064(3) 0.081(3) -0.029(3) 0.021(2) -0.023(2) C44 0.042(2) 0.067(3) 0.069(3) -0.033(2) 0.015(2) -0.009(2) C45 0.092(4) 0.074(3) 0.066(3) -0.010(3) 0.019(3) 0.010(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 N1 1.959(2) . ? Ti1 C6 2.221(3) . ? Ti1 C2 2.259(3) . ? Ti1 C4 2.277(3) . ? Ti1 C10 2.296(3) . ? Ti1 C7 2.326(3) . ? Ti1 C3 2.342(3) . ? Ti1 C1 2.356(3) . ? Ti1 C9 2.464(3) . ? Ti1 C8 2.475(3) . ? Ti1 Si1 2.8707(11) . ? Ti1 H1A 2.27(3) . ? Al1 C33 2.005(3) . ? Al1 C27 2.012(3) . ? Al1 C21 2.014(3) . ? Al1 C1 2.051(3) . ? Si1 N1 1.767(3) . ? Si1 C16 1.866(4) . ? Si1 C15 1.867(4) . ? Si1 C6 1.869(3) . ? N1 C17 1.499(4) . ? F1 C22 1.362(4) . ? F2 C23 1.342(4) . ? F3 C24 1.349(4) . ? F4 C25 1.350(4) . ? F5 C26 1.353(4) . ? F6 C28 1.365(4) . ? F7 C29 1.355(4) . ? F8 C30 1.340(4) . ? F9 C31 1.346(4) . ? F10 C32 1.355(4) . ? F11 C34 1.349(4) . ? F12 C35 1.342(4) . ? F13 C36 1.343(4) . ? F14 C37 1.350(4) . ? F15 C38 1.365(3) . ? C1 C2 1.480(4) . ? C1 H1A 0.99(3) . ? C1 H1B 0.95(3) . ? C2 C3 1.388(5) . ? C2 H2 1.00(3) . ? C3 C4 1.407(4) . ? C3 H3 1.01(3) . ? C4 C5 1.508(5) . ? C4 H4 0.94(3) . ? C5 H5A 1.08(4) . ? C5 H5B 0.97(4) . ? C5 H5C 0.90(4) . ? C6 C7 1.439(4) . ? C6 C10 1.446(4) . ? C7 C8 1.409(4) . ? C7 C11 1.499(5) . ? C8 C9 1.430(4) . ? C8 C12 1.496(5) . ? C9 C10 1.405(4) . ? C9 C13 1.488(4) . ? C10 C14 1.507(5) . ? C11 H11A 0.99(4) . ? C11 H11B 0.99(4) . ? C11 H11C 0.94(5) . ? C12 H12A 0.98(5) . ? C12 H12B 0.94(4) . ? C12 H12C 0.92(4) . ? C13 H13A 0.93(5) . ? C13 H13B 0.98(4) . ? C13 H13C 1.06(4) . ? C14 H14A 0.89(6) . ? C14 H14B 0.96(5) . ? C14 H14C 0.95(5) . ? C15 H15A 0.94(5) . ? C15 H15B 0.97(4) . ? C15 H15C 0.92(5) . ? C16 H16A 1.00(5) . ? C16 H16B 0.92(5) . ? C16 H16C 0.92(5) . ? C17 C19 1.528(5) . ? C17 C20 1.528(5) . ? C17 C18 1.534(5) . ? C18 H18A 0.97(4) . ? C18 H18B 0.95(4) . ? C18 H18C 1.02(4) . ? C19 H19A 0.97(3) . ? C19 H19B 0.96(4) . ? C19 H19C 1.03(3) . ? C20 H20A 0.99(4) . ? C20 H20B 0.97(4) . ? C20 H20C 1.00(4) . ? C21 C26 1.374(4) . ? C21 C22 1.376(4) . ? C22 C23 1.375(5) . ? C23 C24 1.360(6) . ? C24 C25 1.362(6) . ? C25 C26 1.383(5) . ? C27 C28 1.380(4) . ? C27 C32 1.387(4) . ? C28 C29 1.368(5) . ? C29 C30 1.375(5) . ? C30 C31 1.372(5) . ? C31 C32 1.373(5) . ? C33 C38 1.371(4) . ? C33 C34 1.385(4) . ? C34 C35 1.380(5) . ? C35 C36 1.371(5) . ? C36 C37 1.367(5) . ? C37 C38 1.383(4) . ? C39 C40 1.376(6) . ? C39 C44 1.416(6) . ? C39 C45 1.476(6) . ? C40 C41 1.385(7) . ? C40 H40 0.96 . ? C41 C42 1.366(7) . ? C41 H41 0.96 . ? C42 C43 1.388(7) . ? C42 H42 0.96 . ? C43 C44 1.367(6) . ? C43 H43 0.96 . ? C44 H44 0.96 . ? C45 H45A 0.96 . ? C45 H45B 0.96 . ? C45 H45C 0.96 . ? 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 N1 Ti1 C6 77.79(11) . . ? N1 Ti1 C2 137.55(11) . . ? C6 Ti1 C2 141.60(11) . . ? N1 Ti1 C4 98.95(11) . . ? C6 Ti1 C4 133.86(12) . . ? C2 Ti1 C4 66.50(12) . . ? N1 Ti1 C10 101.01(11) . . ? C6 Ti1 C10 37.29(10) . . ? C2 Ti1 C10 107.95(11) . . ? C4 Ti1 C10 153.52(12) . . ? N1 Ti1 C7 97.54(11) . . ? C6 Ti1 C7 36.80(11) . . ? C2 Ti1 C7 123.67(11) . . ? C4 Ti1 C7 100.45(12) . . ? C10 Ti1 C7 59.84(11) . . ? N1 Ti1 C3 131.70(11) . . ? C6 Ti1 C3 139.71(11) . . ? C2 Ti1 C3 35.06(11) . . ? C4 Ti1 C3 35.45(11) . . ? C10 Ti1 C3 127.25(11) . . ? C7 Ti1 C3 104.57(11) . . ? N1 Ti1 C1 104.74(11) . . ? C6 Ti1 C1 141.63(12) . . ? C2 Ti1 C1 37.34(11) . . ? C4 Ti1 C1 84.18(12) . . ? C10 Ti1 C1 107.14(11) . . ? C7 Ti1 C1 156.30(11) . . ? C3 Ti1 C1 66.10(12) . . ? N1 Ti1 C9 134.07(10) . . ? C6 Ti1 C9 59.07(10) . . ? C2 Ti1 C9 82.58(11) . . ? C4 Ti1 C9 121.55(12) . . ? C10 Ti1 C9 34.09(11) . . ? C7 Ti1 C9 57.31(10) . . ? C3 Ti1 C9 93.58(11) . . ? C1 Ti1 C9 100.35(11) . . ? N1 Ti1 C8 131.23(10) . . ? C6 Ti1 C8 58.77(11) . . ? C2 Ti1 C8 90.90(11) . . ? C4 Ti1 C8 96.33(12) . . ? C10 Ti1 C8 57.31(11) . . ? C7 Ti1 C8 33.96(10) . . ? C3 Ti1 C8 81.90(11) . . ? C1 Ti1 C8 122.77(11) . . ? C9 Ti1 C8 33.65(10) . . ? N1 Ti1 Si1 37.23(7) . . ? C6 Ti1 Si1 40.61(8) . . ? C2 Ti1 Si1 165.93(9) . . ? C4 Ti1 Si1 123.48(9) . . ? C10 Ti1 Si1 67.79(8) . . ? C7 Ti1 Si1 66.80(8) . . ? C3 Ti1 Si1 157.67(9) . . ? C1 Ti1 Si1 129.60(8) . . ? C9 Ti1 Si1 97.95(8) . . ? C8 Ti1 Si1 97.29(8) . . ? N1 Ti1 H1A 82.6(9) . . ? C6 Ti1 H1A 145.3(8) . . ? C2 Ti1 H1A 55.8(9) . . ? C4 Ti1 H1A 77.2(8) . . ? C10 Ti1 H1A 122.5(8) . . ? C7 Ti1 H1A 177.6(8) . . ? C3 Ti1 H1A 73.7(8) . . ? C1 Ti1 H1A 24.5(9) . . ? C9 Ti1 H1A 124.2(9) . . ? C8 Ti1 H1A 146.1(9) . . ? Si1 Ti1 H1A 114.2(8) . . ? C33 Al1 C27 113.14(13) . . ? C33 Al1 C21 109.07(13) . . ? C27 Al1 C21 111.68(13) . . ? C33 Al1 C1 108.24(13) . . ? C27 Al1 C1 103.79(13) . . ? C21 Al1 C1 110.79(13) . . ? N1 Si1 C16 116.7(2) . . ? N1 Si1 C15 116.4(2) . . ? C16 Si1 C15 105.7(2) . . ? N1 Si1 C6 92.72(12) . . ? C16 Si1 C6 113.0(2) . . ? C15 Si1 C6 112.2(2) . . ? N1 Si1 Ti1 42.13(8) . . ? C16 Si1 Ti1 129.56(15) . . ? C15 Si1 Ti1 124.71(14) . . ? C6 Si1 Ti1 50.66(9) . . ? C17 N1 Si1 120.7(2) . . ? C17 N1 Ti1 138.3(2) . . ? Si1 N1 Ti1 100.64(12) . . ? C2 C1 Al1 108.4(2) . . ? C2 C1 Ti1 67.8(2) . . ? Al1 C1 Ti1 169.8(2) . . ? C2 C1 H1A 117.1(19) . . ? Al1 C1 H1A 101.9(19) . . ? Ti1 C1 H1A 72.8(19) . . ? C2 C1 H1B 112.5(18) . . ? Al1 C1 H1B 106.1(18) . . ? Ti1 C1 H1B 84.0(18) . . ? H1A C1 H1B 109.8(26) . . ? C3 C2 C1 126.5(3) . . ? C3 C2 Ti1 75.7(2) . . ? C1 C2 Ti1 74.9(2) . . ? C3 C2 H2 117.7(18) . . ? C1 C2 H2 115.8(18) . . ? Ti1 C2 H2 122.7(18) . . ? C2 C3 C4 125.7(3) . . ? C2 C3 Ti1 69.2(2) . . ? C4 C3 Ti1 69.8(2) . . ? C2 C3 H3 114.3(17) . . ? C4 C3 H3 118.5(17) . . ? Ti1 C3 H3 127.2(17) . . ? C3 C4 C5 120.6(3) . . ? C3 C4 Ti1 74.8(2) . . ? C5 C4 Ti1 132.8(3) . . ? C3 C4 H4 114.6(21) . . ? C5 C4 H4 117.0(21) . . ? Ti1 C4 H4 88.1(21) . . ? C4 C5 H5A 111.0(19) . . ? C4 C5 H5B 111.9(24) . . ? H5A C5 H5B 104.9(30) . . ? C4 C5 H5C 113.2(25) . . ? H5A C5 H5C 108.9(31) . . ? H5B C5 H5C 106.5(34) . . ? C7 C6 C10 106.1(3) . . ? C7 C6 Si1 121.7(2) . . ? C10 C6 Si1 123.0(2) . . ? C7 C6 Ti1 75.6(2) . . ? C10 C6 Ti1 74.2(2) . . ? Si1 C6 Ti1 88.73(11) . . ? C8 C7 C6 108.7(3) . . ? C8 C7 C11 124.2(3) . . ? C6 C7 C11 127.0(3) . . ? C8 C7 Ti1 78.8(2) . . ? C6 C7 Ti1 67.6(2) . . ? C11 C7 Ti1 121.2(2) . . ? C7 C8 C9 108.3(3) . . ? C7 C8 C12 126.3(3) . . ? C9 C8 C12 125.2(3) . . ? C7 C8 Ti1 67.2(2) . . ? C9 C8 Ti1 72.8(2) . . ? C12 C8 Ti1 130.8(2) . . ? C10 C9 C8 108.0(3) . . ? C10 C9 C13 127.0(3) . . ? C8 C9 C13 124.6(3) . . ? C10 C9 Ti1 66.4(2) . . ? C8 C9 Ti1 73.6(2) . . ? C13 C9 Ti1 130.9(2) . . ? C9 C10 C6 108.9(3) . . ? C9 C10 C14 124.5(3) . . ? C6 C10 C14 126.5(3) . . ? C9 C10 Ti1 79.5(2) . . ? C6 C10 Ti1 68.5(2) . . ? C14 C10 Ti1 120.0(2) . . ? C7 C11 H11A 110.9(23) . . ? C7 C11 H11B 107.7(23) . . ? H11A C11 H11B 116.1(32) . . ? C7 C11 H11C 112.1(33) . . ? H11A C11 H11C 107.3(39) . . ? H11B C11 H11C 102.5(38) . . ? C8 C12 H12A 113.1(26) . . ? C8 C12 H12B 108.0(26) . . ? H12A C12 H12B 102.0(35) . . ? C8 C12 H12C 106.6(24) . . ? H12A C12 H12C 112.8(34) . . ? H12B C12 H12C 114.4(35) . . ? C9 C13 H13A 113.9(28) . . ? C9 C13 H13B 110.2(25) . . ? H13A C13 H13B 114.3(37) . . ? C9 C13 H13C 113.4(23) . . ? H13A C13 H13C 105.7(35) . . ? H13B C13 H13C 98.3(33) . . ? C10 C14 H14A 112.9(36) . . ? C10 C14 H14B 116.5(27) . . ? H14A C14 H14B 107.7(42) . . ? C10 C14 H14C 110.2(28) . . ? H14A C14 H14C 108.6(42) . . ? H14B C14 H14C 100.1(36) . . ? Si1 C15 H15A 108.7(29) . . ? Si1 C15 H15B 115.0(23) . . ? H15A C15 H15B 109.1(36) . . ? Si1 C15 H15C 114.4(27) . . ? H15A C15 H15C 109.4(37) . . ? H15B C15 H15C 99.9(34) . . ? Si1 C16 H16A 107.1(28) . . ? Si1 C16 H16B 107.2(29) . . ? H16A C16 H16B 117.0(38) . . ? Si1 C16 H16C 112.1(30) . . ? H16A C16 H16C 107.8(40) . . ? H16B C16 H16C 105.8(40) . . ? N1 C17 C19 112.0(3) . . ? N1 C17 C20 111.3(3) . . ? C19 C17 C20 107.2(3) . . ? N1 C17 C18 107.6(3) . . ? C19 C17 C18 109.5(3) . . ? C20 C17 C18 109.3(3) . . ? C17 C18 H18A 110.5(22) . . ? C17 C18 H18B 110.2(21) . . ? H18A C18 H18B 106.9(30) . . ? C17 C18 H18C 107.6(23) . . ? H18A C18 H18C 114.0(31) . . ? H18B C18 H18C 107.5(31) . . ? C17 C19 H19A 113.8(19) . . ? C17 C19 H19B 108.9(22) . . ? H19A C19 H19B 110.4(29) . . ? C17 C19 H19C 110.0(18) . . ? H19A C19 H19C 106.1(27) . . ? H19B C19 H19C 107.4(29) . . ? C17 C20 H20A 113.0(23) . . ? C17 C20 H20B 108.3(22) . . ? H20A C20 H20B 113.7(32) . . ? C17 C20 H20C 112.6(24) . . ? H20A C20 H20C 105.7(32) . . ? H20B C20 H20C 103.3(32) . . ? C26 C21 C22 113.5(3) . . ? C26 C21 Al1 118.9(2) . . ? C22 C21 Al1 127.6(2) . . ? F1 C22 C21 119.3(3) . . ? F1 C22 C23 116.1(3) . . ? C21 C22 C23 124.6(3) . . ? F2 C23 C24 119.9(3) . . ? F2 C23 C22 121.3(4) . . ? C24 C23 C22 118.9(3) . . ? F3 C24 C23 119.9(4) . . ? F3 C24 C25 120.2(4) . . ? C23 C24 C25 119.9(3) . . ? F4 C25 C24 120.4(3) . . ? F4 C25 C26 120.7(4) . . ? C24 C25 C26 118.9(3) . . ? F5 C26 C21 118.8(3) . . ? F5 C26 C25 117.1(3) . . ? C21 C26 C25 124.2(3) . . ? C28 C27 C32 113.2(3) . . ? C28 C27 Al1 126.4(2) . . ? C32 C27 Al1 120.3(2) . . ? F6 C28 C29 115.9(3) . . ? F6 C28 C27 119.3(3) . . ? C29 C28 C27 124.8(3) . . ? F7 C29 C28 121.2(3) . . ? F7 C29 C30 119.5(3) . . ? C28 C29 C30 119.3(3) . . ? F8 C30 C31 120.6(3) . . ? F8 C30 C29 120.4(3) . . ? C31 C30 C29 119.0(3) . . ? F9 C31 C30 119.5(3) . . ? F9 C31 C32 121.2(3) . . ? C30 C31 C32 119.3(3) . . ? F10 C32 C31 116.9(3) . . ? F10 C32 C27 118.7(3) . . ? C31 C32 C27 124.4(3) . . ? C38 C33 C34 114.2(3) . . ? C38 C33 Al1 120.3(2) . . ? C34 C33 Al1 125.4(2) . . ? F11 C34 C35 116.8(3) . . ? F11 C34 C33 119.7(3) . . ? C35 C34 C33 123.5(3) . . ? F12 C35 C36 119.3(3) . . ? F12 C35 C34 121.3(3) . . ? C36 C35 C34 119.4(3) . . ? F13 C36 C37 120.2(3) . . ? F13 C36 C35 120.2(3) . . ? C37 C36 C35 119.6(3) . . ? F14 C37 C36 120.1(3) . . ? F14 C37 C38 121.2(3) . . ? C36 C37 C38 118.7(3) . . ? F15 C38 C33 119.0(3) . . ? F15 C38 C37 116.5(3) . . ? C33 C38 C37 124.5(3) . . ? C40 C39 C44 117.1(4) . . ? C40 C39 C45 122.8(4) . . ? C44 C39 C45 120.2(4) . . ? C39 C40 C41 121.9(4) . . ? C39 C40 H40 119.1(3) . . ? C41 C40 H40 119.0(3) . . ? C42 C41 C40 120.8(5) . . ? C42 C41 H41 119.5(3) . . ? C40 C41 H41 119.7(3) . . ? C41 C42 C43 118.2(5) . . ? C41 C42 H42 121.1(3) . . ? C43 C42 H42 120.8(3) . . ? C44 C43 C42 121.7(5) . . ? C44 C43 H43 119.1(3) . . ? C42 C43 H43 119.1(3) . . ? C43 C44 C39 120.3(4) . . ? C43 C44 H44 119.7(3) . . ? C39 C44 H44 120.0(3) . . ? C39 C45 H45A 109.0(3) . . ? C39 C45 H45B 109.4(2) . . ? H45A C45 H45B 109.5 . . ? C39 C45 H45C 110.0(2) . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? _refine_diff_density_max 0.486 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.062