Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Cristina Santamaria' _publ_contact_author_address ; Quimica Inorganica Universidad de Alcala Campus Universitario Alcala de Henares Madrid 28871 SPAIN ; _publ_contact_author_email CRISTINA.SANTAMARIA@UAH.ES _publ_section_title ; Group 13 Organoderivatives Supported on a Molecular Metallic Oxide. ; _publ_requested_category FM loop_ _publ_author_name 'Cristina Santamaria' 'O.Gonzalez-del Moral' 'Alberto Hernan-Gomez' 'Avelino Martin' ; M.Mena ; data_3 _database_code_depnum_ccdc_archive 'CCDC 660805' _audit_creation_date 2007-06-04T10:54:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C63 H97 Al1 O8 Ti6, C6 H14' _chemical_formula_sum 'C69 H111 Al1 O8 Ti6' _chemical_formula_weight 1382.96 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.039(7) _cell_length_b 26.797(7) _cell_length_c 13.441(8) _cell_angle_alpha 90 _cell_angle_beta 101.57(5) _cell_angle_gamma 90 _cell_volume 8482(6) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 152 _cell_measurement_theta_min 4 _cell_measurement_theta_max 20 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_diffrn 1.083 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2936 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -4 1 0.102 0 5 -1 0.044 18 -4 -5 0.088 -4 1 1 0.126 1 9 -19 0.055 1 2 11 0.073 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.59 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.8429 _exptl_absorpt_correction_T_max 0.8762 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1028 _diffrn_reflns_av_unetI/netI 0.0862 _diffrn_reflns_number 84262 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.12 _diffrn_reflns_theta_full 25.12 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 7496 _reflns_number_gt 4750 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1141P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7496 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1058 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.1987 _refine_ls_wR_factor_gt 0.1796 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.456 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.093 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' O O 0.0106 0.006 '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' 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 C1 C 0.3690(2) 0.1908(2) 0.4056(4) 0.0338(12) Uani 1 1 d . . . H1 H 0.3458 0.193 0.4576 0.041 Uiso 1 1 d R . . C3 C 0.5 0.0404(3) 0.25 0.050(2) Uani 1 2 d S . . H3A H 0.5244 0.0282 0.2058 0.06 Uiso 0.5 1 d PR . . H3B H 0.5133 0.0283 0.3169 0.06 Uiso 0.5 1 d PR . . H3C H 0.462 0.0287 0.2241 0.06 Uiso 0.5 1 d PR . . C11 C 0.3259(2) 0.0584(2) 0.3069(4) 0.0348(12) Uani 1 1 d . . . C12 C 0.2899(2) 0.0919(2) 0.3485(4) 0.0327(11) Uani 1 1 d . . . C13 C 0.2600(2) 0.1218(2) 0.2674(4) 0.0371(12) Uani 1 1 d . . . C14 C 0.2782(2) 0.1080(2) 0.1766(4) 0.0416(14) Uani 1 1 d . . . C15 C 0.3197(2) 0.0692(2) 0.2001(4) 0.0349(12) Uani 1 1 d . . . C16 C 0.3651(3) 0.0193(2) 0.3636(5) 0.0494(15) Uani 1 1 d . . . H16A H 0.3536 0.0117 0.4279 0.074 Uiso 1 1 calc R . . H16B H 0.4041 0.032 0.3774 0.074 Uiso 1 1 calc R . . H16C H 0.3629 -0.011 0.3223 0.074 Uiso 1 1 calc R . . C17 C 0.2787(3) 0.0894(3) 0.4543(4) 0.0502(16) Uani 1 1 d . . . H17A H 0.3033 0.0641 0.4933 0.075 Uiso 1 1 calc R . . H17B H 0.2388 0.0805 0.4514 0.075 Uiso 1 1 calc R . . H17C H 0.2866 0.122 0.4872 0.075 Uiso 1 1 calc R . . C18 C 0.2133(3) 0.1569(3) 0.2783(6) 0.0599(18) Uani 1 1 d . . . H18A H 0.1772 0.1388 0.2675 0.09 Uiso 1 1 calc R . . H18B H 0.2109 0.1836 0.2278 0.09 Uiso 1 1 calc R . . H18C H 0.2212 0.1714 0.3466 0.09 Uiso 1 1 calc R . . C19 C 0.2570(3) 0.1297(3) 0.0707(5) 0.067(2) Uani 1 1 d . . . H19A H 0.2261 0.1532 0.0726 0.1 Uiso 1 1 calc R . . H19B H 0.2432 0.1026 0.0231 0.1 Uiso 1 1 calc R . . H19C H 0.2883 0.1471 0.0485 0.1 Uiso 1 1 calc R . . C20 C 0.3468(3) 0.0433(3) 0.1226(5) 0.0583(18) Uani 1 1 d . . . H20A H 0.3746 0.0657 0.1015 0.088 Uiso 1 1 calc R . . H20B H 0.3175 0.0344 0.0634 0.088 Uiso 1 1 calc R . . H20C H 0.366 0.013 0.1525 0.088 Uiso 1 1 calc R . . C21 C 0.3918(2) 0.3365(2) 0.3139(5) 0.0423(13) Uani 1 1 d . . . C22 C 0.3641(2) 0.3206(2) 0.2150(4) 0.0366(13) Uani 1 1 d . . . C23 C 0.3110(2) 0.2979(2) 0.2220(4) 0.0346(12) Uani 1 1 d . . . C24 C 0.3070(2) 0.2992(2) 0.3278(4) 0.0388(13) Uani 1 1 d . . . C25 C 0.3570(2) 0.3231(2) 0.3826(4) 0.0396(13) Uani 1 1 d . . . C26 C 0.4487(3) 0.3639(3) 0.3402(6) 0.0605(18) Uani 1 1 d . . . H26A H 0.4784 0.3405 0.3715 0.091 Uiso 1 1 calc R . . H26B H 0.4459 0.3911 0.3879 0.091 Uiso 1 1 calc R . . H26C H 0.4581 0.3777 0.2782 0.091 Uiso 1 1 calc R . . C27 C 0.3884(3) 0.3252(3) 0.1189(5) 0.0597(18) Uani 1 1 d . . . H27A H 0.4201 0.3019 0.1224 0.09 Uiso 1 1 calc R . . H27B H 0.4018 0.3594 0.1129 0.09 Uiso 1 1 calc R . . H27C H 0.3588 0.3173 0.0595 0.09 Uiso 1 1 calc R . . C28 C 0.2686(3) 0.2764(3) 0.1361(5) 0.0517(16) Uani 1 1 d . . . H28A H 0.2816 0.2815 0.0723 0.078 Uiso 1 1 calc R . . H28B H 0.2318 0.2929 0.1324 0.078 Uiso 1 1 calc R . . H28C H 0.2645 0.2405 0.1474 0.078 Uiso 1 1 calc R . . C29 C 0.2571(3) 0.2838(3) 0.3721(6) 0.065(2) Uani 1 1 d . . . H29A H 0.2481 0.3103 0.4166 0.098 Uiso 1 1 calc R . . H29B H 0.2663 0.253 0.4114 0.098 Uiso 1 1 calc R . . H29C H 0.2242 0.2779 0.3171 0.098 Uiso 1 1 calc R . . C30 C 0.3658(3) 0.3362(3) 0.4967(5) 0.0614(19) Uani 1 1 d . . . H30A H 0.3467 0.3678 0.5049 0.092 Uiso 1 1 calc R . . H30B H 0.4065 0.3395 0.5251 0.092 Uiso 1 1 calc R . . H30C H 0.3497 0.3097 0.5326 0.092 Uiso 1 1 calc R . . C31 C 0.5462(2) 0.1811(2) 0.5683(4) 0.0410(14) Uani 1 1 d . . . C32 C 0.5074(2) 0.2177(2) 0.5884(3) 0.0383(13) Uani 1 1 d . . . C33 C 0.4582(2) 0.1928(2) 0.6036(3) 0.0408(14) Uani 1 1 d . . . C34 C 0.4670(2) 0.1407(2) 0.5958(4) 0.0388(13) Uani 1 1 d . . . C35 C 0.5221(2) 0.1338(2) 0.5727(4) 0.0415(14) Uani 1 1 d . . . C36 C 0.6055(3) 0.1904(3) 0.5534(5) 0.062(2) Uani 1 1 d . . . H36A H 0.6206 0.1599 0.5287 0.093 Uiso 1 1 calc R . . H36B H 0.6295 0.2003 0.6182 0.093 Uiso 1 1 calc R . . H36C H 0.6051 0.2172 0.5036 0.093 Uiso 1 1 calc R . . C37 C 0.5184(4) 0.2738(3) 0.5912(5) 0.070(2) Uani 1 1 d . . . H37A H 0.4929 0.2903 0.6293 0.105 Uiso 1 1 calc R . . H37B H 0.5115 0.2869 0.5217 0.105 Uiso 1 1 calc R . . H37C H 0.5579 0.2803 0.6243 0.105 Uiso 1 1 calc R . . C38 C 0.4099(3) 0.2166(3) 0.6470(5) 0.061(2) Uani 1 1 d . . . H38A H 0.4239 0.2254 0.7185 0.091 Uiso 1 1 calc R . . H38B H 0.3784 0.1929 0.6419 0.091 Uiso 1 1 calc R . . H38C H 0.3966 0.2468 0.6084 0.091 Uiso 1 1 calc R . . C39 C 0.4265(3) 0.1003(3) 0.6162(5) 0.075(2) Uani 1 1 d . . . H39A H 0.3886 0.1147 0.6126 0.112 Uiso 1 1 calc R . . H39B H 0.4402 0.0863 0.6839 0.112 Uiso 1 1 calc R . . H39C H 0.4244 0.0739 0.5651 0.112 Uiso 1 1 calc R . . C40 C 0.5477(4) 0.0826(3) 0.5583(5) 0.076(2) Uani 1 1 d . . . H40A H 0.5825 0.0779 0.6096 0.114 Uiso 1 1 calc R . . H40B H 0.5565 0.0806 0.4904 0.114 Uiso 1 1 calc R . . H40C H 0.5203 0.0564 0.5659 0.114 Uiso 1 1 calc R . . Al1 Al 0.5 0.11472(8) 0.25 0.0259(4) Uani 1 2 d S . . O1 O 0.53483(14) 0.15242(13) 0.3566(2) 0.0290(8) Uani 1 1 d . . . O12 O 0.36990(14) 0.19751(13) 0.2082(2) 0.0305(8) Uani 1 1 d . . . O13 O 0.43741(14) 0.12290(13) 0.3264(2) 0.0304(8) Uani 1 1 d . . . O23 O 0.46374(14) 0.23757(13) 0.3648(2) 0.0307(8) Uani 1 1 d . . . Ti1 Ti 0.36124(4) 0.14245(3) 0.28757(6) 0.0257(2) Uani 1 1 d . . . Ti2 Ti 0.38687(4) 0.24568(3) 0.31000(6) 0.0268(2) Uani 1 1 d . . . Ti3 Ti 0.46701(3) 0.17657(3) 0.42728(6) 0.0250(2) Uani 1 1 d . . . H2 H 0.562(2) 0.181(2) 0.325(4) 0.041(15) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.024(2) 0.050(3) 0.027(3) 0.005(2) 0.005(2) 0.007(2) C3 0.054(5) 0.039(5) 0.067(6) 0 0.038(5) 0 C11 0.035(3) 0.031(3) 0.042(3) 0.004(2) 0.016(2) -0.007(2) C12 0.036(3) 0.035(3) 0.032(3) 0.001(2) 0.019(2) -0.003(2) C13 0.027(3) 0.035(3) 0.051(3) 0.003(3) 0.012(2) -0.002(2) C14 0.030(3) 0.051(4) 0.040(3) -0.003(3) -0.001(2) -0.006(3) C15 0.040(3) 0.034(3) 0.033(3) -0.012(2) 0.013(2) -0.011(2) C16 0.054(4) 0.032(3) 0.063(4) 0.007(3) 0.012(3) 0.003(3) C17 0.056(4) 0.058(4) 0.044(3) 0.007(3) 0.026(3) -0.003(3) C18 0.039(3) 0.065(4) 0.079(5) 0.013(4) 0.018(3) 0.011(3) C19 0.057(4) 0.095(6) 0.040(4) 0.013(4) -0.009(3) -0.019(4) C20 0.056(4) 0.074(5) 0.053(4) -0.024(3) 0.030(3) -0.013(4) C21 0.044(3) 0.034(3) 0.053(3) 0.004(3) 0.017(3) 0.004(3) C22 0.039(3) 0.036(3) 0.037(3) 0.017(2) 0.013(2) 0.017(2) C23 0.024(3) 0.042(3) 0.037(3) 0.011(2) 0.004(2) 0.010(2) C24 0.038(3) 0.042(3) 0.041(3) 0.010(2) 0.018(2) 0.023(3) C25 0.047(3) 0.032(3) 0.043(3) -0.005(2) 0.016(3) 0.015(3) C26 0.041(4) 0.060(4) 0.079(5) -0.010(4) 0.009(3) -0.004(3) C27 0.067(4) 0.079(5) 0.040(3) 0.024(3) 0.026(3) 0.010(4) C28 0.042(3) 0.062(4) 0.049(4) 0.020(3) 0.002(3) 0.002(3) C29 0.056(4) 0.065(5) 0.088(5) 0.004(4) 0.045(4) 0.004(3) C30 0.067(4) 0.062(4) 0.057(4) -0.022(3) 0.016(3) 0.022(4) C31 0.032(3) 0.070(4) 0.019(2) 0.007(3) -0.001(2) 0.007(3) C32 0.043(3) 0.059(4) 0.011(2) -0.007(2) 0.001(2) -0.004(3) C33 0.042(3) 0.071(4) 0.011(2) -0.002(2) 0.007(2) 0.018(3) C34 0.049(3) 0.052(4) 0.016(2) 0.007(2) 0.008(2) 0.001(3) C35 0.044(3) 0.059(4) 0.019(2) 0.024(2) 0.002(2) 0.019(3) C36 0.033(3) 0.120(7) 0.035(3) 0.000(4) 0.010(3) 0.001(4) C37 0.105(6) 0.067(5) 0.032(3) -0.004(3) -0.002(4) -0.009(4) C38 0.042(3) 0.109(6) 0.033(3) -0.002(3) 0.012(3) 0.026(4) C39 0.072(5) 0.105(7) 0.047(4) 0.024(4) 0.013(4) -0.026(5) C40 0.103(6) 0.078(5) 0.048(4) 0.027(4) 0.016(4) 0.045(5) Al1 0.0279(10) 0.0284(11) 0.0237(10) 0 0.0107(8) 0 O1 0.0277(17) 0.037(2) 0.0222(16) 0.0006(14) 0.0062(13) 0.0020(15) O12 0.0287(18) 0.041(2) 0.0236(17) 0.0042(15) 0.0089(14) 0.0061(15) O13 0.0319(18) 0.0344(19) 0.0276(17) 0.0078(15) 0.0124(14) 0.0063(15) O23 0.0331(18) 0.039(2) 0.0215(16) -0.0010(14) 0.0078(14) 0.0041(15) Ti1 0.0249(4) 0.0313(5) 0.0218(4) 0.0018(4) 0.0070(3) 0.0014(4) Ti2 0.0275(5) 0.0305(5) 0.0228(4) 0.0029(4) 0.0057(3) 0.0077(4) Ti3 0.0247(4) 0.0356(5) 0.0152(4) 0.0029(4) 0.0051(3) 0.0062(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 Ti1 2.028(5) . ? C1 Ti2 2.055(5) . ? C1 Ti3 2.347(5) . ? C1 H1 0.9801 . ? C3 Al1 1.993(9) . ? C3 H3A 0.9702 . ? C3 H3B 0.9479 . ? C3 H3C 0.9622 . ? C11 C12 1.436(7) . ? C11 C15 1.442(8) . ? C11 C16 1.508(8) . ? C11 Ti1 2.439(5) . ? C12 C13 1.426(8) . ? C12 C17 1.501(7) . ? C12 Ti1 2.451(5) . ? C13 C14 1.425(8) . ? C13 C18 1.495(8) . ? C13 Ti1 2.456(5) . ? C14 C15 1.431(8) . ? C14 C19 1.526(8) . ? C14 Ti1 2.424(5) . ? C15 C20 1.505(8) . ? C15 Ti1 2.399(5) . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 C25 1.411(8) . ? C21 C22 1.427(8) . ? C21 C26 1.529(9) . ? C21 Ti2 2.437(6) . ? C22 C23 1.433(8) . ? C22 C27 1.526(8) . ? C22 Ti2 2.383(5) . ? C23 C24 1.445(8) . ? C23 C28 1.495(8) . ? C23 Ti2 2.412(5) . ? C24 C25 1.429(8) . ? C24 C29 1.500(8) . ? C24 Ti2 2.448(5) . ? C25 C30 1.547(8) . ? C25 Ti2 2.460(5) . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? C31 C35 1.399(9) . ? C31 C32 1.419(8) . ? C31 C36 1.498(8) . ? C31 Ti3 2.405(5) . ? C32 C33 1.409(8) . ? C32 C37 1.525(9) . ? C32 Ti3 2.451(5) . ? C33 C34 1.418(8) . ? C33 C38 1.538(8) . ? C33 Ti3 2.461(5) . ? C34 C35 1.432(8) . ? C34 C39 1.517(9) . ? C34 Ti3 2.460(5) . ? C35 C40 1.533(9) . ? C35 Ti3 2.418(5) . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? Al1 O1 1.815(4) . ? Al1 O1 1.815(4) 2_655 ? Al1 O13 1.997(3) . ? Al1 O13 1.997(3) 2_655 ? Al1 Ti3 3.1324(19) . ? Al1 Ti3 3.1324(19) 2_655 ? O1 Ti3 2.145(3) . ? O1 H2 1.13(6) . ? O12 Ti1 1.857(4) . ? O12 Ti2 1.866(4) . ? O13 Ti1 1.875(3) . ? O13 Ti3 2.006(4) . ? O23 Ti3 1.832(4) . ? O23 Ti2 1.860(4) . ? Ti1 Ti2 2.8370(15) . ? Ti1 Ti3 2.985(2) . ? Ti2 Ti3 2.8997(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 Ti1 C1 Ti2 88.0(2) . . ? Ti1 C1 Ti3 85.73(19) . . ? Ti2 C1 Ti3 82.12(19) . . ? Ti1 C1 H1 128.4 . . ? Ti2 C1 H1 128.5 . . ? Ti3 C1 H1 128.5 . . ? Al1 C3 H3A 109.6 . . ? Al1 C3 H3B 109.9 . . ? H3A C3 H3B 109.6 . . ? Al1 C3 H3C 109 . . ? H3A C3 H3C 108.5 . . ? H3B C3 H3C 110.3 . . ? C12 C11 C15 108.1(5) . . ? C12 C11 C16 126.9(5) . . ? C15 C11 C16 125.0(5) . . ? C12 C11 Ti1 73.4(3) . . ? C15 C11 Ti1 71.2(3) . . ? C16 C11 Ti1 120.0(4) . . ? C13 C12 C11 107.7(4) . . ? C13 C12 C17 126.2(5) . . ? C11 C12 C17 125.4(5) . . ? C13 C12 Ti1 73.3(3) . . ? C11 C12 Ti1 72.5(3) . . ? C17 C12 Ti1 127.7(4) . . ? C14 C13 C12 108.4(5) . . ? C14 C13 C18 127.8(5) . . ? C12 C13 C18 123.5(5) . . ? C14 C13 Ti1 71.8(3) . . ? C12 C13 Ti1 72.9(3) . . ? C18 C13 Ti1 126.5(4) . . ? C13 C14 C15 108.6(5) . . ? C13 C14 C19 126.7(6) . . ? C15 C14 C19 124.7(6) . . ? C13 C14 Ti1 74.3(3) . . ? C15 C14 Ti1 71.8(3) . . ? C19 C14 Ti1 120.5(4) . . ? C14 C15 C11 107.2(5) . . ? C14 C15 C20 124.2(5) . . ? C11 C15 C20 128.5(6) . . ? C14 C15 Ti1 73.7(3) . . ? C11 C15 Ti1 74.2(3) . . ? C20 C15 Ti1 121.4(4) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C25 C21 C22 107.8(5) . . ? C25 C21 C26 126.2(6) . . ? C22 C21 C26 126.0(6) . . ? C25 C21 Ti2 74.1(3) . . ? C22 C21 Ti2 70.7(3) . . ? C26 C21 Ti2 121.5(4) . . ? C21 C22 C23 108.7(5) . . ? C21 C22 C27 125.3(6) . . ? C23 C22 C27 125.9(5) . . ? C21 C22 Ti2 74.9(3) . . ? C23 C22 Ti2 73.7(3) . . ? C27 C22 Ti2 115.8(4) . . ? C22 C23 C24 106.9(5) . . ? C22 C23 C28 126.3(5) . . ? C24 C23 C28 126.8(5) . . ? C22 C23 Ti2 71.5(3) . . ? C24 C23 Ti2 74.1(3) . . ? C28 C23 Ti2 119.1(4) . . ? C25 C24 C23 107.6(5) . . ? C25 C24 C29 125.2(6) . . ? C23 C24 C29 126.9(6) . . ? C25 C24 Ti2 73.5(3) . . ? C23 C24 Ti2 71.4(3) . . ? C29 C24 Ti2 125.6(4) . . ? C21 C25 C24 109.0(5) . . ? C21 C25 C30 127.6(6) . . ? C24 C25 C30 123.1(5) . . ? C21 C25 Ti2 72.4(3) . . ? C24 C25 Ti2 72.6(3) . . ? C30 C25 Ti2 126.3(4) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C35 C31 C32 108.9(5) . . ? C35 C31 C36 124.8(6) . . ? C32 C31 C36 126.1(6) . . ? C35 C31 Ti3 73.6(3) . . ? C32 C31 Ti3 74.8(3) . . ? C36 C31 Ti3 121.8(4) . . ? C33 C32 C31 107.7(5) . . ? C33 C32 C37 127.6(6) . . ? C31 C32 C37 124.7(6) . . ? C33 C32 Ti3 73.7(3) . . ? C31 C32 Ti3 71.3(3) . . ? C37 C32 Ti3 120.1(4) . . ? C32 C33 C34 108.3(5) . . ? C32 C33 C38 125.3(6) . . ? C34 C33 C38 124.9(6) . . ? C32 C33 Ti3 72.9(3) . . ? C34 C33 Ti3 73.2(3) . . ? C38 C33 Ti3 131.0(4) . . ? C33 C34 C35 107.6(5) . . ? C33 C34 C39 125.3(6) . . ? C35 C34 C39 127.0(6) . . ? C33 C34 Ti3 73.3(3) . . ? C35 C34 Ti3 71.3(3) . . ? C39 C34 Ti3 124.3(4) . . ? C31 C35 C34 107.6(5) . . ? C31 C35 C40 128.7(6) . . ? C34 C35 C40 123.7(6) . . ? C31 C35 Ti3 72.6(3) . . ? C34 C35 Ti3 74.5(3) . . ? C40 C35 Ti3 119.4(4) . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O1 Al1 O1 112.4(2) . 2_655 ? O1 Al1 C3 123.82(12) . . ? O1 Al1 C3 123.82(12) 2_655 . ? O1 Al1 O13 78.96(15) . . ? O1 Al1 O13 93.97(15) 2_655 . ? C3 Al1 O13 96.30(12) . . ? O1 Al1 O13 93.97(15) . 2_655 ? O1 Al1 O13 78.96(15) 2_655 2_655 ? C3 Al1 O13 96.30(12) . 2_655 ? O13 Al1 O13 167.4(2) . 2_655 ? O1 Al1 Ti3 41.57(11) . . ? O1 Al1 Ti3 99.15(13) 2_655 . ? C3 Al1 Ti3 121.95(4) . . ? O13 Al1 Ti3 38.62(11) . . ? O13 Al1 Ti3 131.70(12) 2_655 . ? O1 Al1 Ti3 99.15(13) . 2_655 ? O1 Al1 Ti3 41.57(11) 2_655 2_655 ? C3 Al1 Ti3 121.95(4) . 2_655 ? O13 Al1 Ti3 131.70(12) . 2_655 ? O13 Al1 Ti3 38.62(11) 2_655 2_655 ? Ti3 Al1 Ti3 116.11(8) . 2_655 ? Al1 O1 Ti3 104.27(15) . . ? Al1 O1 H2 107(3) . . ? Ti3 O1 H2 120(3) . . ? Ti1 O12 Ti2 99.31(16) . . ? Ti1 O13 Al1 132.98(17) . . ? Ti1 O13 Ti3 100.49(16) . . ? Al1 O13 Ti3 102.97(16) . . ? Ti3 O23 Ti2 103.52(18) . . ? O12 Ti1 O13 99.58(15) . . ? O12 Ti1 C1 86.47(19) . . ? O13 Ti1 C1 91.69(18) . . ? O12 Ti1 C15 116.86(17) . . ? O13 Ti1 C15 101.26(18) . . ? C1 Ti1 C15 150.4(2) . . ? O12 Ti1 C14 97.04(18) . . ? O13 Ti1 C14 134.68(19) . . ? C1 Ti1 C14 131.3(2) . . ? C15 Ti1 C14 34.5(2) . . ? O12 Ti1 C11 151.22(17) . . ? O13 Ti1 C11 93.06(17) . . ? C1 Ti1 C11 119.1(2) . . ? C15 Ti1 C11 34.67(18) . . ? C14 Ti1 C11 56.79(19) . . ? O12 Ti1 C12 142.92(17) . . ? O13 Ti1 C12 117.50(17) . . ? C1 Ti1 C12 93.0(2) . . ? C15 Ti1 C12 57.41(17) . . ? C14 Ti1 C12 56.62(19) . . ? C11 Ti1 C12 34.14(17) . . ? O12 Ti1 C13 109.77(17) . . ? O13 Ti1 C13 149.09(17) . . ? C1 Ti1 C13 99.4(2) . . ? C15 Ti1 C13 57.04(19) . . ? C14 Ti1 C13 33.94(19) . . ? C11 Ti1 C13 56.34(18) . . ? C12 Ti1 C13 33.78(18) . . ? O12 Ti1 Ti2 40.46(11) . . ? O13 Ti1 Ti2 93.66(11) . . ? C1 Ti1 Ti2 46.37(15) . . ? C15 Ti1 Ti2 155.43(14) . . ? C14 Ti1 Ti2 124.86(15) . . ? C11 Ti1 Ti2 164.14(13) . . ? C12 Ti1 Ti2 130.93(13) . . ? C13 Ti1 Ti2 114.87(14) . . ? O12 Ti1 Ti3 86.47(11) . . ? O13 Ti1 Ti3 41.37(11) . . ? C1 Ti1 Ti3 51.63(14) . . ? C15 Ti1 Ti3 140.98(14) . . ? C14 Ti1 Ti3 175.42(15) . . ? C11 Ti1 Ti3 119.11(13) . . ? C12 Ti1 Ti3 121.58(13) . . ? C13 Ti1 Ti3 146.96(14) . . ? Ti2 Ti1 Ti3 59.67(3) . . ? O23 Ti2 O12 105.27(15) . . ? O23 Ti2 C1 89.11(18) . . ? O12 Ti2 C1 85.47(19) . . ? O23 Ti2 C22 114.45(18) . . ? O12 Ti2 C22 101.37(18) . . ? C1 Ti2 C22 152.1(2) . . ? O23 Ti2 C23 148.81(18) . . ? O12 Ti2 C23 90.55(17) . . ? C1 Ti2 C23 119.32(19) . . ? C22 Ti2 C23 34.78(18) . . ? O23 Ti2 C21 93.91(18) . . ? O12 Ti2 C21 135.18(18) . . ? C1 Ti2 C21 135.8(2) . . ? C22 Ti2 C21 34.4(2) . . ? C23 Ti2 C21 57.28(19) . . ? O23 Ti2 C24 140.05(18) . . ? O12 Ti2 C24 114.65(18) . . ? C1 Ti2 C24 95.3(2) . . ? C22 Ti2 C24 57.18(18) . . ? C23 Ti2 C24 34.59(18) . . ? C21 Ti2 C24 56.5(2) . . ? O23 Ti2 C25 106.69(18) . . ? O12 Ti2 C25 146.73(17) . . ? C1 Ti2 C25 104.0(2) . . ? C22 Ti2 C25 56.51(19) . . ? C23 Ti2 C25 56.84(19) . . ? C21 Ti2 C25 33.50(19) . . ? C24 Ti2 C25 33.9(2) . . ? O23 Ti2 Ti1 96.05(12) . . ? O12 Ti2 Ti1 40.23(11) . . ? C1 Ti2 Ti1 45.59(15) . . ? C22 Ti2 Ti1 137.98(15) . . ? C23 Ti2 Ti1 112.78(14) . . ? C21 Ti2 Ti1 170.00(14) . . ? C24 Ti2 Ti1 115.11(15) . . ? C25 Ti2 Ti1 142.19(15) . . ? O23 Ti2 Ti3 37.90(11) . . ? O12 Ti2 Ti3 88.88(11) . . ? C1 Ti2 Ti3 53.30(14) . . ? C22 Ti2 Ti3 152.30(14) . . ? C23 Ti2 Ti3 172.62(13) . . ? C21 Ti2 Ti3 127.02(15) . . ? C24 Ti2 Ti3 140.37(13) . . ? C25 Ti2 Ti3 122.53(14) . . ? Ti1 Ti2 Ti3 62.71(4) . . ? O23 Ti3 O13 110.68(14) . . ? O23 Ti3 O1 91.88(14) . . ? O13 Ti3 O1 71.49(13) . . ? O23 Ti3 C1 81.28(17) . . ? O13 Ti3 C1 79.71(17) . . ? O1 Ti3 C1 145.85(16) . . ? O23 Ti3 C31 105.71(19) . . ? O13 Ti3 C31 133.29(19) . . ? O1 Ti3 C31 79.16(16) . . ? C1 Ti3 C31 134.94(19) . . ? O23 Ti3 C35 139.40(19) . . ? O13 Ti3 C35 105.61(19) . . ? O1 Ti3 C35 82.73(16) . . ? C1 Ti3 C35 123.41(19) . . ? C31 Ti3 C35 33.7(2) . . ? O23 Ti3 C32 88.65(18) . . ? O13 Ti3 C32 160.67(17) . . ? O1 Ti3 C32 109.02(16) . . ? C1 Ti3 C32 104.26(19) . . ? C31 Ti3 C32 34.0(2) . . ? C35 Ti3 C32 56.2(2) . . ? O23 Ti3 C34 139.66(18) . . ? O13 Ti3 C34 106.05(17) . . ? O1 Ti3 C34 115.51(17) . . ? C1 Ti3 C34 89.53(19) . . ? C31 Ti3 C34 56.00(19) . . ? C35 Ti3 C34 34.14(19) . . ? C32 Ti3 C34 55.6(2) . . ? O23 Ti3 C33 106.24(19) . . ? O13 Ti3 C33 133.64(18) . . ? O1 Ti3 C33 134.44(16) . . ? C1 Ti3 C33 79.17(19) . . ? C31 Ti3 C33 55.95(18) . . ? C35 Ti3 C33 56.24(19) . . ? C32 Ti3 C33 33.3(2) . . ? C34 Ti3 C33 33.5(2) . . ? O23 Ti3 Ti2 38.58(11) . . ? O13 Ti3 Ti2 89.06(10) . . ? O1 Ti3 Ti2 115.66(10) . . ? C1 Ti3 Ti2 44.58(13) . . ? C31 Ti3 Ti2 136.98(17) . . ? C35 Ti3 Ti2 159.77(14) . . ? C32 Ti3 Ti2 107.17(15) . . ? C34 Ti3 Ti2 128.81(14) . . ? C33 Ti3 Ti2 103.55(14) . . ? O23 Ti3 Ti1 91.84(11) . . ? O13 Ti3 Ti1 38.14(10) . . ? O1 Ti3 Ti1 104.84(10) . . ? C1 Ti3 Ti1 42.64(13) . . ? C31 Ti3 Ti1 161.97(16) . . ? C35 Ti3 Ti1 128.50(16) . . ? C32 Ti3 Ti1 146.11(14) . . ? C34 Ti3 Ti1 107.57(14) . . ? C33 Ti3 Ti1 115.64(15) . . ? Ti2 Ti3 Ti1 57.62(4) . . ? O23 Ti3 Al1 96.75(11) . . ? O13 Ti3 Al1 38.40(9) . . ? O1 Ti3 Al1 34.16(9) . . ? C1 Ti3 Al1 113.12(14) . . ? C31 Ti3 Al1 110.16(14) . . ? C35 Ti3 Al1 100.56(15) . . ? C32 Ti3 Al1 142.62(14) . . ? C34 Ti3 Al1 122.74(15) . . ? C33 Ti3 Al1 155.55(14) . . ? Ti2 Ti3 Al1 99.57(5) . . ? Ti1 Ti3 Al1 70.92(4) . . ? # SQUEEZE RESULTS loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.013 0.000 0.000 1259.1 -11.3 _platon_squeeze_details ;One hexane molecule crystallized with every molecule of this compound. The disordered molecule was found in the difference fourier map, but it was not possible to get a chemical sensible model for it, so Squeeze procedure was used to remove its contribution to the structure factors. ; # Attachment '4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 660806' _audit_creation_date 2007-07-23T10:35:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C39 H61 B1 O3 Ti3' _chemical_formula_sum 'C39 H61 B1 O3 Ti3' _chemical_formula_weight 732.33 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.313(3) _cell_length_b 19.171(17) _cell_length_c 19.088(12) _cell_angle_alpha 90 _cell_angle_beta 105.61(3) _cell_angle_gamma 90 _cell_volume 3987(5) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 33 _cell_measurement_theta_min 3 _cell_measurement_theta_max 16 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.22 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.619 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_T_max 1.001 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1413 _diffrn_reflns_av_unetI/netI 0.107 _diffrn_reflns_number 48845 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 6984 _reflns_number_gt 4126 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+12.4795P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6984 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1341 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.1785 _refine_ls_wR_factor_gt 0.1428 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.453 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.091 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.4268(5) 0.0797(3) 0.8336(3) 0.0351(13) Uani 1 1 d . . . H1 H 0.4517 0.0472 0.8759 0.042 Uiso 1 1 calc R . . C11 C 0.2633(6) 0.2623(3) 0.9022(3) 0.0426(15) Uani 1 1 d . . . C12 C 0.3662(5) 0.2252(4) 0.9443(3) 0.0449(16) Uani 1 1 d . . . C13 C 0.3289(6) 0.1547(4) 0.9502(3) 0.0539(19) Uani 1 1 d . . . C14 C 0.2018(6) 0.1493(4) 0.9140(4) 0.0497(17) Uani 1 1 d . . . C15 C 0.1613(5) 0.2163(4) 0.8842(3) 0.0438(16) Uani 1 1 d . . . C16 C 0.2591(10) 0.3386(4) 0.8820(5) 0.087(3) Uani 1 1 d . . . H16A H 0.21 0.3446 0.8315 0.13 Uiso 1 1 calc R . . H16B H 0.3427 0.3556 0.8869 0.13 Uiso 1 1 calc R . . H16C H 0.2219 0.3653 0.9144 0.13 Uiso 1 1 calc R . . C17 C 0.4898(7) 0.2569(6) 0.9799(5) 0.097(4) Uani 1 1 d . . . H17A H 0.5429 0.2217 1.01 0.146 Uiso 1 1 calc R . . H17B H 0.4795 0.2962 1.0106 0.146 Uiso 1 1 calc R . . H17C H 0.5275 0.2734 0.9424 0.146 Uiso 1 1 calc R . . C18 C 0.4047(9) 0.0988(5) 0.9984(5) 0.100(4) Uani 1 1 d . . . H18A H 0.3739 0.0527 0.9802 0.15 Uiso 1 1 calc R . . H18B H 0.3984 0.1045 1.0483 0.15 Uiso 1 1 calc R . . H18C H 0.4908 0.1033 0.9978 0.15 Uiso 1 1 calc R . . C19 C 0.1207(10) 0.0864(5) 0.9107(6) 0.114(4) Uani 1 1 d . . . H19A H 0.1715 0.0456 0.9295 0.17 Uiso 1 1 calc R . . H19B H 0.0742 0.0779 0.8602 0.17 Uiso 1 1 calc R . . H19C H 0.0637 0.0949 0.9404 0.17 Uiso 1 1 calc R . . C20 C 0.0304(6) 0.2345(6) 0.8485(4) 0.087(3) Uani 1 1 d . . . H20A H 0.0271 0.2698 0.8108 0.13 Uiso 1 1 calc R . . H20B H -0.0079 0.2531 0.8849 0.13 Uiso 1 1 calc R . . H20C H -0.0139 0.1927 0.8262 0.13 Uiso 1 1 calc R . . C21 C 0.7322(5) 0.1111(4) 0.7652(4) 0.0434(16) Uani 1 1 d . . . C22 C 0.7392(5) 0.0844(3) 0.8363(4) 0.0432(16) Uani 1 1 d . . . C23 C 0.7357(5) 0.1417(4) 0.8833(4) 0.0438(15) Uani 1 1 d . . . C24 C 0.7271(5) 0.2045(3) 0.8433(4) 0.0426(16) Uani 1 1 d . . . C25 C 0.7217(5) 0.1856(4) 0.7696(4) 0.0476(17) Uani 1 1 d . . . C26 C 0.7324(7) 0.0713(5) 0.6973(5) 0.075(2) Uani 1 1 d . . . H26A H 0.6557 0.0803 0.6598 0.112 Uiso 1 1 calc R . . H26B H 0.7394 0.0212 0.7082 0.112 Uiso 1 1 calc R . . H26C H 0.8021 0.0863 0.6797 0.112 Uiso 1 1 calc R . . C27 C 0.7658(7) 0.0095(4) 0.8613(5) 0.074(3) Uani 1 1 d . . . H27A H 0.7059 -0.0057 0.8869 0.111 Uiso 1 1 calc R . . H27B H 0.8487 0.0064 0.8942 0.111 Uiso 1 1 calc R . . H27C H 0.76 -0.0206 0.819 0.111 Uiso 1 1 calc R . . C28 C 0.7527(6) 0.1327(5) 0.9642(4) 0.074(2) Uani 1 1 d . . . H28A H 0.6898 0.101 0.9723 0.111 Uiso 1 1 calc R . . H28B H 0.745 0.1782 0.9861 0.111 Uiso 1 1 calc R . . H28C H 0.8343 0.1133 0.9866 0.111 Uiso 1 1 calc R . . C29 C 0.7241(6) 0.2781(4) 0.8691(5) 0.074(3) Uani 1 1 d . . . H29A H 0.7847 0.3061 0.8533 0.11 Uiso 1 1 calc R . . H29B H 0.7435 0.2787 0.9224 0.11 Uiso 1 1 calc R . . H29C H 0.642 0.2978 0.8487 0.11 Uiso 1 1 calc R . . C30 C 0.7052(7) 0.2367(4) 0.7079(5) 0.077(3) Uani 1 1 d . . . H30A H 0.7007 0.2113 0.6626 0.116 Uiso 1 1 calc R . . H30B H 0.775 0.2689 0.7179 0.116 Uiso 1 1 calc R . . H30C H 0.6292 0.2631 0.7028 0.116 Uiso 1 1 calc R . . C31 C 0.1792(5) -0.0351(3) 0.7106(4) 0.0461(16) Uani 1 1 d . . . C32 C 0.2817(5) -0.0580(3) 0.7667(3) 0.0425(15) Uani 1 1 d . . . C33 C 0.3835(5) -0.0653(3) 0.7348(3) 0.0404(14) Uani 1 1 d . . . C34 C 0.3425(6) -0.0457(3) 0.6610(3) 0.0435(15) Uani 1 1 d . . . C35 C 0.2177(6) -0.0281(3) 0.6466(4) 0.0488(17) Uani 1 1 d . . . C36 C 0.0517(6) -0.0232(4) 0.7193(5) 0.072(2) Uani 1 1 d . . . H36A H 0.0499 -0.0365 0.7686 0.109 Uiso 1 1 calc R . . H36B H -0.0074 -0.0516 0.6838 0.109 Uiso 1 1 calc R . . H36C H 0.0301 0.0262 0.7112 0.109 Uiso 1 1 calc R . . C37 C 0.2852(7) -0.0771(4) 0.8436(4) 0.065(2) Uani 1 1 d . . . H37A H 0.3445 -0.0473 0.8774 0.098 Uiso 1 1 calc R . . H37B H 0.3097 -0.126 0.8525 0.098 Uiso 1 1 calc R . . H37C H 0.2035 -0.0705 0.8511 0.098 Uiso 1 1 calc R . . C38 C 0.5071(6) -0.0933(4) 0.7718(4) 0.063(2) Uani 1 1 d . . . H38A H 0.5271 -0.0821 0.8238 0.095 Uiso 1 1 calc R . . H38B H 0.5684 -0.0723 0.7505 0.095 Uiso 1 1 calc R . . H38C H 0.5073 -0.1441 0.7656 0.095 Uiso 1 1 calc R . . C39 C 0.4162(8) -0.0466(4) 0.6060(5) 0.075(2) Uani 1 1 d . . . H39A H 0.4924 -0.0727 0.6256 0.112 Uiso 1 1 calc R . . H39B H 0.4358 0.0014 0.5953 0.112 Uiso 1 1 calc R . . H39C H 0.3682 -0.069 0.5612 0.112 Uiso 1 1 calc R . . C40 C 0.1349(8) -0.0108(4) 0.5701(4) 0.077(3) Uani 1 1 d . . . H40A H 0.1775 0.022 0.5459 0.116 Uiso 1 1 calc R . . H40B H 0.0583 0.0103 0.5745 0.116 Uiso 1 1 calc R . . H40C H 0.1163 -0.0538 0.5414 0.116 Uiso 1 1 calc R . . C51 C 0.2394(5) 0.2328(3) 0.6399(3) 0.0368(14) Uani 1 1 d . . . H51 H 0.3302 0.2284 0.6606 0.044 Uiso 1 1 calc R . . C52 C 0.2068(5) 0.3115(3) 0.6286(4) 0.0452(16) Uani 1 1 d . . . H52A H 0.2455 0.3365 0.6744 0.054 Uiso 1 1 calc R . . H52B H 0.2432 0.3298 0.5906 0.054 Uiso 1 1 calc R . . C53 C 0.0678(6) 0.3284(4) 0.6064(4) 0.0512(17) Uani 1 1 d . . . H53A H 0.0569 0.3789 0.6133 0.061 Uiso 1 1 calc R . . H53B H 0.034 0.3179 0.554 0.061 Uiso 1 1 calc R . . C54 C -0.0059(5) 0.2873(3) 0.6499(4) 0.0438(15) Uani 1 1 d . . . H54A H 0.0056 0.3105 0.6976 0.053 Uiso 1 1 calc R . . H54B H -0.094 0.291 0.6237 0.053 Uiso 1 1 calc R . . C55 C 0.0256(5) 0.2095(3) 0.6636(3) 0.0331(13) Uani 1 1 d . . . H55 H -0.0172 0.1913 0.6994 0.04 Uiso 1 1 calc R . . C56 C -0.0109(5) 0.1645(3) 0.5945(3) 0.0435(15) Uani 1 1 d . . . H56A H -0.0994 0.1716 0.571 0.052 Uiso 1 1 calc R . . H56B H 0.0007 0.1148 0.6088 0.052 Uiso 1 1 calc R . . C57 C 0.0608(5) 0.1794(4) 0.5382(3) 0.0461(15) Uani 1 1 d . . . H57A H 0.0278 0.2225 0.5114 0.055 Uiso 1 1 calc R . . H57B H 0.0463 0.1407 0.5026 0.055 Uiso 1 1 calc R . . C58 C 0.2008(5) 0.1882(4) 0.5706(3) 0.0466(16) Uani 1 1 d . . . H58A H 0.238 0.1414 0.5816 0.056 Uiso 1 1 calc R . . H58B H 0.2353 0.2096 0.5332 0.056 Uiso 1 1 calc R . . O12 O 0.4472(3) 0.2189(2) 0.8042(2) 0.0338(9) Uani 1 1 d . . . O13 O 0.2183(3) 0.13086(19) 0.72996(19) 0.0309(8) Uani 1 1 d . . . O23 O 0.4531(3) 0.1041(2) 0.7007(2) 0.0371(9) Uani 1 1 d . . . Ti1 Ti 0.31373(8) 0.17756(5) 0.82402(5) 0.0278(2) Uani 1 1 d . . . Ti2 Ti 0.53946(8) 0.14180(5) 0.78890(6) 0.0315(3) Uani 1 1 d . . . Ti3 Ti 0.33174(9) 0.05715(5) 0.72953(6) 0.0316(3) Uani 1 1 d . . . B1 B 0.1730(5) 0.2019(3) 0.6982(3) 0.0285(14) Uani 1 1 d . . . H1A H 0.206(4) 0.230(3) 0.753(3) 0.030(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.028(3) 0.036(3) 0.039(3) 0.005(3) 0.006(2) 0.000(2) C11 0.058(4) 0.043(4) 0.036(3) -0.002(3) 0.027(3) 0.008(3) C12 0.031(3) 0.070(5) 0.036(3) -0.014(3) 0.013(3) -0.007(3) C13 0.054(4) 0.083(6) 0.030(3) 0.010(3) 0.021(3) 0.027(4) C14 0.048(4) 0.063(5) 0.048(4) -0.009(3) 0.031(3) -0.012(3) C15 0.025(3) 0.074(5) 0.034(3) -0.009(3) 0.012(2) 0.006(3) C16 0.149(9) 0.053(5) 0.076(6) -0.005(4) 0.061(6) 0.006(5) C17 0.046(4) 0.173(11) 0.073(6) -0.055(6) 0.018(4) -0.030(6) C18 0.137(8) 0.119(8) 0.063(5) 0.044(5) 0.057(6) 0.079(7) C19 0.149(9) 0.099(8) 0.129(9) -0.034(7) 0.100(8) -0.072(7) C20 0.042(4) 0.161(10) 0.059(5) -0.014(6) 0.018(4) 0.026(5) C21 0.022(3) 0.054(4) 0.056(4) -0.007(3) 0.013(3) 0.005(3) C22 0.015(3) 0.032(3) 0.076(5) 0.005(3) 0.002(3) -0.002(2) C23 0.017(3) 0.054(4) 0.056(4) 0.004(3) 0.002(3) -0.003(3) C24 0.015(3) 0.038(4) 0.072(5) 0.002(3) 0.006(3) -0.001(2) C25 0.022(3) 0.045(4) 0.078(5) 0.018(4) 0.017(3) 0.002(3) C26 0.047(4) 0.094(7) 0.088(6) -0.021(5) 0.025(4) 0.005(4) C27 0.049(4) 0.040(4) 0.117(7) 0.018(4) -0.006(4) 0.000(3) C28 0.038(4) 0.101(7) 0.071(5) 0.000(5) -0.004(3) 0.003(4) C29 0.034(4) 0.042(4) 0.142(8) -0.021(5) 0.019(4) -0.009(3) C30 0.054(4) 0.073(6) 0.114(7) 0.053(5) 0.038(4) 0.012(4) C31 0.032(3) 0.025(3) 0.077(5) -0.009(3) 0.008(3) -0.006(3) C32 0.041(3) 0.027(3) 0.055(4) 0.003(3) 0.005(3) -0.007(3) C33 0.036(3) 0.025(3) 0.058(4) -0.005(3) 0.009(3) 0.004(3) C34 0.054(4) 0.028(3) 0.047(4) -0.009(3) 0.012(3) -0.005(3) C35 0.049(4) 0.030(3) 0.056(4) -0.005(3) -0.005(3) -0.005(3) C36 0.038(4) 0.046(5) 0.130(8) -0.012(5) 0.017(4) -0.008(3) C37 0.086(6) 0.034(4) 0.084(6) 0.002(4) 0.036(4) -0.005(4) C38 0.045(4) 0.038(4) 0.094(6) 0.005(4) -0.001(4) 0.002(3) C39 0.106(7) 0.052(5) 0.079(6) -0.010(4) 0.047(5) 0.004(5) C40 0.091(6) 0.060(5) 0.056(5) -0.019(4) -0.024(4) 0.003(4) C51 0.024(3) 0.047(4) 0.039(3) 0.007(3) 0.007(2) -0.002(3) C52 0.038(3) 0.037(4) 0.060(4) 0.011(3) 0.011(3) -0.008(3) C53 0.046(4) 0.039(4) 0.065(4) 0.014(3) 0.009(3) -0.002(3) C54 0.030(3) 0.044(4) 0.056(4) 0.011(3) 0.008(3) 0.010(3) C55 0.028(3) 0.033(3) 0.038(3) 0.008(3) 0.009(2) 0.000(2) C56 0.033(3) 0.045(4) 0.047(4) 0.007(3) 0.002(3) -0.006(3) C57 0.048(4) 0.051(4) 0.034(3) 0.001(3) 0.001(3) -0.004(3) C58 0.049(4) 0.060(4) 0.034(3) 0.003(3) 0.016(3) -0.007(3) O12 0.0202(18) 0.032(2) 0.049(2) -0.0006(18) 0.0085(16) -0.0030(16) O13 0.0252(18) 0.030(2) 0.036(2) 0.0034(17) 0.0064(16) -0.0024(16) O23 0.035(2) 0.035(2) 0.043(2) -0.0006(18) 0.0144(18) 0.0026(18) Ti1 0.0212(4) 0.0322(6) 0.0307(5) 0.0000(4) 0.0081(4) -0.0001(4) Ti2 0.0213(5) 0.0311(6) 0.0431(6) -0.0001(5) 0.0107(4) -0.0013(4) Ti3 0.0276(5) 0.0279(6) 0.0377(6) -0.0007(5) 0.0059(4) 0.0006(4) B1 0.025(3) 0.032(4) 0.026(3) 0.000(3) 0.003(2) 0.001(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 Ti3 2.034(6) . ? C1 Ti2 2.087(6) . ? C1 Ti1 2.250(6) . ? C1 H1 1 . ? C11 C12 1.416(9) . ? C11 C15 1.420(9) . ? C11 C16 1.511(10) . ? C11 Ti1 2.377(6) . ? C12 C13 1.430(10) . ? C12 C17 1.508(9) . ? C12 Ti1 2.393(6) . ? C13 C14 1.422(9) . ? C13 C18 1.518(10) . ? C13 Ti1 2.409(6) . ? C14 C15 1.429(10) . ? C14 C19 1.505(10) . ? C14 Ti1 2.452(6) . ? C15 C20 1.496(9) . ? C15 Ti1 2.432(5) . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 C22 1.432(9) . ? C21 C25 1.437(9) . ? C21 C26 1.505(10) . ? C21 Ti2 2.416(5) . ? C22 C23 1.425(9) . ? C22 C27 1.517(9) . ? C22 Ti2 2.457(5) . ? C23 C24 1.415(9) . ? C23 C28 1.514(10) . ? C23 Ti2 2.454(6) . ? C24 C25 1.437(9) . ? C24 C29 1.500(9) . ? C24 Ti2 2.417(6) . ? C25 C30 1.505(9) . ? C25 Ti2 2.346(5) . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? C31 C35 1.409(10) . ? C31 C32 1.419(9) . ? C31 C36 1.513(9) . ? C31 Ti3 2.429(6) . ? C32 C33 1.447(9) . ? C32 C37 1.503(9) . ? C32 Ti3 2.432(6) . ? C33 C34 1.409(9) . ? C33 C38 1.487(8) . ? C33 Ti3 2.415(6) . ? C34 C35 1.406(9) . ? C34 C39 1.507(9) . ? C34 Ti3 2.388(6) . ? C35 C40 1.543(9) . ? C35 Ti3 2.396(6) . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C51 C58 1.536(8) . ? C51 C52 1.554(9) . ? C51 B1 1.614(8) . ? C51 H51 1 . ? C52 C53 1.548(8) . ? C52 H52A 0.99 . ? C52 H52B 0.99 . ? C53 C54 1.542(8) . ? C53 H53A 0.99 . ? C53 H53B 0.99 . ? C54 C55 1.540(8) . ? C54 H54A 0.99 . ? C54 H54B 0.99 . ? C55 C56 1.538(8) . ? C55 B1 1.627(8) . ? C55 H55 1 . ? C56 C57 1.538(8) . ? C56 H56A 0.99 . ? C56 H56B 0.99 . ? C57 C58 1.547(8) . ? C57 H57A 0.99 . ? C57 H57B 0.99 . ? C58 H58A 0.99 . ? C58 H58B 0.99 . ? O12 Ti1 1.833(4) . ? O12 Ti2 1.877(4) . ? O13 B1 1.522(7) . ? O13 Ti3 1.911(4) . ? O13 Ti1 2.037(4) . ? O23 Ti3 1.845(4) . ? O23 Ti2 1.852(4) . ? Ti1 B1 2.541(6) . ? Ti1 Ti2 2.8919(15) . ? Ti1 Ti3 2.970(2) . ? Ti1 H1A 1.86(5) . ? Ti2 Ti3 2.8297(17) . ? B1 H1A 1.14(5) . ? 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 Ti3 C1 Ti2 86.7(2) . . ? Ti3 C1 Ti1 87.6(2) . . ? Ti2 C1 Ti1 83.6(2) . . ? Ti3 C1 H1 128 . . ? Ti2 C1 H1 128 . . ? Ti1 C1 H1 128 . . ? C12 C11 C15 108.4(6) . . ? C12 C11 C16 126.6(7) . . ? C15 C11 C16 124.9(7) . . ? C12 C11 Ti1 73.4(3) . . ? C15 C11 Ti1 75.0(3) . . ? C16 C11 Ti1 119.9(4) . . ? C11 C12 C13 107.7(5) . . ? C11 C12 C17 125.1(8) . . ? C13 C12 C17 127.1(7) . . ? C11 C12 Ti1 72.1(3) . . ? C13 C12 Ti1 73.3(3) . . ? C17 C12 Ti1 123.1(4) . . ? C14 C13 C12 108.2(6) . . ? C14 C13 C18 125.2(8) . . ? C12 C13 C18 125.7(7) . . ? C14 C13 Ti1 74.7(4) . . ? C12 C13 Ti1 72.1(3) . . ? C18 C13 Ti1 127.6(5) . . ? C13 C14 C15 107.6(6) . . ? C13 C14 C19 127.2(8) . . ? C15 C14 C19 125.1(7) . . ? C13 C14 Ti1 71.3(3) . . ? C15 C14 Ti1 72.2(3) . . ? C19 C14 Ti1 124.9(5) . . ? C11 C15 C14 108.0(5) . . ? C11 C15 C20 127.3(7) . . ? C14 C15 C20 124.4(7) . . ? C11 C15 Ti1 70.7(3) . . ? C14 C15 Ti1 73.8(3) . . ? C20 C15 Ti1 126.6(4) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C25 106.6(6) . . ? C22 C21 C26 128.4(7) . . ? C25 C21 C26 125.0(7) . . ? C22 C21 Ti2 74.5(3) . . ? C25 C21 Ti2 69.8(3) . . ? C26 C21 Ti2 119.7(4) . . ? C23 C22 C21 108.4(6) . . ? C23 C22 C27 124.6(7) . . ? C21 C22 C27 126.4(7) . . ? C23 C22 Ti2 73.0(3) . . ? C21 C22 Ti2 71.3(3) . . ? C27 C22 Ti2 128.7(4) . . ? C24 C23 C22 109.0(6) . . ? C24 C23 C28 128.2(7) . . ? C22 C23 C28 122.5(7) . . ? C24 C23 Ti2 71.7(3) . . ? C22 C23 Ti2 73.2(3) . . ? C28 C23 Ti2 126.2(4) . . ? C23 C24 C25 107.0(6) . . ? C23 C24 C29 128.9(7) . . ? C25 C24 C29 124.1(6) . . ? C23 C24 Ti2 74.6(3) . . ? C25 C24 Ti2 69.8(3) . . ? C29 C24 Ti2 121.0(4) . . ? C24 C25 C21 108.9(6) . . ? C24 C25 C30 124.5(7) . . ? C21 C25 C30 126.6(7) . . ? C24 C25 Ti2 75.2(3) . . ? C21 C25 Ti2 75.1(3) . . ? C30 C25 Ti2 115.3(4) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C35 C31 C32 107.7(5) . . ? C35 C31 C36 127.3(6) . . ? C32 C31 C36 125.0(7) . . ? C35 C31 Ti3 71.7(4) . . ? C32 C31 Ti3 73.1(3) . . ? C36 C31 Ti3 122.3(4) . . ? C31 C32 C33 107.1(6) . . ? C31 C32 C37 127.8(6) . . ? C33 C32 C37 125.0(6) . . ? C31 C32 Ti3 72.9(3) . . ? C33 C32 Ti3 72.0(3) . . ? C37 C32 Ti3 124.0(4) . . ? C34 C33 C32 108.0(5) . . ? C34 C33 C38 125.9(6) . . ? C32 C33 C38 126.0(6) . . ? C34 C33 Ti3 71.9(3) . . ? C32 C33 Ti3 73.3(3) . . ? C38 C33 Ti3 123.9(4) . . ? C35 C34 C33 107.6(6) . . ? C35 C34 C39 125.5(7) . . ? C33 C34 C39 126.8(6) . . ? C35 C34 Ti3 73.2(4) . . ? C33 C34 Ti3 74.0(3) . . ? C39 C34 Ti3 120.7(5) . . ? C34 C35 C31 109.6(6) . . ? C34 C35 C40 124.0(7) . . ? C31 C35 C40 126.2(7) . . ? C34 C35 Ti3 72.6(3) . . ? C31 C35 Ti3 74.3(4) . . ? C40 C35 Ti3 124.1(5) . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C58 C51 C52 114.7(5) . . ? C58 C51 B1 108.2(5) . . ? C52 C51 B1 108.3(5) . . ? C58 C51 H51 108.5 . . ? C52 C51 H51 108.5 . . ? B1 C51 H51 108.5 . . ? C53 C52 C51 115.3(5) . . ? C53 C52 H52A 108.5 . . ? C51 C52 H52A 108.5 . . ? C53 C52 H52B 108.5 . . ? C51 C52 H52B 108.5 . . ? H52A C52 H52B 107.5 . . ? C54 C53 C52 113.7(5) . . ? C54 C53 H53A 108.8 . . ? C52 C53 H53A 108.8 . . ? C54 C53 H53B 108.8 . . ? C52 C53 H53B 108.8 . . ? H53A C53 H53B 107.7 . . ? C55 C54 C53 116.9(5) . . ? C55 C54 H54A 108.1 . . ? C53 C54 H54A 108.1 . . ? C55 C54 H54B 108.1 . . ? C53 C54 H54B 108.1 . . ? H54A C54 H54B 107.3 . . ? C56 C55 C54 113.6(5) . . ? C56 C55 B1 107.9(4) . . ? C54 C55 B1 108.7(5) . . ? C56 C55 H55 108.8 . . ? C54 C55 H55 108.8 . . ? B1 C55 H55 108.8 . . ? C55 C56 C57 115.2(5) . . ? C55 C56 H56A 108.5 . . ? C57 C56 H56A 108.5 . . ? C55 C56 H56B 108.5 . . ? C57 C56 H56B 108.5 . . ? H56A C56 H56B 107.5 . . ? C56 C57 C58 114.6(5) . . ? C56 C57 H57A 108.6 . . ? C58 C57 H57A 108.6 . . ? C56 C57 H57B 108.6 . . ? C58 C57 H57B 108.6 . . ? H57A C57 H57B 107.6 . . ? C51 C58 C57 115.4(5) . . ? C51 C58 H58A 108.4 . . ? C57 C58 H58A 108.4 . . ? C51 C58 H58B 108.4 . . ? C57 C58 H58B 108.4 . . ? H58A C58 H58B 107.5 . . ? Ti1 O12 Ti2 102.42(19) . . ? B1 O13 Ti3 144.5(3) . . ? B1 O13 Ti1 90.0(3) . . ? Ti3 O13 Ti1 97.55(15) . . ? Ti3 O23 Ti2 99.88(19) . . ? O12 Ti1 O13 106.19(16) . . ? O12 Ti1 C1 84.00(19) . . ? O13 Ti1 C1 81.95(18) . . ? O12 Ti1 C11 100.6(2) . . ? O13 Ti1 C11 133.95(19) . . ? C1 Ti1 C11 138.3(2) . . ? O12 Ti1 C12 91.6(2) . . ? O13 Ti1 C12 161.72(17) . . ? C1 Ti1 C12 104.6(2) . . ? C11 Ti1 C12 34.5(2) . . ? O12 Ti1 C13 116.4(2) . . ? O13 Ti1 C13 132.8(2) . . ? C1 Ti1 C13 83.2(2) . . ? C11 Ti1 C13 57.4(2) . . ? C12 Ti1 C13 34.6(2) . . ? O12 Ti1 C15 134.0(2) . . ? O13 Ti1 C15 105.99(18) . . ? C1 Ti1 C15 132.5(2) . . ? C11 Ti1 C15 34.3(2) . . ? C12 Ti1 C15 56.9(2) . . ? C13 Ti1 C15 56.7(2) . . ? O12 Ti1 C14 148.2(2) . . ? O13 Ti1 C14 105.59(19) . . ? C1 Ti1 C14 98.5(2) . . ? C11 Ti1 C14 57.0(2) . . ? C12 Ti1 C14 56.9(2) . . ? C13 Ti1 C14 34.0(2) . . ? C15 Ti1 C14 34.0(2) . . ? O12 Ti1 B1 93.83(19) . . ? O13 Ti1 B1 36.78(18) . . ? C1 Ti1 B1 115.3(2) . . ? C11 Ti1 B1 105.8(2) . . ? C12 Ti1 B1 140.1(2) . . ? C13 Ti1 B1 146.7(2) . . ? C15 Ti1 B1 92.7(2) . . ? C14 Ti1 B1 113.1(2) . . ? O12 Ti1 Ti2 39.35(13) . . ? O13 Ti1 Ti2 89.04(11) . . ? C1 Ti1 Ti2 45.81(14) . . ? C11 Ti1 Ti2 133.13(16) . . ? C12 Ti1 Ti2 107.84(14) . . ? C13 Ti1 Ti2 111.05(16) . . ? C15 Ti1 Ti2 164.77(15) . . ? C14 Ti1 Ti2 139.85(18) . . ? B1 Ti1 Ti2 101.08(14) . . ? O12 Ti1 Ti3 90.90(13) . . ? O13 Ti1 Ti3 39.62(10) . . ? C1 Ti1 Ti3 43.19(15) . . ? C11 Ti1 Ti3 168.46(16) . . ? C12 Ti1 Ti3 147.09(18) . . ? C13 Ti1 Ti3 117.9(2) . . ? C15 Ti1 Ti3 134.22(17) . . ? C14 Ti1 Ti3 112.70(18) . . ? B1 Ti1 Ti3 72.35(15) . . ? Ti2 Ti1 Ti3 57.71(4) . . ? O12 Ti1 H1A 91.5(15) . . ? O13 Ti1 H1A 60.5(16) . . ? C1 Ti1 H1A 139.3(16) . . ? C11 Ti1 H1A 82.4(16) . . ? C12 Ti1 H1A 116.0(16) . . ? C13 Ti1 H1A 133.4(15) . . ? C15 Ti1 H1A 76.9(15) . . ? C14 Ti1 H1A 105.9(15) . . ? B1 Ti1 H1A 24.5(16) . . ? Ti2 Ti1 H1A 113.8(15) . . ? Ti3 Ti1 H1A 96.7(16) . . ? O23 Ti2 O12 105.63(17) . . ? O23 Ti2 C1 85.3(2) . . ? O12 Ti2 C1 87.6(2) . . ? O23 Ti2 C25 105.6(2) . . ? O12 Ti2 C25 107.0(2) . . ? C1 Ti2 C25 158.1(2) . . ? O23 Ti2 C21 90.96(19) . . ? O12 Ti2 C21 142.1(2) . . ? C1 Ti2 C21 128.3(2) . . ? C25 Ti2 C21 35.1(2) . . ? O23 Ti2 C24 140.6(2) . . ? O12 Ti2 C24 90.17(19) . . ? C1 Ti2 C24 132.1(2) . . ? C25 Ti2 C24 35.1(2) . . ? C21 Ti2 C24 57.9(2) . . ? O23 Ti2 C23 145.0(2) . . ? O12 Ti2 C23 108.5(2) . . ? C1 Ti2 C23 103.4(2) . . ? C25 Ti2 C23 57.0(2) . . ? C21 Ti2 C23 56.8(2) . . ? C24 Ti2 C23 33.8(2) . . ? O23 Ti2 C22 111.6(2) . . ? O12 Ti2 C22 142.2(2) . . ? C1 Ti2 C22 101.3(2) . . ? C25 Ti2 C22 57.2(2) . . ? C21 Ti2 C22 34.2(2) . . ? C24 Ti2 C22 56.6(2) . . ? C23 Ti2 C22 33.7(2) . . ? O23 Ti2 Ti3 39.98(12) . . ? O12 Ti2 Ti3 94.42(12) . . ? C1 Ti2 Ti3 45.87(16) . . ? C25 Ti2 Ti3 144.39(19) . . ? C21 Ti2 Ti3 118.66(16) . . ? C24 Ti2 Ti3 174.80(15) . . ? C23 Ti2 Ti3 141.55(17) . . ? C22 Ti2 Ti3 118.22(15) . . ? O23 Ti2 Ti1 91.19(12) . . ? O12 Ti2 Ti1 38.23(11) . . ? C1 Ti2 Ti1 50.63(16) . . ? C25 Ti2 Ti1 145.08(18) . . ? C21 Ti2 Ti1 177.46(16) . . ? C24 Ti2 Ti1 120.73(16) . . ? C23 Ti2 Ti1 120.73(16) . . ? C22 Ti2 Ti1 143.41(17) . . ? Ti3 Ti2 Ti1 62.54(5) . . ? O23 Ti3 O13 101.27(17) . . ? O23 Ti3 C1 87.0(2) . . ? O13 Ti3 C1 91.0(2) . . ? O23 Ti3 C34 95.0(2) . . ? O13 Ti3 C34 138.3(2) . . ? C1 Ti3 C34 128.2(2) . . ? O23 Ti3 C35 116.6(2) . . ? O13 Ti3 C35 105.3(2) . . ? C1 Ti3 C35 147.1(2) . . ? C34 Ti3 C35 34.2(2) . . ? O23 Ti3 C33 107.1(2) . . ? O13 Ti3 C33 150.99(18) . . ? C1 Ti3 C33 96.2(2) . . ? C34 Ti3 C33 34.1(2) . . ? C35 Ti3 C33 56.4(2) . . ? O23 Ti3 C31 150.1(2) . . ? O13 Ti3 C31 95.05(19) . . ? C1 Ti3 C31 117.9(2) . . ? C34 Ti3 C31 57.0(2) . . ? C35 Ti3 C31 34.0(2) . . ? C33 Ti3 C31 56.8(2) . . ? O23 Ti3 C32 141.25(19) . . ? O13 Ti3 C32 117.45(19) . . ? C1 Ti3 C32 90.7(2) . . ? C34 Ti3 C32 57.3(2) . . ? C35 Ti3 C32 56.4(2) . . ? C33 Ti3 C32 34.7(2) . . ? C31 Ti3 C32 33.9(2) . . ? O23 Ti3 Ti2 40.14(13) . . ? O13 Ti3 Ti2 93.48(12) . . ? C1 Ti3 Ti2 47.41(16) . . ? C34 Ti3 Ti2 122.27(16) . . ? C35 Ti3 Ti2 153.81(18) . . ? C33 Ti3 Ti2 112.01(15) . . ? C31 Ti3 Ti2 163.17(17) . . ? C32 Ti3 Ti2 129.59(15) . . ? O23 Ti3 Ti1 88.88(13) . . ? O13 Ti3 Ti1 42.83(11) . . ? C1 Ti3 Ti1 49.18(17) . . ? C34 Ti3 Ti1 175.26(16) . . ? C35 Ti3 Ti1 144.92(17) . . ? C33 Ti3 Ti1 141.80(16) . . ? C31 Ti3 Ti1 119.61(17) . . ? C32 Ti3 Ti1 117.99(17) . . ? Ti2 Ti3 Ti1 59.76(4) . . ? O13 B1 C51 115.7(4) . . ? O13 B1 C55 116.1(5) . . ? C51 B1 C55 107.7(4) . . ? O13 B1 Ti1 53.3(2) . . ? C51 B1 Ti1 115.4(4) . . ? C55 B1 Ti1 135.5(4) . . ? O13 B1 H1A 94(3) . . ? C51 B1 H1A 111(3) . . ? C55 B1 H1A 112(2) . . ?