# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Hans Breunig' _publ_contact_author_email HBREUNIG@UNI-BREMEN.DE _publ_section_title ; Polynuclear Titanocene Complexes with Antimony Ligands: [(Cp2Ti)2(SbR2)2] (R = Et),[(Cp2Ti)3(SbR)3Sb] [R = 2-(Me2NCH2)C6H4] and [(Cp2Ti)5(SbR)2Sb7] (R = Me3SiCH2) ; _publ_requested_category FM loop_ _publ_author_name 'Hans Breunig' 'Enno Lork' 'Ovidiu Moldovan' 'Ciprian Rat' 'Uwe Rosenthal' 'Cristian Silvestru' # Attachment 'cifs_files_1-3.cif' data_om3 _database_code_depnum_ccdc_archive 'CCDC 652789' _audit_creation_date 2007-02-16T20:25:09-00:00 _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 'C28 H40 Sb2 Ti2' _chemical_formula_sum 'C28 H40 Sb2 Ti2' _chemical_formula_weight 715.9 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.625(2) _cell_length_b 10.084(2) _cell_length_c 16.072(3) _cell_angle_alpha 78.120(10) _cell_angle_beta 87.49(2) _cell_angle_gamma 88.66(2) _cell_volume 1366.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 5.175 _cell_measurement_theta_max 24.989 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description blocks _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.74 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.533 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_absorpt_correction_T_min 0.3117 _exptl_absorpt_correction_T_max 0.7858 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_unetI/netI 0.0447 _diffrn_reflns_number 7566 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 6216 _reflns_number_gt 5189 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0789P)^2^+0.2837P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6216 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1175 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.015 _refine_diff_density_min -2.241 _refine_diff_density_rms 0.185 #----------------------------------------------------------------------------# # 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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 0.4635(6) 0.8344(5) 0.3620(3) 0.0330(11) Uani 1 1 d . . . H1A H 0.3634 0.8056 0.3441 0.04 Uiso 1 1 calc R . . H1B H 0.4415 0.9103 0.3914 0.04 Uiso 1 1 calc R . . C2 C 0.5665(8) 0.8851(7) 0.2829(4) 0.0549(17) Uani 1 1 d . . . H2A H 0.6659 0.9143 0.2999 0.082 Uiso 1 1 calc R . . H2B H 0.5151 0.9618 0.2463 0.082 Uiso 1 1 calc R . . H2C H 0.5849 0.8119 0.2518 0.082 Uiso 1 1 calc R . . C3 C 0.7782(5) 0.7737(5) 0.4606(3) 0.0297(10) Uani 1 1 d . . . H3A H 0.8483 0.7127 0.4988 0.036 Uiso 1 1 calc R . . H3B H 0.8306 0.795 0.4035 0.036 Uiso 1 1 calc R . . C4 C 0.7559(7) 0.9037(5) 0.4929(4) 0.0427(13) Uani 1 1 d . . . H4A H 0.6881 0.9659 0.4551 0.064 Uiso 1 1 calc R . . H4B H 0.8568 0.946 0.494 0.064 Uiso 1 1 calc R . . H4C H 0.7083 0.8837 0.5505 0.064 Uiso 1 1 calc R . . C5 C 0.6251(6) 0.6141(6) 0.6650(3) 0.0399(13) Uani 1 1 d . . . H5 H 0.7154 0.6339 0.6288 0.048 Uiso 1 1 calc R . . C6 C 0.5743(7) 0.4865(6) 0.7031(4) 0.0437(14) Uani 1 1 d . . . H6 H 0.6247 0.4037 0.698 0.052 Uiso 1 1 calc R . . C7 C 0.4371(8) 0.4985(7) 0.7504(3) 0.0514(17) Uani 1 1 d . . . H7 H 0.3758 0.4266 0.7818 0.062 Uiso 1 1 calc R . . C8 C 0.4080(8) 0.6369(8) 0.7423(4) 0.0545(17) Uani 1 1 d . . . H8 H 0.3238 0.6763 0.7693 0.065 Uiso 1 1 calc R . . C9 C 0.5217(8) 0.7082(7) 0.6885(4) 0.0486(15) Uani 1 1 d . . . H9 H 0.5275 0.8039 0.671 0.058 Uiso 1 1 calc R . . C10 C 0.1703(5) 0.5988(5) 0.5151(3) 0.0299(10) Uani 1 1 d . . . H10 H 0.186 0.5649 0.4644 0.036 Uiso 1 1 calc R . . C11 C 0.1961(5) 0.7327(5) 0.5245(3) 0.0324(11) Uani 1 1 d . . . H11 H 0.2306 0.8056 0.4807 0.039 Uiso 1 1 calc R . . C12 C 0.1624(6) 0.7392(5) 0.6088(3) 0.0339(11) Uani 1 1 d . . . H12 H 0.1712 0.8173 0.6327 0.041 Uiso 1 1 calc R . . C13 C 0.1129(6) 0.6110(5) 0.6531(3) 0.0333(11) Uani 1 1 d . . . H13 H 0.0827 0.5875 0.7118 0.04 Uiso 1 1 calc R . . C14 C 0.1164(5) 0.5244(5) 0.5954(3) 0.0323(11) Uani 1 1 d . . . H14 H 0.0876 0.4318 0.6079 0.039 Uiso 1 1 calc R . . C15 C 0.2964(6) 0.1652(5) 0.1009(4) 0.0334(11) Uani 1 1 d . . . H15A H 0.352 0.1081 0.1483 0.04 Uiso 1 1 calc R . . H15B H 0.3617 0.17 0.0482 0.04 Uiso 1 1 calc R . . C16 C 0.2740(7) 0.3076(6) 0.1185(5) 0.0471(15) Uani 1 1 d . . . H16A H 0.2114 0.3625 0.0743 0.071 Uiso 1 1 calc R . . H16B H 0.3755 0.3494 0.1183 0.071 Uiso 1 1 calc R . . H16C H 0.2209 0.3023 0.1743 0.071 Uiso 1 1 calc R . . C17 C -0.0131(6) 0.0860(6) 0.2145(3) 0.0344(11) Uani 1 1 d . . . H17A H -0.039 0.1821 0.2145 0.041 Uiso 1 1 calc R . . H17B H -0.1103 0.0341 0.2272 0.041 Uiso 1 1 calc R . . C18 C 0.0994(7) 0.0339(7) 0.2852(4) 0.0466(14) Uani 1 1 d . . . H18A H 0.1413 -0.0549 0.279 0.07 Uiso 1 1 calc R . . H18B H 0.0444 0.0255 0.3406 0.07 Uiso 1 1 calc R . . H18C H 0.1847 0.0978 0.2812 0.07 Uiso 1 1 calc R . . C19 C 0.1412(6) 0.3065(7) -0.0943(4) 0.0526(17) Uani 1 1 d . . . H19 H 0.2234 0.295 -0.0559 0.063 Uiso 1 1 calc R . . C20 C 0.0278(6) 0.4092(5) -0.1033(3) 0.0366(12) Uani 1 1 d . . . H20 H 0.0174 0.4789 -0.0715 0.044 Uiso 1 1 calc R . . C21 C -0.0665(7) 0.3902(6) -0.1671(4) 0.0435(14) Uani 1 1 d . . . H21 H -0.1529 0.4462 -0.187 0.052 Uiso 1 1 calc R . . C22 C -0.0166(10) 0.2784(8) -0.1974(4) 0.063(2) Uani 1 1 d . . . H22 H -0.0613 0.2439 -0.2414 0.075 Uiso 1 1 calc R . . C23 C 0.1129(9) 0.2242(7) -0.1512(5) 0.063(2) Uani 1 1 d . . . H23 H 0.1708 0.1454 -0.1577 0.075 Uiso 1 1 calc R . . C24 C -0.2865(5) 0.1914(6) 0.0640(3) 0.0373(12) Uani 1 1 d . . . H24 H -0.2537 0.1729 0.1209 0.045 Uiso 1 1 calc R . . C25 C -0.3280(6) 0.0958(5) 0.0194(4) 0.0421(14) Uani 1 1 d . . . H25 H -0.3254 0.0004 0.0396 0.051 Uiso 1 1 calc R . . C26 C -0.3747(6) 0.1634(8) -0.0606(4) 0.0490(16) Uani 1 1 d . . . H26 H -0.4118 0.1227 -0.1041 0.059 Uiso 1 1 calc R . . C27 C -0.3567(7) 0.3009(7) -0.0648(4) 0.0511(17) Uani 1 1 d . . . H27 H -0.379 0.3712 -0.1122 0.061 Uiso 1 1 calc R . . C28 C -0.3004(6) 0.3191(6) 0.0124(4) 0.0441(14) Uani 1 1 d . . . H28 H -0.2763 0.4029 0.0268 0.053 Uiso 1 1 calc R . . Ti1 Ti 0.37735(9) 0.58549(8) 0.60810(5) 0.02155(17) Uani 1 1 d . . . Ti2 Ti -0.10553(9) 0.20001(8) -0.05499(5) 0.02206(17) Uani 1 1 d . . . Sb1 Sb 0.56500(3) 0.66515(3) 0.451972(17) 0.01975(10) Uani 1 1 d . . . Sb2 Sb 0.07663(3) 0.07043(3) 0.086819(18) 0.02198(10) Uani 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 0.030(2) 0.034(3) 0.028(2) 0.0073(19) -0.0028(19) 0.014(2) C2 0.060(4) 0.052(4) 0.040(3) 0.014(3) 0.015(3) 0.020(3) C3 0.019(2) 0.026(2) 0.044(3) -0.006(2) 0.0027(19) -0.0060(17) C4 0.043(3) 0.027(3) 0.060(4) -0.013(2) 0.006(3) -0.007(2) C5 0.030(3) 0.063(4) 0.027(2) -0.009(2) -0.006(2) -0.007(2) C6 0.046(3) 0.047(3) 0.040(3) -0.009(2) -0.028(3) 0.008(3) C7 0.051(4) 0.079(5) 0.017(2) 0.009(3) -0.006(2) -0.025(3) C8 0.047(4) 0.091(5) 0.033(3) -0.032(3) -0.004(3) 0.005(3) C9 0.058(4) 0.050(3) 0.044(3) -0.020(3) -0.019(3) -0.002(3) C10 0.016(2) 0.041(3) 0.035(3) -0.014(2) -0.0032(18) 0.0092(19) C11 0.023(2) 0.033(3) 0.036(3) 0.002(2) 0.0059(19) 0.0078(19) C12 0.035(3) 0.029(2) 0.041(3) -0.015(2) 0.006(2) 0.003(2) C13 0.025(2) 0.037(3) 0.036(3) -0.004(2) 0.011(2) 0.002(2) C14 0.017(2) 0.030(2) 0.048(3) -0.004(2) -0.001(2) 0.0016(18) C15 0.021(2) 0.034(3) 0.047(3) -0.012(2) -0.006(2) 0.0010(19) C16 0.039(3) 0.038(3) 0.070(4) -0.021(3) -0.010(3) -0.001(2) C17 0.030(2) 0.051(3) 0.024(2) -0.013(2) 0.0014(19) 0.008(2) C18 0.051(4) 0.061(4) 0.029(3) -0.015(3) -0.009(2) 0.023(3) C19 0.023(3) 0.065(4) 0.055(4) 0.022(3) 0.007(2) -0.014(3) C20 0.039(3) 0.036(3) 0.034(3) -0.007(2) 0.015(2) -0.017(2) C21 0.043(3) 0.041(3) 0.037(3) 0.016(2) -0.004(2) -0.014(2) C22 0.094(6) 0.073(5) 0.022(3) -0.013(3) 0.022(3) -0.047(4) C23 0.062(4) 0.038(3) 0.080(5) -0.006(3) 0.056(4) -0.005(3) C24 0.018(2) 0.070(4) 0.023(2) -0.009(2) 0.0046(18) 0.012(2) C25 0.024(2) 0.031(3) 0.064(4) -0.001(2) 0.023(2) 0.003(2) C26 0.022(3) 0.086(5) 0.049(3) -0.037(3) 0.001(2) 0.000(3) C27 0.037(3) 0.071(4) 0.034(3) 0.011(3) 0.010(2) 0.025(3) C28 0.035(3) 0.038(3) 0.063(4) -0.022(3) 0.014(3) 0.002(2) Ti1 0.0197(4) 0.0256(4) 0.0188(4) -0.0037(3) 0.0007(3) -0.0003(3) Ti2 0.0196(4) 0.0264(4) 0.0187(4) -0.0024(3) 0.0053(3) -0.0014(3) Sb1 0.01652(15) 0.02089(16) 0.01981(15) -0.00002(11) 0.00043(10) 0.00275(10) Sb2 0.01681(15) 0.02727(17) 0.02158(16) -0.00523(11) 0.00235(11) 0.00202(11) #----------------------------------------------------------------------------# # 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 C2 1.523(7) . ? C1 Sb1 2.190(4) . ? C3 C4 1.511(7) . ? C3 Sb1 2.186(4) . ? C5 C6 1.378(9) . ? C5 C9 1.385(9) . ? C5 Ti1 2.407(5) . ? C6 C7 1.395(9) . ? C6 Ti1 2.394(5) . ? C7 C8 1.393(10) . ? C7 Ti1 2.350(5) . ? C8 C9 1.390(10) . ? C8 Ti1 2.347(6) . ? C9 Ti1 2.371(6) . ? C10 C11 1.412(7) . ? C10 C14 1.418(7) . ? C10 Ti1 2.362(5) . ? C11 C12 1.389(7) . ? C11 Ti1 2.389(5) . ? C12 C13 1.408(7) . ? C12 Ti1 2.390(5) . ? C13 C14 1.398(7) . ? C13 Ti1 2.387(5) . ? C14 Ti1 2.376(5) . ? C15 C16 1.526(7) . ? C15 Sb2 2.184(5) . ? C17 C18 1.528(7) . ? C17 Sb2 2.195(5) . ? C19 C23 1.387(10) . ? C19 C20 1.398(9) . ? C19 Ti2 2.406(5) . ? C20 C21 1.383(8) . ? C20 Ti2 2.395(5) . ? C21 C22 1.371(10) . ? C21 Ti2 2.365(5) . ? C22 C23 1.406(11) . ? C22 Ti2 2.362(5) . ? C23 Ti2 2.369(5) . ? C24 C25 1.376(8) . ? C24 C28 1.386(8) . ? C24 Ti2 2.404(5) . ? C25 C26 1.398(9) . ? C25 Ti2 2.365(5) . ? C26 C27 1.386(10) . ? C26 Ti2 2.368(5) . ? C27 C28 1.401(9) . ? C27 Ti2 2.370(6) . ? C28 Ti2 2.393(5) . ? Ti1 Sb1 2.9046(10) . ? Ti1 Sb1 2.9105(10) 2_666 ? Ti2 Sb2 2.8797(10) 2 ? Ti2 Sb2 2.8916(11) . ? Sb1 Ti1 2.9105(10) 2_666 ? Sb2 Ti2 2.8797(10) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 Sb1 113.9(3) . . ? C4 C3 Sb1 115.0(3) . . ? C6 C5 C9 108.1(6) . . ? C6 C5 Ti1 72.8(3) . . ? C9 C5 Ti1 71.7(3) . . ? C5 C6 C7 109.2(6) . . ? C5 C6 Ti1 73.8(3) . . ? C7 C6 Ti1 71.2(3) . . ? C8 C7 C6 106.2(5) . . ? C8 C7 Ti1 72.7(3) . . ? C6 C7 Ti1 74.7(3) . . ? C9 C8 C7 109.1(6) . . ? C9 C8 Ti1 73.8(3) . . ? C7 C8 Ti1 72.8(3) . . ? C5 C9 C8 107.4(6) . . ? C5 C9 Ti1 74.6(3) . . ? C8 C9 Ti1 71.9(3) . . ? C11 C10 C14 107.4(4) . . ? C11 C10 Ti1 73.7(3) . . ? C14 C10 Ti1 73.1(3) . . ? C12 C11 C10 108.1(4) . . ? C12 C11 Ti1 73.1(3) . . ? C10 C11 Ti1 71.7(3) . . ? C11 C12 C13 108.7(4) . . ? C11 C12 Ti1 73.1(3) . . ? C13 C12 Ti1 72.7(3) . . ? C14 C13 C12 107.8(5) . . ? C14 C13 Ti1 72.5(3) . . ? C12 C13 Ti1 73.0(3) . . ? C13 C14 C10 108.1(4) . . ? C13 C14 Ti1 73.3(3) . . ? C10 C14 Ti1 72.1(3) . . ? C16 C15 Sb2 112.5(3) . . ? C18 C17 Sb2 114.2(3) . . ? C23 C19 C20 108.2(6) . . ? C23 C19 Ti2 71.6(3) . . ? C20 C19 Ti2 72.6(3) . . ? C21 C20 C19 107.0(6) . . ? C21 C20 Ti2 71.9(3) . . ? C19 C20 Ti2 73.5(3) . . ? C22 C21 C20 109.8(6) . . ? C22 C21 Ti2 73.0(3) . . ? C20 C21 Ti2 74.3(3) . . ? C21 C22 C23 107.3(6) . . ? C21 C22 Ti2 73.3(3) . . ? C23 C22 Ti2 73.0(3) . . ? C19 C23 C22 107.7(6) . . ? C19 C23 Ti2 74.6(3) . . ? C22 C23 Ti2 72.5(3) . . ? C25 C24 C28 109.0(5) . . ? C25 C24 Ti2 71.7(3) . . ? C28 C24 Ti2 72.8(3) . . ? C24 C25 C26 108.2(5) . . ? C24 C25 Ti2 74.8(3) . . ? C26 C25 Ti2 72.9(3) . . ? C27 C26 C25 107.2(5) . . ? C27 C26 Ti2 73.1(3) . . ? C25 C26 Ti2 72.7(3) . . ? C26 C27 C28 108.7(5) . . ? C26 C27 Ti2 72.9(3) . . ? C28 C27 Ti2 73.8(3) . . ? C24 C28 C27 106.8(5) . . ? C24 C28 Ti2 73.6(3) . . ? C27 C28 Ti2 72.0(3) . . ? C8 Ti1 C7 34.5(2) . . ? C8 Ti1 C10 135.2(2) . . ? C7 Ti1 C10 140.7(2) . . ? C8 Ti1 C9 34.3(2) . . ? C7 Ti1 C9 57.4(2) . . ? C10 Ti1 C9 144.6(2) . . ? C8 Ti1 C14 109.9(2) . . ? C7 Ti1 C14 105.9(2) . . ? C10 Ti1 C14 34.82(18) . . ? C9 Ti1 C14 139.2(2) . . ? C8 Ti1 C13 79.2(2) . . ? C7 Ti1 C13 89.1(2) . . ? C10 Ti1 C13 57.35(18) . . ? C9 Ti1 C13 105.2(2) . . ? C14 Ti1 C13 34.13(18) . . ? C8 Ti1 C11 113.1(2) . . ? C7 Ti1 C11 141.2(2) . . ? C10 Ti1 C11 34.58(17) . . ? C9 Ti1 C11 110.2(2) . . ? C14 Ti1 C11 57.19(17) . . ? C13 Ti1 C11 56.84(17) . . ? C8 Ti1 C12 81.4(2) . . ? C7 Ti1 C12 107.5(2) . . ? C10 Ti1 C12 56.99(17) . . ? C9 Ti1 C12 90.7(2) . . ? C14 Ti1 C12 56.80(17) . . ? C13 Ti1 C12 34.28(17) . . ? C11 Ti1 C12 33.80(18) . . ? C8 Ti1 C6 56.1(2) . . ? C7 Ti1 C6 34.2(2) . . ? C10 Ti1 C6 159.09(19) . . ? C9 Ti1 C6 56.0(2) . . ? C14 Ti1 C6 132.0(2) . . ? C13 Ti1 C6 123.2(2) . . ? C11 Ti1 C6 166.2(2) . . ? C12 Ti1 C6 137.4(2) . . ? C8 Ti1 C5 56.1(2) . . ? C7 Ti1 C5 56.7(2) . . ? C10 Ti1 C5 162.53(19) . . ? C9 Ti1 C5 33.7(2) . . ? C14 Ti1 C5 162.61(19) . . ? C13 Ti1 C5 135.15(19) . . ? C11 Ti1 C5 135.0(2) . . ? C12 Ti1 C5 124.0(2) . . ? C6 Ti1 C5 33.4(2) . . ? C8 Ti1 Sb1 129.45(18) . . ? C7 Ti1 Sb1 133.48(16) . . ? C10 Ti1 Sb1 84.05(12) . . ? C9 Ti1 Sb1 95.28(17) . . ? C14 Ti1 Sb1 117.40(14) . . ? C13 Ti1 Sb1 136.71(13) . . ? C11 Ti1 Sb1 80.46(12) . . ? C12 Ti1 Sb1 109.84(13) . . ? C6 Ti1 Sb1 99.94(17) . . ? C5 Ti1 Sb1 79.44(13) . . ? C8 Ti1 Sb1 130.8(2) . 2_666 ? C7 Ti1 Sb1 96.39(19) . 2_666 ? C10 Ti1 Sb1 80.66(12) . 2_666 ? C9 Ti1 Sb1 133.58(17) . 2_666 ? C14 Ti1 Sb1 81.02(13) . 2_666 ? C13 Ti1 Sb1 112.52(13) . 2_666 ? C11 Ti1 Sb1 112.67(13) . 2_666 ? C12 Ti1 Sb1 135.48(13) . 2_666 ? C6 Ti1 Sb1 80.54(15) . 2_666 ? C5 Ti1 Sb1 100.48(15) . 2_666 ? Sb1 Ti1 Sb1 75.38(2) . 2_666 ? C22 Ti2 C25 138.3(3) . . ? C22 Ti2 C21 33.7(2) . . ? C25 Ti2 C21 133.9(2) . . ? C22 Ti2 C26 105.8(3) . . ? C25 Ti2 C26 34.4(2) . . ? C21 Ti2 C26 101.8(2) . . ? C22 Ti2 C23 34.6(3) . . ? C25 Ti2 C23 157.0(2) . . ? C21 Ti2 C23 56.4(2) . . ? C26 Ti2 C23 136.8(3) . . ? C22 Ti2 C27 98.3(3) . . ? C25 Ti2 C27 56.5(2) . . ? C21 Ti2 C27 78.2(2) . . ? C26 Ti2 C27 34.0(2) . . ? C23 Ti2 C27 132.0(3) . . ? C22 Ti2 C28 122.2(3) . . ? C25 Ti2 C28 56.42(19) . . ? C21 Ti2 C28 91.5(2) . . ? C26 Ti2 C28 56.8(2) . . ? C23 Ti2 C28 144.8(2) . . ? C27 Ti2 C28 34.2(2) . . ? C22 Ti2 C20 56.5(2) . . ? C25 Ti2 C20 145.38(19) . . ? C21 Ti2 C20 33.76(19) . . ? C26 Ti2 C20 126.9(2) . . ? C23 Ti2 C20 56.5(2) . . ? C27 Ti2 C20 94.7(2) . . ? C28 Ti2 C20 89.00(19) . . ? C22 Ti2 C24 153.9(3) . . ? C25 Ti2 C24 33.5(2) . . ? C21 Ti2 C24 125.1(2) . . ? C26 Ti2 C24 56.16(19) . . ? C23 Ti2 C24 166.8(3) . . ? C27 Ti2 C24 55.92(18) . . ? C28 Ti2 C24 33.6(2) . . ? C20 Ti2 C24 116.3(2) . . ? C22 Ti2 C19 56.5(2) . . ? C25 Ti2 C19 165.2(2) . . ? C21 Ti2 C19 55.9(2) . . ? C26 Ti2 C19 157.7(2) . . ? C23 Ti2 C19 33.8(3) . . ? C27 Ti2 C19 128.4(2) . . ? C28 Ti2 C19 118.2(2) . . ? C20 Ti2 C19 33.9(2) . . ? C24 Ti2 C19 133.9(2) . . ? C22 Ti2 Sb2 87.29(18) . 2 ? C25 Ti2 Sb2 78.25(14) . 2 ? C21 Ti2 Sb2 120.46(16) . 2 ? C26 Ti2 Sb2 83.59(17) . 2 ? C23 Ti2 Sb2 79.37(16) . 2 ? C27 Ti2 Sb2 116.66(19) . 2 ? C28 Ti2 Sb2 134.40(14) . 2 ? C20 Ti2 Sb2 135.89(13) . 2 ? C24 Ti2 Sb2 107.14(15) . 2 ? C19 Ti2 Sb2 106.93(19) . 2 ? C22 Ti2 Sb2 127.2(2) . . ? C25 Ti2 Sb2 88.49(16) . . ? C21 Ti2 Sb2 133.76(14) . . ? C26 Ti2 Sb2 122.72(18) . . ? C23 Ti2 Sb2 92.7(2) . . ? C27 Ti2 Sb2 133.27(14) . . ? C28 Ti2 Sb2 102.23(17) . . ? C20 Ti2 Sb2 101.81(14) . . ? C24 Ti2 Sb2 77.67(12) . . ? C19 Ti2 Sb2 79.09(15) . . ? Sb2 Ti2 Sb2 79.42(3) 2 . ? C3 Sb1 C1 93.5(2) . . ? C3 Sb1 Ti1 116.64(14) . . ? C1 Sb1 Ti1 113.18(13) . . ? C3 Sb1 Ti1 112.62(13) . 2_666 ? C1 Sb1 Ti1 116.68(15) . 2_666 ? Ti1 Sb1 Ti1 104.62(3) . 2_666 ? C15 Sb2 C17 93.4(2) . . ? C15 Sb2 Ti2 114.76(13) . 2 ? C17 Sb2 Ti2 115.77(15) . 2 ? C15 Sb2 Ti2 116.46(15) . . ? C17 Sb2 Ti2 116.88(14) . . ? Ti2 Sb2 Ti2 100.58(3) 2 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 C5 C6 C7 0.7(6) . . . . ? Ti1 C5 C6 C7 -62.8(4) . . . . ? C9 C5 C6 Ti1 63.5(4) . . . . ? C5 C6 C7 C8 -1.8(6) . . . . ? Ti1 C6 C7 C8 -66.3(4) . . . . ? C5 C6 C7 Ti1 64.5(4) . . . . ? C6 C7 C8 C9 2.3(7) . . . . ? Ti1 C7 C8 C9 -65.4(4) . . . . ? C6 C7 C8 Ti1 67.7(4) . . . . ? C6 C5 C9 C8 0.7(6) . . . . ? Ti1 C5 C9 C8 64.9(4) . . . . ? C6 C5 C9 Ti1 -64.2(4) . . . . ? C7 C8 C9 C5 -1.9(7) . . . . ? Ti1 C8 C9 C5 -66.7(4) . . . . ? C7 C8 C9 Ti1 64.8(4) . . . . ? C14 C10 C11 C12 1.3(5) . . . . ? Ti1 C10 C11 C12 -64.6(4) . . . . ? C14 C10 C11 Ti1 65.9(3) . . . . ? C10 C11 C12 C13 -0.8(6) . . . . ? Ti1 C11 C12 C13 -64.5(4) . . . . ? C10 C11 C12 Ti1 63.6(3) . . . . ? C11 C12 C13 C14 0.0(6) . . . . ? Ti1 C12 C13 C14 -64.7(3) . . . . ? C11 C12 C13 Ti1 64.7(4) . . . . ? C12 C13 C14 C10 0.8(6) . . . . ? Ti1 C13 C14 C10 -64.2(3) . . . . ? C12 C13 C14 Ti1 65.0(4) . . . . ? C11 C10 C14 C13 -1.3(5) . . . . ? Ti1 C10 C14 C13 65.0(3) . . . . ? C11 C10 C14 Ti1 -66.3(3) . . . . ? C23 C19 C20 C21 -1.4(6) . . . . ? Ti2 C19 C20 C21 -64.6(3) . . . . ? C23 C19 C20 Ti2 63.2(4) . . . . ? C19 C20 C21 C22 0.7(6) . . . . ? Ti2 C20 C21 C22 -65.0(4) . . . . ? C19 C20 C21 Ti2 65.7(4) . . . . ? C20 C21 C22 C23 0.3(6) . . . . ? Ti2 C21 C22 C23 -65.5(4) . . . . ? C20 C21 C22 Ti2 65.8(4) . . . . ? C20 C19 C23 C22 1.5(6) . . . . ? Ti2 C19 C23 C22 65.4(4) . . . . ? C20 C19 C23 Ti2 -63.9(4) . . . . ? C21 C22 C23 C19 -1.1(6) . . . . ? Ti2 C22 C23 C19 -66.8(4) . . . . ? C21 C22 C23 Ti2 65.7(4) . . . . ? C28 C24 C25 C26 -2.2(6) . . . . ? Ti2 C24 C25 C26 -65.8(4) . . . . ? C28 C24 C25 Ti2 63.6(4) . . . . ? C24 C25 C26 C27 1.7(6) . . . . ? Ti2 C25 C26 C27 -65.4(4) . . . . ? C24 C25 C26 Ti2 67.1(3) . . . . ? C25 C26 C27 C28 -0.5(6) . . . . ? Ti2 C26 C27 C28 -65.7(4) . . . . ? C25 C26 C27 Ti2 65.2(4) . . . . ? C25 C24 C28 C27 1.9(6) . . . . ? Ti2 C24 C28 C27 64.8(4) . . . . ? C25 C24 C28 Ti2 -62.9(3) . . . . ? C26 C27 C28 C24 -0.9(6) . . . . ? Ti2 C27 C28 C24 -65.9(4) . . . . ? C26 C27 C28 Ti2 65.1(4) . . . . ? C9 C8 Ti1 C7 116.5(6) . . . . ? C9 C8 Ti1 C10 -125.2(4) . . . . ? C7 C8 Ti1 C10 118.3(4) . . . . ? C7 C8 Ti1 C9 -116.5(6) . . . . ? C9 C8 Ti1 C14 -154.2(4) . . . . ? C7 C8 Ti1 C14 89.3(4) . . . . ? C9 C8 Ti1 C13 -138.9(4) . . . . ? C7 C8 Ti1 C13 104.5(4) . . . . ? C9 C8 Ti1 C11 -92.3(4) . . . . ? C7 C8 Ti1 C11 151.2(4) . . . . ? C9 C8 Ti1 C12 -104.2(4) . . . . ? C7 C8 Ti1 C12 139.3(4) . . . . ? C9 C8 Ti1 C6 77.9(4) . . . . ? C7 C8 Ti1 C6 -38.6(4) . . . . ? C9 C8 Ti1 C5 37.4(4) . . . . ? C7 C8 Ti1 C5 -79.1(4) . . . . ? C9 C8 Ti1 Sb1 4.4(5) . . . . ? C7 C8 Ti1 Sb1 -112.1(4) . . . . ? C9 C8 Ti1 Sb1 110.6(4) . . . 2_666 ? C7 C8 Ti1 Sb1 -6.0(5) . . . 2_666 ? C6 C7 Ti1 C8 -112.8(5) . . . . ? C8 C7 Ti1 C10 -101.5(4) . . . . ? C6 C7 Ti1 C10 145.7(3) . . . . ? C8 C7 Ti1 C9 36.7(4) . . . . ? C6 C7 Ti1 C9 -76.1(4) . . . . ? C8 C7 Ti1 C14 -102.1(4) . . . . ? C6 C7 Ti1 C14 145.1(4) . . . . ? C8 C7 Ti1 C13 -72.0(4) . . . . ? C6 C7 Ti1 C13 175.2(4) . . . . ? C8 C7 Ti1 C11 -45.1(5) . . . . ? C6 C7 Ti1 C11 -158.0(4) . . . . ? C8 C7 Ti1 C12 -42.6(4) . . . . ? C6 C7 Ti1 C12 -155.4(4) . . . . ? C8 C7 Ti1 C6 112.8(5) . . . . ? C8 C7 Ti1 C5 77.1(4) . . . . ? C6 C7 Ti1 C5 -35.7(4) . . . . ? C8 C7 Ti1 Sb1 99.6(4) . . . . ? C6 C7 Ti1 Sb1 -13.3(5) . . . . ? C8 C7 Ti1 Sb1 175.5(4) . . . 2_666 ? C6 C7 Ti1 Sb1 62.6(4) . . . 2_666 ? C11 C10 Ti1 C8 61.4(4) . . . . ? C14 C10 Ti1 C8 -53.0(4) . . . . ? C11 C10 Ti1 C7 113.4(4) . . . . ? C14 C10 Ti1 C7 -1.0(5) . . . . ? C11 C10 Ti1 C9 8.9(5) . . . . ? C14 C10 Ti1 C9 -105.5(4) . . . . ? C11 C10 Ti1 C14 114.4(4) . . . . ? C11 C10 Ti1 C13 77.6(3) . . . . ? C14 C10 Ti1 C13 -36.8(3) . . . . ? C14 C10 Ti1 C11 -114.4(4) . . . . ? C11 C10 Ti1 C12 36.5(3) . . . . ? C14 C10 Ti1 C12 -77.9(3) . . . . ? C11 C10 Ti1 C6 175.9(5) . . . . ? C14 C10 Ti1 C6 61.5(6) . . . . ? C11 C10 Ti1 C5 -62.7(7) . . . . ? C14 C10 Ti1 C5 -177.1(6) . . . . ? C11 C10 Ti1 Sb1 -81.8(3) . . . . ? C14 C10 Ti1 Sb1 163.8(3) . . . . ? C11 C10 Ti1 Sb1 -157.9(3) . . . 2_666 ? C14 C10 Ti1 Sb1 87.7(3) . . . 2_666 ? C5 C9 Ti1 C8 114.6(6) . . . . ? C5 C9 Ti1 C7 77.6(4) . . . . ? C8 C9 Ti1 C7 -37.0(4) . . . . ? C5 C9 Ti1 C10 -149.1(4) . . . . ? C8 C9 Ti1 C10 96.3(5) . . . . ? C5 C9 Ti1 C14 153.5(3) . . . . ? C8 C9 Ti1 C14 38.9(6) . . . . ? C5 C9 Ti1 C13 156.6(4) . . . . ? C8 C9 Ti1 C13 41.9(5) . . . . ? C5 C9 Ti1 C11 -143.7(3) . . . . ? C8 C9 Ti1 C11 101.7(4) . . . . ? C5 C9 Ti1 C12 -172.0(4) . . . . ? C8 C9 Ti1 C12 73.4(4) . . . . ? C5 C9 Ti1 C6 36.5(4) . . . . ? C8 C9 Ti1 C6 -78.1(5) . . . . ? C8 C9 Ti1 C5 -114.6(6) . . . . ? C5 C9 Ti1 Sb1 -62.0(4) . . . . ? C8 C9 Ti1 Sb1 -176.6(4) . . . . ? C5 C9 Ti1 Sb1 12.9(5) . . . 2_666 ? C8 C9 Ti1 Sb1 -101.8(4) . . . 2_666 ? C13 C14 Ti1 C8 27.3(4) . . . . ? C10 C14 Ti1 C8 143.2(3) . . . . ? C13 C14 Ti1 C7 63.4(4) . . . . ? C10 C14 Ti1 C7 179.3(3) . . . . ? C13 C14 Ti1 C10 -115.9(4) . . . . ? C13 C14 Ti1 C9 5.3(5) . . . . ? C10 C14 Ti1 C9 121.2(4) . . . . ? C10 C14 Ti1 C13 115.9(4) . . . . ? C13 C14 Ti1 C11 -78.0(3) . . . . ? C10 C14 Ti1 C11 37.9(3) . . . . ? C13 C14 Ti1 C12 -37.4(3) . . . . ? C10 C14 Ti1 C12 78.5(3) . . . . ? C13 C14 Ti1 C6 89.1(4) . . . . ? C10 C14 Ti1 C6 -155.0(3) . . . . ? C13 C14 Ti1 C5 61.2(7) . . . . ? C10 C14 Ti1 C5 177.1(6) . . . . ? C13 C14 Ti1 Sb1 -134.1(3) . . . . ? C10 C14 Ti1 Sb1 -18.2(3) . . . . ? C13 C14 Ti1 Sb1 157.6(3) . . . 2_666 ? C10 C14 Ti1 Sb1 -86.5(3) . . . 2_666 ? C14 C13 Ti1 C8 -153.9(4) . . . . ? C12 C13 Ti1 C8 90.5(4) . . . . ? C14 C13 Ti1 C7 -120.7(3) . . . . ? C12 C13 Ti1 C7 123.8(4) . . . . ? C14 C13 Ti1 C10 37.6(3) . . . . ? C12 C13 Ti1 C10 -78.0(3) . . . . ? C14 C13 Ti1 C9 -176.4(3) . . . . ? C12 C13 Ti1 C9 68.0(4) . . . . ? C12 C13 Ti1 C14 -115.6(5) . . . . ? C14 C13 Ti1 C11 79.1(3) . . . . ? C12 C13 Ti1 C11 -36.5(3) . . . . ? C14 C13 Ti1 C12 115.6(5) . . . . ? C14 C13 Ti1 C6 -117.4(3) . . . . ? C12 C13 Ti1 C6 127.0(3) . . . . ? C14 C13 Ti1 C5 -158.2(3) . . . . ? C12 C13 Ti1 C5 86.2(4) . . . . ? C14 C13 Ti1 Sb1 68.3(3) . . . . ? C12 C13 Ti1 Sb1 -47.3(4) . . . . ? C14 C13 Ti1 Sb1 -24.1(3) . . . 2_666 ? C12 C13 Ti1 Sb1 -139.7(3) . . . 2_666 ? C12 C11 Ti1 C8 -21.5(4) . . . . ? C10 C11 Ti1 C8 -137.7(3) . . . . ? C12 C11 Ti1 C7 4.4(5) . . . . ? C10 C11 Ti1 C7 -111.8(4) . . . . ? C12 C11 Ti1 C10 116.2(4) . . . . ? C12 C11 Ti1 C9 -58.3(4) . . . . ? C10 C11 Ti1 C9 -174.5(3) . . . . ? C12 C11 Ti1 C14 78.0(3) . . . . ? C10 C11 Ti1 C14 -38.2(3) . . . . ? C12 C11 Ti1 C13 37.0(3) . . . . ? C10 C11 Ti1 C13 -79.2(3) . . . . ? C10 C11 Ti1 C12 -116.2(4) . . . . ? C12 C11 Ti1 C6 -57.6(9) . . . . ? C10 C11 Ti1 C6 -173.8(8) . . . . ? C12 C11 Ti1 C5 -86.0(4) . . . . ? C10 C11 Ti1 C5 157.8(3) . . . . ? C12 C11 Ti1 Sb1 -150.4(3) . . . . ? C10 C11 Ti1 Sb1 93.4(3) . . . . ? C12 C11 Ti1 Sb1 139.9(3) . . . 2_666 ? C10 C11 Ti1 Sb1 23.7(3) . . . 2_666 ? C11 C12 Ti1 C8 160.1(4) . . . . ? C13 C12 Ti1 C8 -83.4(4) . . . . ? C11 C12 Ti1 C7 -177.1(3) . . . . ? C13 C12 Ti1 C7 -60.6(4) . . . . ? C11 C12 Ti1 C10 -37.4(3) . . . . ? C13 C12 Ti1 C10 79.1(3) . . . . ? C11 C12 Ti1 C9 127.0(3) . . . . ? C13 C12 Ti1 C9 -116.5(3) . . . . ? C11 C12 Ti1 C14 -79.2(3) . . . . ? C13 C12 Ti1 C14 37.2(3) . . . . ? C11 C12 Ti1 C13 -116.5(5) . . . . ? C13 C12 Ti1 C11 116.5(5) . . . . ? C11 C12 Ti1 C6 162.7(3) . . . . ? C13 C12 Ti1 C6 -80.8(4) . . . . ? C11 C12 Ti1 C5 121.7(3) . . . . ? C13 C12 Ti1 C5 -121.9(3) . . . . ? C11 C12 Ti1 Sb1 31.2(3) . . . . ? C13 C12 Ti1 Sb1 147.6(3) . . . . ? C11 C12 Ti1 Sb1 -57.9(4) . . . 2_666 ? C13 C12 Ti1 Sb1 58.5(4) . . . 2_666 ? C5 C6 Ti1 C8 -78.4(4) . . . . ? C7 C6 Ti1 C8 39.0(4) . . . . ? C5 C6 Ti1 C7 -117.4(6) . . . . ? C5 C6 Ti1 C10 152.2(5) . . . . ? C7 C6 Ti1 C10 -90.3(7) . . . . ? C5 C6 Ti1 C9 -36.8(4) . . . . ? C7 C6 Ti1 C9 80.6(4) . . . . ? C5 C6 Ti1 C14 -165.3(3) . . . . ? C7 C6 Ti1 C14 -47.8(5) . . . . ? C5 C6 Ti1 C13 -123.2(4) . . . . ? C7 C6 Ti1 C13 -5.7(5) . . . . ? C5 C6 Ti1 C11 -37.6(10) . . . . ? C7 C6 Ti1 C11 79.8(10) . . . . ? C5 C6 Ti1 C12 -81.5(5) . . . . ? C7 C6 Ti1 C12 35.9(5) . . . . ? C7 C6 Ti1 C5 117.4(6) . . . . ? C5 C6 Ti1 Sb1 52.8(4) . . . . ? C7 C6 Ti1 Sb1 170.3(4) . . . . ? C5 C6 Ti1 Sb1 126.0(4) . . . 2_666 ? C7 C6 Ti1 Sb1 -116.5(4) . . . 2_666 ? C6 C5 Ti1 C8 78.3(4) . . . . ? C9 C5 Ti1 C8 -38.1(4) . . . . ? C6 C5 Ti1 C7 36.6(4) . . . . ? C9 C5 Ti1 C7 -79.8(4) . . . . ? C6 C5 Ti1 C10 -146.4(6) . . . . ? C9 C5 Ti1 C10 97.3(7) . . . . ? C6 C5 Ti1 C9 116.4(5) . . . . ? C6 C5 Ti1 C14 39.2(8) . . . . ? C9 C5 Ti1 C14 -77.2(8) . . . . ? C6 C5 Ti1 C13 83.4(4) . . . . ? C9 C5 Ti1 C13 -33.0(5) . . . . ? C6 C5 Ti1 C11 168.1(3) . . . . ? C9 C5 Ti1 C11 51.8(5) . . . . ? C6 C5 Ti1 C12 126.1(4) . . . . ? C9 C5 Ti1 C12 9.7(5) . . . . ? C9 C5 Ti1 C6 -116.4(5) . . . . ? C6 C5 Ti1 Sb1 -127.0(4) . . . . ? C9 C5 Ti1 Sb1 116.6(4) . . . . ? C6 C5 Ti1 Sb1 -54.2(4) . . . 2_666 ? C9 C5 Ti1 Sb1 -170.6(4) . . . 2_666 ? C21 C22 Ti2 C25 101.3(4) . . . . ? C23 C22 Ti2 C25 -144.0(4) . . . . ? C23 C22 Ti2 C21 114.6(6) . . . . ? C21 C22 Ti2 C26 87.7(4) . . . . ? C23 C22 Ti2 C26 -157.7(4) . . . . ? C21 C22 Ti2 C23 -114.6(6) . . . . ? C21 C22 Ti2 C27 53.7(4) . . . . ? C23 C22 Ti2 C27 168.3(4) . . . . ? C21 C22 Ti2 C28 27.3(5) . . . . ? C23 C22 Ti2 C28 141.9(4) . . . . ? C21 C22 Ti2 C20 -36.5(4) . . . . ? C23 C22 Ti2 C20 78.2(4) . . . . ? C21 C22 Ti2 C24 45.2(7) . . . . ? C23 C22 Ti2 C24 159.8(5) . . . . ? C21 C22 Ti2 C19 -77.3(4) . . . . ? C23 C22 Ti2 C19 37.3(4) . . . . ? C21 C22 Ti2 Sb2 170.3(4) . . . 2 ? C23 C22 Ti2 Sb2 -75.1(4) . . . 2 ? C21 C22 Ti2 Sb2 -115.2(4) . . . . ? C23 C22 Ti2 Sb2 -0.6(5) . . . . ? C24 C25 Ti2 C22 -138.6(4) . . . . ? C26 C25 Ti2 C22 -23.7(6) . . . . ? C24 C25 Ti2 C21 -89.6(4) . . . . ? C26 C25 Ti2 C21 25.4(5) . . . . ? C24 C25 Ti2 C26 -114.9(5) . . . . ? C24 C25 Ti2 C23 163.0(7) . . . . ? C26 C25 Ti2 C23 -82.1(8) . . . . ? C24 C25 Ti2 C27 -77.4(4) . . . . ? C26 C25 Ti2 C27 37.5(4) . . . . ? C24 C25 Ti2 C28 -36.1(3) . . . . ? C26 C25 Ti2 C28 78.9(4) . . . . ? C24 C25 Ti2 C20 -39.1(5) . . . . ? C26 C25 Ti2 C20 75.8(5) . . . . ? C26 C25 Ti2 C24 114.9(5) . . . . ? C24 C25 Ti2 C19 37.0(10) . . . . ? C26 C25 Ti2 C19 152.0(8) . . . . ? C24 C25 Ti2 Sb2 149.2(3) . . . 2 ? C26 C25 Ti2 Sb2 -95.9(4) . . . 2 ? C24 C25 Ti2 Sb2 69.7(3) . . . . ? C26 C25 Ti2 Sb2 -175.4(4) . . . . ? C20 C21 Ti2 C22 -116.9(6) . . . . ? C22 C21 Ti2 C25 -115.1(5) . . . . ? C20 C21 Ti2 C25 128.0(4) . . . . ? C22 C21 Ti2 C26 -100.8(5) . . . . ? C20 C21 Ti2 C26 142.3(4) . . . . ? C22 C21 Ti2 C23 38.3(4) . . . . ? C20 C21 Ti2 C23 -78.6(4) . . . . ? C22 C21 Ti2 C27 -125.4(5) . . . . ? C20 C21 Ti2 C27 117.6(4) . . . . ? C22 C21 Ti2 C28 -157.2(5) . . . . ? C20 C21 Ti2 C28 85.9(4) . . . . ? C22 C21 Ti2 C20 116.9(6) . . . . ? C22 C21 Ti2 C24 -157.6(4) . . . . ? C20 C21 Ti2 C24 85.5(4) . . . . ? C22 C21 Ti2 C19 79.2(5) . . . . ? C20 C21 Ti2 C19 -37.7(4) . . . . ? C22 C21 Ti2 Sb2 -11.3(5) . . . 2 ? C20 C21 Ti2 Sb2 -128.2(3) . . . 2 ? C22 C21 Ti2 Sb2 94.3(5) . . . . ? C20 C21 Ti2 Sb2 -22.7(5) . . . . ? C27 C26 Ti2 C22 -81.3(4) . . . . ? C25 C26 Ti2 C22 163.9(4) . . . . ? C27 C26 Ti2 C25 114.8(5) . . . . ? C27 C26 Ti2 C21 -46.8(4) . . . . ? C25 C26 Ti2 C21 -161.6(4) . . . . ? C27 C26 Ti2 C23 -99.7(4) . . . . ? C25 C26 Ti2 C23 145.5(4) . . . . ? C25 C26 Ti2 C27 -114.8(5) . . . . ? C27 C26 Ti2 C28 37.2(3) . . . . ? C25 C26 Ti2 C28 -77.6(4) . . . . ? C27 C26 Ti2 C20 -21.6(4) . . . . ? C25 C26 Ti2 C20 -136.4(4) . . . . ? C27 C26 Ti2 C24 77.7(4) . . . . ? C25 C26 Ti2 C24 -37.1(3) . . . . ? C27 C26 Ti2 C19 -46.8(8) . . . . ? C25 C26 Ti2 C19 -161.6(6) . . . . ? C27 C26 Ti2 Sb2 -166.7(4) . . . 2 ? C25 C26 Ti2 Sb2 78.5(3) . . . 2 ? C27 C26 Ti2 Sb2 120.3(3) . . . . ? C25 C26 Ti2 Sb2 5.5(4) . . . . ? C19 C23 Ti2 C22 114.7(6) . . . . ? C19 C23 Ti2 C25 -158.2(6) . . . . ? C22 C23 Ti2 C25 87.1(7) . . . . ? C19 C23 Ti2 C21 77.4(4) . . . . ? C22 C23 Ti2 C21 -37.3(4) . . . . ? C19 C23 Ti2 C26 147.0(4) . . . . ? C22 C23 Ti2 C26 32.3(6) . . . . ? C19 C23 Ti2 C27 99.1(5) . . . . ? C22 C23 Ti2 C27 -15.6(6) . . . . ? C19 C23 Ti2 C28 50.0(7) . . . . ? C22 C23 Ti2 C28 -64.8(7) . . . . ? C19 C23 Ti2 C20 36.6(4) . . . . ? C22 C23 Ti2 C20 -78.1(4) . . . . ? C19 C23 Ti2 C24 -23.5(12) . . . . ? C22 C23 Ti2 C24 -138.2(10) . . . . ? C22 C23 Ti2 C19 -114.7(6) . . . . ? C19 C23 Ti2 Sb2 -144.5(4) . . . 2 ? C22 C23 Ti2 Sb2 100.8(4) . . . 2 ? C19 C23 Ti2 Sb2 -65.8(4) . . . . ? C22 C23 Ti2 Sb2 179.5(4) . . . . ? C26 C27 Ti2 C22 106.0(4) . . . . ? C28 C27 Ti2 C22 -138.0(4) . . . . ? C26 C27 Ti2 C25 -37.9(4) . . . . ? C28 C27 Ti2 C25 78.1(4) . . . . ? C26 C27 Ti2 C21 133.2(4) . . . . ? C28 C27 Ti2 C21 -110.8(4) . . . . ? C28 C27 Ti2 C26 116.0(5) . . . . ? C26 C27 Ti2 C23 114.9(4) . . . . ? C28 C27 Ti2 C23 -129.1(4) . . . . ? C26 C27 Ti2 C28 -116.0(5) . . . . ? C26 C27 Ti2 C20 162.8(4) . . . . ? C28 C27 Ti2 C20 -81.2(4) . . . . ? C26 C27 Ti2 C24 -78.5(4) . . . . ? C28 C27 Ti2 C24 37.5(3) . . . . ? C26 C27 Ti2 C19 159.4(4) . . . . ? C28 C27 Ti2 C19 -84.7(4) . . . . ? C26 C27 Ti2 Sb2 14.9(4) . . . 2 ? C28 C27 Ti2 Sb2 130.8(3) . . . 2 ? C26 C27 Ti2 Sb2 -86.1(4) . . . . ? C28 C27 Ti2 Sb2 29.9(5) . . . . ? C24 C28 Ti2 C22 165.9(3) . . . . ? C27 C28 Ti2 C22 51.5(4) . . . . ? C24 C28 Ti2 C25 36.0(3) . . . . ? C27 C28 Ti2 C25 -78.4(4) . . . . ? C24 C28 Ti2 C21 -179.4(4) . . . . ? C27 C28 Ti2 C21 66.2(4) . . . . ? C24 C28 Ti2 C26 77.4(4) . . . . ? C27 C28 Ti2 C26 -37.0(4) . . . . ? C24 C28 Ti2 C23 -156.8(5) . . . . ? C27 C28 Ti2 C23 88.8(6) . . . . ? C24 C28 Ti2 C27 114.4(5) . . . . ? C24 C28 Ti2 C20 -145.7(4) . . . . ? C27 C28 Ti2 C20 99.9(4) . . . . ? C27 C28 Ti2 C24 -114.4(5) . . . . ? C24 C28 Ti2 C19 -127.9(3) . . . . ? C27 C28 Ti2 C19 117.7(4) . . . . ? C24 C28 Ti2 Sb2 43.3(4) . . . 2 ? C27 C28 Ti2 Sb2 -71.1(4) . . . 2 ? C24 C28 Ti2 Sb2 -43.8(3) . . . . ? C27 C28 Ti2 Sb2 -158.2(4) . . . . ? C21 C20 Ti2 C22 36.4(4) . . . . ? C19 C20 Ti2 C22 -78.3(5) . . . . ? C21 C20 Ti2 C25 -91.7(5) . . . . ? C19 C20 Ti2 C25 153.6(4) . . . . ? C19 C20 Ti2 C21 -114.7(5) . . . . ? C21 C20 Ti2 C26 -48.5(4) . . . . ? C19 C20 Ti2 C26 -163.2(4) . . . . ? C21 C20 Ti2 C23 78.1(4) . . . . ? C19 C20 Ti2 C23 -36.5(4) . . . . ? C21 C20 Ti2 C27 -60.5(4) . . . . ? C19 C20 Ti2 C27 -175.2(4) . . . . ? C21 C20 Ti2 C28 -94.2(4) . . . . ? C19 C20 Ti2 C28 151.1(4) . . . . ? C21 C20 Ti2 C24 -114.6(4) . . . . ? C19 C20 Ti2 C24 130.7(4) . . . . ? C21 C20 Ti2 C19 114.7(5) . . . . ? C21 C20 Ti2 Sb2 76.6(4) . . . 2 ? C19 C20 Ti2 Sb2 -38.1(5) . . . 2 ? C21 C20 Ti2 Sb2 163.5(3) . . . . ? C19 C20 Ti2 Sb2 48.8(4) . . . . ? C25 C24 Ti2 C22 89.5(6) . . . . ? C28 C24 Ti2 C22 -28.0(7) . . . . ? C28 C24 Ti2 C25 -117.5(5) . . . . ? C25 C24 Ti2 C21 118.3(4) . . . . ? C28 C24 Ti2 C21 0.8(4) . . . . ? C25 C24 Ti2 C26 38.0(4) . . . . ? C28 C24 Ti2 C26 -79.5(4) . . . . ? C25 C24 Ti2 C23 -149.8(9) . . . . ? C28 C24 Ti2 C23 92.7(10) . . . . ? C25 C24 Ti2 C27 79.4(4) . . . . ? C28 C24 Ti2 C27 -38.2(4) . . . . ? C25 C24 Ti2 C28 117.5(5) . . . . ? C25 C24 Ti2 C20 156.4(3) . . . . ? C28 C24 Ti2 C20 38.9(4) . . . . ? C25 C24 Ti2 C19 -167.7(4) . . . . ? C28 C24 Ti2 C19 74.8(4) . . . . ? C25 C24 Ti2 Sb2 -31.6(3) . . . 2 ? C28 C24 Ti2 Sb2 -149.2(3) . . . 2 ? C25 C24 Ti2 Sb2 -106.3(3) . . . . ? C28 C24 Ti2 Sb2 136.1(4) . . . . ? C23 C19 Ti2 C22 -38.2(4) . . . . ? C20 C19 Ti2 C22 78.4(4) . . . . ? C23 C19 Ti2 C25 145.3(8) . . . . ? C20 C19 Ti2 C25 -98.1(8) . . . . ? C23 C19 Ti2 C21 -79.1(5) . . . . ? C20 C19 Ti2 C21 37.6(3) . . . . ? C23 C19 Ti2 C26 -79.1(8) . . . . ? C20 C19 Ti2 C26 37.5(8) . . . . ? C20 C19 Ti2 C23 116.6(6) . . . . ? C23 C19 Ti2 C27 -110.5(5) . . . . ? C20 C19 Ti2 C27 6.2(5) . . . . ? C23 C19 Ti2 C28 -149.9(4) . . . . ? C20 C19 Ti2 C28 -33.3(4) . . . . ? C23 C19 Ti2 C20 -116.6(6) . . . . ? C23 C19 Ti2 C24 172.8(4) . . . . ? C20 C19 Ti2 C24 -70.6(4) . . . . ? C23 C19 Ti2 Sb2 36.7(5) . . . 2 ? C20 C19 Ti2 Sb2 153.3(3) . . . 2 ? C23 C19 Ti2 Sb2 111.9(4) . . . . ? C20 C19 Ti2 Sb2 -131.4(4) . . . . ? C4 C3 Sb1 C1 60.1(4) . . . . ? C4 C3 Sb1 Ti1 -58.1(4) . . . . ? C4 C3 Sb1 Ti1 -179.1(4) . . . 2_666 ? C2 C1 Sb1 C3 54.3(5) . . . . ? C2 C1 Sb1 Ti1 175.2(4) . . . . ? C2 C1 Sb1 Ti1 -63.3(5) . . . 2_666 ? C8 Ti1 Sb1 C3 6.1(3) . . . . ? C7 Ti1 Sb1 C3 -40.2(3) . . . . ? C10 Ti1 Sb1 C3 152.98(19) . . . . ? C9 Ti1 Sb1 C3 8.6(2) . . . . ? C14 Ti1 Sb1 C3 163.3(2) . . . . ? C13 Ti1 Sb1 C3 127.4(2) . . . . ? C11 Ti1 Sb1 C3 118.3(2) . . . . ? C12 Ti1 Sb1 C3 101.3(2) . . . . ? C6 Ti1 Sb1 C3 -47.7(2) . . . . ? C5 Ti1 Sb1 C3 -21.3(2) . . . . ? Sb1 Ti1 Sb1 C3 -125.14(15) 2_666 . . . ? C8 Ti1 Sb1 C1 -100.7(3) . . . . ? C7 Ti1 Sb1 C1 -147.0(3) . . . . ? C10 Ti1 Sb1 C1 46.2(2) . . . . ? C9 Ti1 Sb1 C1 -98.2(2) . . . . ? C14 Ti1 Sb1 C1 56.5(2) . . . . ? C13 Ti1 Sb1 C1 20.6(3) . . . . ? C11 Ti1 Sb1 C1 11.5(2) . . . . ? C12 Ti1 Sb1 C1 -5.5(2) . . . . ? C6 Ti1 Sb1 C1 -154.5(2) . . . . ? C5 Ti1 Sb1 C1 -128.1(2) . . . . ? Sb1 Ti1 Sb1 C1 128.06(17) 2_666 . . . ? C8 Ti1 Sb1 Ti1 131.2(2) . . . 2_666 ? C7 Ti1 Sb1 Ti1 84.9(3) . . . 2_666 ? C10 Ti1 Sb1 Ti1 -81.87(12) . . . 2_666 ? C9 Ti1 Sb1 Ti1 133.74(17) . . . 2_666 ? C14 Ti1 Sb1 Ti1 -71.52(14) . . . 2_666 ? C13 Ti1 Sb1 Ti1 -107.48(19) . . . 2_666 ? C11 Ti1 Sb1 Ti1 -116.60(13) . . . 2_666 ? C12 Ti1 Sb1 Ti1 -133.57(14) . . . 2_666 ? C6 Ti1 Sb1 Ti1 77.40(15) . . . 2_666 ? C5 Ti1 Sb1 Ti1 103.87(16) . . . 2_666 ? Sb1 Ti1 Sb1 Ti1 0 2_666 . . 2_666 ? C16 C15 Sb2 C17 -58.9(5) . . . . ? C16 C15 Sb2 Ti2 -179.4(4) . . . 2 ? C16 C15 Sb2 Ti2 63.5(5) . . . . ? C18 C17 Sb2 C15 -49.4(5) . . . . ? C18 C17 Sb2 Ti2 70.3(4) . . . 2 ? C18 C17 Sb2 Ti2 -171.5(4) . . . . ? C22 Ti2 Sb2 C15 46.4(3) . . . . ? C25 Ti2 Sb2 C15 -157.0(2) . . . . ? C21 Ti2 Sb2 C15 2.3(3) . . . . ? C26 Ti2 Sb2 C15 -160.1(2) . . . . ? C23 Ti2 Sb2 C15 46.0(2) . . . . ? C27 Ti2 Sb2 C15 -118.5(3) . . . . ? C28 Ti2 Sb2 C15 -101.9(2) . . . . ? C20 Ti2 Sb2 C15 -10.3(2) . . . . ? C24 Ti2 Sb2 C15 -125.0(2) . . . . ? C19 Ti2 Sb2 C15 14.9(2) . . . . ? Sb2 Ti2 Sb2 C15 124.68(15) 2 . . . ? C22 Ti2 Sb2 C17 155.5(3) . . . . ? C25 Ti2 Sb2 C17 -47.9(2) . . . . ? C21 Ti2 Sb2 C17 111.4(3) . . . . ? C26 Ti2 Sb2 C17 -51.0(3) . . . . ? C23 Ti2 Sb2 C17 155.1(2) . . . . ? C27 Ti2 Sb2 C17 -9.4(3) . . . . ? C28 Ti2 Sb2 C17 7.3(2) . . . . ? C20 Ti2 Sb2 C17 98.8(2) . . . . ? C24 Ti2 Sb2 C17 -15.8(2) . . . . ? C19 Ti2 Sb2 C17 124.1(3) . . . . ? Sb2 Ti2 Sb2 C17 -126.19(17) 2 . . . ? C22 Ti2 Sb2 Ti2 -78.3(2) . . . 2 ? C25 Ti2 Sb2 Ti2 78.33(14) . . . 2 ? C21 Ti2 Sb2 Ti2 -122.4(2) . . . 2 ? C26 Ti2 Sb2 Ti2 75.23(18) . . . 2 ? C23 Ti2 Sb2 Ti2 -78.66(17) . . . 2 ? C27 Ti2 Sb2 Ti2 116.8(3) . . . 2 ? C28 Ti2 Sb2 Ti2 133.45(14) . . . 2 ? C20 Ti2 Sb2 Ti2 -135.00(13) . . . 2 ? C24 Ti2 Sb2 Ti2 110.35(15) . . . 2 ? C19 Ti2 Sb2 Ti2 -109.73(19) . . . 2 ? Sb2 Ti2 Sb2 Ti2 0 2 . . 2 ? #===END data_om10 _database_code_depnum_ccdc_archive 'CCDC 710425' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C61 H75 Sb9 Si2 Ti5' _chemical_formula_sum 'C61 H75 Sb9 Si2 Ti5' _chemical_formula_weight 2199.64 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' 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 42 n m' _symmetry_space_group_name_Hall 'P 4n -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y, -x, z' 'y, x, z' _cell_length_a 30.281(3) _cell_length_b 30.281(3) _cell_length_c 8.074(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7403(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 53 _cell_measurement_theta_min 3.50 _cell_measurement_theta_max 11.49 _exptl_crystal_description ? _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.9 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.973 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4152 _exptl_absorpt_coefficient_mu 3.795 _exptl_absorpt_correction_type refdelF _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Stuart & Walker, Acta Cryst A, 1983' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 197 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'random variation +/-2.0' _diffrn_reflns_number 23933 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 22.51 _reflns_number_total 3468 _reflns_number_gt 3126 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond, Crystal Impact' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0861P)^2^+128.1821P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(15) _refine_ls_number_reflns 3468 _refine_ls_number_parameters 166 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1771 _refine_ls_wR_factor_gt 0.1704 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.17328(4) 0.82672(4) 0.4967(3) 0.0525(6) Uani 1 2 d S . . Sb2 Sb 0.21910(4) 0.78090(4) 0.0225(3) 0.0504(5) Uani 1 2 d S . . Sb3 Sb 0.23401(4) 0.76599(4) 0.3567(3) 0.0466(5) Uani 1 2 d S . . Sb4 Sb 0.22849(7) 0.87203(5) 0.0210(2) 0.0681(5) Uani 1 1 d . . . Sb5 Sb 0.29670(7) 0.88587(6) 0.2547(2) 0.0760(6) Uani 1 1 d . . . Sb6 Sb 0.17968(7) 0.90332(5) 0.2929(3) 0.0745(6) Uani 1 1 d . . . Ti1 Ti 0.32654(14) 0.79916(18) 0.3974(6) 0.0685(13) Uani 1 1 d . . . C1 C 0.3918(7) 0.7669(8) 0.326(3) 0.085(8) Uiso 1 1 d G . . H1 H 0.4129 0.7629 0.4119 0.102 Uiso 1 1 calc R . . C2 C 0.3588(8) 0.7362(6) 0.278(4) 0.127(13) Uiso 1 1 d G . . H2 H 0.3539 0.7080 0.3263 0.152 Uiso 1 1 calc R . . C3 C 0.3343(8) 0.7550(9) 0.146(4) 0.119(12) Uiso 1 1 d G . . H3 H 0.3102 0.7416 0.0897 0.143 Uiso 1 1 calc R . . C4 C 0.3522(9) 0.7974(9) 0.112(3) 0.153(17) Uiso 1 1 d G . . H4 H 0.3422 0.8173 0.0292 0.184 Uiso 1 1 calc R . . C5 C 0.3877(8) 0.8048(7) 0.223(4) 0.105(11) Uiso 1 1 d G . . H5 H 0.4056 0.8305 0.2283 0.126 Uiso 1 1 calc R . . C6 C 0.3368(7) 0.8466(5) 0.623(3) 0.094(9) Uiso 1 1 d G . . H6 H 0.3368 0.8776 0.6038 0.112 Uiso 1 1 calc R . . C7 C 0.2994(5) 0.8205(8) 0.664(4) 0.107(11) Uiso 1 1 d G . . H7 H 0.2700 0.8308 0.6757 0.128 Uiso 1 1 calc R . . C8 C 0.3137(8) 0.7761(7) 0.683(4) 0.133(14) Uiso 1 1 d G . . H8 H 0.2956 0.7516 0.7097 0.159 Uiso 1 1 calc R . . C9 C 0.3600(8) 0.7748(6) 0.654(4) 0.105(11) Uiso 1 1 d G . . H9 H 0.3782 0.7493 0.6589 0.125 Uiso 1 1 calc R . . C10 C 0.3743(5) 0.8184(7) 0.618(3) 0.086(9) Uiso 1 1 d G . . H10 H 0.4037 0.8272 0.5934 0.104 Uiso 1 1 calc R . . Ti2 Ti 0.2472(3) 0.96612(17) 0.3845(7) 0.105(2) Uani 1 1 d . . . C11 C 0.2142(7) 0.9497(10) 0.649(4) 0.116(12) Uiso 1 1 d G . . H11 H 0.1849 0.9385 0.6560 0.139 Uiso 1 1 calc R . . C12 C 0.2535(9) 0.9242(7) 0.650(4) 0.122(13) Uiso 1 1 d G . . H12 H 0.2552 0.8929 0.6576 0.146 Uiso 1 1 calc R . . C13 C 0.2899(7) 0.9536(10) 0.639(4) 0.128(13) Uiso 1 1 d G . . H13 H 0.3202 0.9455 0.6366 0.154 Uiso 1 1 calc R . . C14 C 0.2730(10) 0.9973(8) 0.630(4) 0.146(16) Uiso 1 1 d G . . H14 H 0.2901 1.0235 0.6220 0.175 Uiso 1 1 calc R . . C15 C 0.2262(10) 0.9949(8) 0.637(5) 0.19(2) Uiso 1 1 d G . . H15 H 0.2064 1.0192 0.6340 0.224 Uiso 1 1 calc R . . C16 C 0.2512(12) 1.0404(9) 0.316(4) 0.140(15) Uiso 1 1 d G . . H16 H 0.2559 1.0608 0.4042 0.168 Uiso 1 1 calc R . . C17 C 0.2846(7) 1.0187(11) 0.224(5) 0.145(16) Uiso 1 1 d G . . H17 H 0.3156 1.0219 0.2386 0.175 Uiso 1 1 calc R . . C18 C 0.2636(10) 0.9912(10) 0.105(4) 0.126(14) Uiso 1 1 d G . . H18 H 0.2781 0.9729 0.0262 0.151 Uiso 1 1 calc R . . C19 C 0.2173(9) 0.9960(11) 0.124(4) 0.153(18) Uiso 1 1 d G . . H19 H 0.1952 0.9814 0.0605 0.183 Uiso 1 1 calc R . . C20 C 0.2096(8) 1.0264(11) 0.255(5) 0.170(18) Uiso 1 1 d G . . H20 H 0.1815 1.0357 0.2941 0.204 Uiso 1 1 calc R . . Ti3 Ti 0.08695(15) 0.91305(15) 0.2155(15) 0.129(4) Uani 1 2 d S . . C21 C 0.1171 0.8829 -0.067(7) 0.14(2) Uiso 1 2 d SD . . H21 H 0.1390 0.8610 -0.0867 0.169 Uiso 1 2 calc SR . . C22 C 0.1240(5) 0.9290(5) -0.050(4) 0.18(2) Uiso 1 1 d D . . H22 H 0.1517 0.9435 -0.0572 0.219 Uiso 1 1 calc R . . C23 C 0.0829(5) 0.9502(5) -0.020(7) 0.21(3) Uiso 1 1 d D . . H23 H 0.0784 0.9809 -0.0024 0.254 Uiso 1 1 calc R . . C26 C 0.0904 0.9096 0.530(6) 0.15(2) Uiso 1 2 d SD . . H26 H 0.1095 0.8905 0.5904 0.179 Uiso 1 2 calc SR . . C27 C 0.0467(6) 0.9000(6) 0.477(5) 0.18(2) Uiso 1 1 d D . . H27 H 0.0311 0.8734 0.4974 0.217 Uiso 1 1 calc R . . C28 C 0.0302(9) 0.9368(9) 0.387(5) 0.19(2) Uiso 1 1 d D . . H28 H 0.0021 0.9389 0.3354 0.227 Uiso 1 1 calc R . . C31 C 0.3477(11) 0.9049(11) 0.065(5) 0.102(11) Uiso 1 1 d . . . H31C H 0.3573 0.8775 0.0085 0.122 Uiso 1 1 calc R . . H31D H 0.3328 0.9234 -0.0193 0.122 Uiso 1 1 calc R . . Si1 Si 0.3980(5) 0.9346(5) 0.134(2) 0.144(5) Uiso 1 1 d D . . C32 C 0.4432(15) 0.9051(15) 0.034(6) 0.21(3) Uiso 1 1 d D . . H32A H 0.4713 0.9192 0.0627 0.314 Uiso 1 1 calc R . . H32B H 0.4391 0.9060 -0.0867 0.314 Uiso 1 1 calc R . . H32C H 0.4433 0.8743 0.0713 0.314 Uiso 1 1 calc R . . C33 C 0.398(2) 0.9900(15) 0.054(7) 0.31(4) Uiso 1 1 d D . . H33A H 0.4247 1.0054 0.0937 0.461 Uiso 1 1 calc R . . H33B H 0.3719 1.0056 0.0932 0.461 Uiso 1 1 calc R . . H33C H 0.3983 0.9892 -0.0669 0.461 Uiso 1 1 calc R . . C34 C 0.4041(15) 0.9309(13) 0.352(4) 0.153(17) Uiso 1 1 d D . . H34A H 0.4305 0.9473 0.3864 0.229 Uiso 1 1 calc R . . H34B H 0.4072 0.8999 0.3844 0.229 Uiso 1 1 calc R . . H34C H 0.3781 0.9436 0.4063 0.229 Uiso 1 1 calc R . . C35 C 0.123(3) 1.112(3) 0.045(9) 0.10(4) Uiso 0.25 1 d PG A -1 H35 H 0.1383 1.1190 0.1450 0.123 Uiso 0.25 1 calc PR A -1 C36 C 0.144(2) 1.087(3) -0.076(11) 0.09(3) Uiso 0.25 1 d PG A -1 H36 H 0.1726 1.0758 -0.0581 0.104 Uiso 0.25 1 calc PR A -1 C37 C 0.121(3) 1.077(3) -0.222(10) 0.10(4) Uiso 0.25 1 d PG A -1 H37 H 0.1353 1.0594 -0.3044 0.124 Uiso 0.25 1 calc PR A -1 C38 C 0.079(3) 1.093(3) -0.248(10) 0.24(10) Uiso 0.25 1 d PG A -1 H38 H 0.0637 1.0861 -0.3475 0.293 Uiso 0.25 1 calc PR A -1 C39 C 0.058(2) 1.118(3) -0.127(12) 0.06(3) Uiso 0.25 1 d PG A -1 H39 H 0.0294 1.1292 -0.1444 0.078 Uiso 0.25 1 calc PR A -1 C40 C 0.081(3) 1.128(3) 0.019(10) 0.3(2) Uiso 0.25 1 d PG A -1 H40 H 0.0667 1.1457 0.1018 0.405 Uiso 0.25 1 calc PR A -1 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 Sb1 0.0524(7) 0.0524(7) 0.0527(12) -0.0060(8) 0.0060(8) 0.0121(9) Sb2 0.0499(7) 0.0499(7) 0.0514(11) -0.0054(8) 0.0054(8) 0.0060(9) Sb3 0.0459(6) 0.0459(6) 0.0481(11) -0.0016(7) 0.0016(7) 0.0087(8) Sb4 0.1010(13) 0.0514(9) 0.0520(9) 0.0034(9) 0.0065(10) 0.0077(8) Sb5 0.0942(13) 0.0751(11) 0.0585(10) -0.0092(10) 0.0185(11) -0.0324(10) Sb6 0.1056(14) 0.0531(9) 0.0647(10) -0.0029(9) 0.0049(12) 0.0280(9) Ti1 0.045(2) 0.113(4) 0.048(3) 0.002(3) 0.006(2) -0.001(2) Ti2 0.187(7) 0.061(3) 0.067(3) -0.011(3) 0.031(4) -0.028(4) Ti3 0.126(6) 0.126(6) 0.133(9) 0.006(4) -0.006(4) 0.096(6) _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 Sb1 Sb3 2.836(3) . ? Sb1 Sb6 2.850(3) 7_665 ? Sb1 Sb6 2.850(3) . ? Sb2 Sb3 2.773(4) . ? Sb2 Sb4 2.774(2) 7_665 ? Sb2 Sb4 2.774(2) . ? Sb3 Ti1 2.995(4) 7_665 ? Sb3 Ti1 2.995(4) . ? Sb4 Sb6 2.811(3) . ? Sb4 Sb5 2.829(3) . ? Sb5 C31 2.25(3) . ? Sb5 Ti1 3.006(6) . ? Sb5 Ti2 3.042(6) . ? Sb6 Ti2 2.888(7) . ? Sb6 Ti3 2.892(6) . ? Ti1 C1 2.28(2) . ? Ti1 C5 2.33(3) . ? Ti1 C6 2.34(2) . ? Ti1 C2 2.35(3) . ? Ti1 C10 2.36(2) . ? Ti1 C7 2.39(3) . ? Ti1 C9 2.42(3) . ? Ti1 C4 2.43(3) . ? Ti1 C8 2.44(3) . ? Ti1 C3 2.44(3) . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C2 C3 1.4200 . ? C3 C4 1.4200 . ? C4 C5 1.4200 . ? C6 C7 1.4200 . ? C6 C10 1.4200 . ? C7 C8 1.4200 . ? C8 C9 1.4200 . ? C9 C10 1.4200 . ? Ti2 C15 2.31(3) . ? Ti2 C16 2.32(3) . ? Ti2 C14 2.33(3) . ? Ti2 C17 2.35(3) . ? Ti2 C20 2.39(3) . ? Ti2 C11 2.41(3) . ? Ti2 C18 2.43(3) . ? Ti2 C13 2.45(3) . ? Ti2 C19 2.46(3) . ? Ti2 C12 2.50(3) . ? C11 C15 1.4200 . ? C11 C12 1.4200 . ? C12 C13 1.4200 . ? C13 C14 1.4200 . ? C14 C15 1.4200 . ? C16 C17 1.4200 . ? C16 C20 1.4200 . ? C17 C18 1.4200 . ? C18 C19 1.4200 . ? C19 C20 1.4200 . ? Ti3 C23 2.21(6) 7_665 ? Ti3 C23 2.21(6) . ? Ti3 C28 2.32(5) 7_665 ? Ti3 C28 2.32(5) . ? Ti3 C22 2.47(3) 7_665 ? Ti3 C22 2.47(3) . ? Ti3 C27 2.47(3) 7_665 ? Ti3 C27 2.47(4) . ? Ti3 C26 2.55(5) . ? Ti3 C21 2.62(5) . ? Ti3 Sb6 2.892(6) 7_665 ? C21 C22 1.419(13) . ? C21 C22 1.419(13) 7_665 ? C22 C23 1.421(12) . ? C23 C23 1.418(18) 7_665 ? C26 C27 1.423(17) . ? C26 C27 1.424(17) 7_665 ? C27 C28 1.422(12) . ? C28 C28 1.410(18) 7_665 ? C31 Si1 1.86(4) . ? Si1 C34 1.78(3) . ? Si1 C33 1.80(4) . ? Si1 C32 1.82(4) . ? C35 C36 1.3900 . ? C35 C40 1.3900(11) . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? 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 Sb3 Sb1 Sb6 104.68(8) . 7_665 ? Sb3 Sb1 Sb6 104.68(8) . . ? Sb6 Sb1 Sb6 77.14(10) 7_665 . ? Sb3 Sb2 Sb4 98.60(7) . 7_665 ? Sb3 Sb2 Sb4 98.60(7) . . ? Sb4 Sb2 Sb4 101.76(10) 7_665 . ? Sb2 Sb3 Sb1 100.18(9) . . ? Sb2 Sb3 Ti1 101.80(10) . 7_665 ? Sb1 Sb3 Ti1 110.22(11) . 7_665 ? Sb2 Sb3 Ti1 101.80(10) . . ? Sb1 Sb3 Ti1 110.22(11) . . ? Ti1 Sb3 Ti1 128.0(2) 7_665 . ? Sb2 Sb4 Sb6 106.14(8) . . ? Sb2 Sb4 Sb5 102.67(8) . . ? Sb6 Sb4 Sb5 79.22(8) . . ? C31 Sb5 Sb4 94.8(9) . . ? C31 Sb5 Ti1 106.1(9) . . ? Sb4 Sb5 Ti1 110.22(11) . . ? C31 Sb5 Ti2 111.6(8) . . ? Sb4 Sb5 Ti2 89.33(16) . . ? Ti1 Sb5 Ti2 135.56(16) . . ? Sb4 Sb6 Sb1 102.26(7) . . ? Sb4 Sb6 Ti2 92.86(14) . . ? Sb1 Sb6 Ti2 115.85(15) . . ? Sb4 Sb6 Ti3 112.1(2) . . ? Sb1 Sb6 Ti3 98.14(16) . . ? Ti2 Sb6 Ti3 132.49(18) . . ? C1 Ti1 C5 35.9(3) . . ? C1 Ti1 C6 110.1(8) . . ? C5 Ti1 C6 108.6(8) . . ? C1 Ti1 C2 35.7(3) . . ? C5 Ti1 C2 58.8(4) . . ? C6 Ti1 C2 139.6(9) . . ? C1 Ti1 C10 76.4(7) . . ? C5 Ti1 C10 87.1(8) . . ? C6 Ti1 C10 35.1(3) . . ? C2 Ti1 C10 104.7(9) . . ? C1 Ti1 C7 129.9(8) . . ? C5 Ti1 C7 142.7(8) . . ? C6 Ti1 C7 34.9(3) . . ? C2 Ti1 C7 136.9(9) . . ? C10 Ti1 C7 57.8(4) . . ? C1 Ti1 C9 73.9(8) . . ? C5 Ti1 C9 101.9(9) . . ? C6 Ti1 C9 57.6(4) . . ? C2 Ti1 C9 86.0(9) . . ? C10 Ti1 C9 34.5(3) . . ? C7 Ti1 C9 57.0(4) . . ? C1 Ti1 C4 58.3(4) . . ? C5 Ti1 C4 34.6(4) . . ? C6 Ti1 C4 135.1(9) . . ? C2 Ti1 C4 57.4(5) . . ? C10 Ti1 C4 121.5(8) . . ? C7 Ti1 C4 165.4(9) . . ? C9 Ti1 C4 132.1(8) . . ? C1 Ti1 C8 104.7(8) . . ? C5 Ti1 C8 135.8(9) . . ? C6 Ti1 C8 57.4(4) . . ? C2 Ti1 C8 102.7(9) . . ? C10 Ti1 C8 57.1(4) . . ? C7 Ti1 C8 34.2(4) . . ? C9 Ti1 C8 34.0(4) . . ? C4 Ti1 C8 160.0(9) . . ? C1 Ti1 C3 58.1(4) . . ? C5 Ti1 C3 57.5(5) . . ? C6 Ti1 C3 166.0(8) . . ? C2 Ti1 C3 34.4(4) . . ? C10 Ti1 C3 134.5(8) . . ? C7 Ti1 C3 158.2(9) . . ? C9 Ti1 C3 120.3(9) . . ? C4 Ti1 C3 33.9(4) . . ? C8 Ti1 C3 130.1(9) . . ? C1 Ti1 Sb3 129.8(6) . . ? C5 Ti1 Sb3 134.6(7) . . ? C6 Ti1 Sb3 114.6(6) . . ? C2 Ti1 Sb3 94.1(6) . . ? C10 Ti1 Sb3 137.5(5) . . ? C7 Ti1 Sb3 82.4(5) . . ? C9 Ti1 Sb3 112.5(6) . . ? C4 Ti1 Sb3 100.8(7) . . ? C8 Ti1 Sb3 81.9(5) . . ? C3 Ti1 Sb3 79.4(6) . . ? C1 Ti1 Sb5 122.6(6) . . ? C5 Ti1 Sb5 86.8(6) . . ? C6 Ti1 Sb5 78.6(5) . . ? C2 Ti1 Sb5 132.6(7) . . ? C10 Ti1 Sb5 104.9(5) . . ? C7 Ti1 Sb5 90.3(6) . . ? C9 Ti1 Sb5 136.0(5) . . ? C4 Ti1 Sb5 75.7(6) . . ? C8 Ti1 Sb5 124.4(6) . . ? C3 Ti1 Sb5 100.9(7) . . ? Sb3 Ti1 Sb5 88.27(13) . . ? C2 C1 C5 108.0 . . ? C2 C1 Ti1 74.9(11) . . ? C5 C1 Ti1 74.1(11) . . ? C1 C2 C3 108.0 . . ? C1 C2 Ti1 69.4(10) . . ? C3 C2 Ti1 76.4(10) . . ? C4 C3 C2 108.0 . . ? C4 C3 Ti1 72.7(10) . . ? C2 C3 Ti1 69.2(9) . . ? C3 C4 C5 108.0 . . ? C3 C4 Ti1 73.5(10) . . ? C5 C4 Ti1 68.8(9) . . ? C4 C5 C1 108.0 . . ? C4 C5 Ti1 76.6(10) . . ? C1 C5 Ti1 70.0(10) . . ? C7 C6 C10 108.0 . . ? C7 C6 Ti1 74.3(10) . . ? C10 C6 Ti1 73.2(10) . . ? C8 C7 C6 108.0 . . ? C8 C7 Ti1 74.8(10) . . ? C6 C7 Ti1 70.8(10) . . ? C9 C8 C7 108.0 . . ? C9 C8 Ti1 72.4(10) . . ? C7 C8 Ti1 71.0(10) . . ? C8 C9 C10 108.0 . . ? C8 C9 Ti1 73.6(10) . . ? C10 C9 Ti1 70.5(10) . . ? C9 C10 C6 108.0 . . ? C9 C10 Ti1 75.0(10) . . ? C6 C10 Ti1 71.7(10) . . ? C15 Ti2 C16 81.9(10) . . ? C15 Ti2 C14 35.6(5) . . ? C16 Ti2 C14 78.0(10) . . ? C15 Ti2 C17 111.5(12) . . ? C16 Ti2 C17 35.4(4) . . ? C14 Ti2 C17 92.0(10) . . ? C15 Ti2 C20 88.2(11) . . ? C16 Ti2 C20 35.0(4) . . ? C14 Ti2 C20 102.9(12) . . ? C17 Ti2 C20 58.0(5) . . ? C15 Ti2 C11 34.9(4) . . ? C16 Ti2 C11 115.6(11) . . ? C14 Ti2 C11 57.9(5) . . ? C17 Ti2 C11 146.2(11) . . ? C20 Ti2 C11 110.4(10) . . ? C15 Ti2 C18 139.4(9) . . ? C16 Ti2 C18 57.7(5) . . ? C14 Ti2 C18 126.5(10) . . ? C17 Ti2 C18 34.5(4) . . ? C20 Ti2 C18 56.8(5) . . ? C11 Ti2 C18 166.3(10) . . ? C15 Ti2 C13 57.6(5) . . ? C16 Ti2 C13 108.7(10) . . ? C14 Ti2 C13 34.4(4) . . ? C17 Ti2 C13 108.2(10) . . ? C20 Ti2 C13 137.3(12) . . ? C11 Ti2 C13 56.3(5) . . ? C18 Ti2 C13 135.7(10) . . ? C15 Ti2 C19 121.0(11) . . ? C16 Ti2 C19 57.3(5) . . ? C14 Ti2 C19 134.6(10) . . ? C17 Ti2 C19 57.0(5) . . ? C20 Ti2 C19 34.0(4) . . ? C11 Ti2 C19 132.9(11) . . ? C18 Ti2 C19 33.7(4) . . ? C13 Ti2 C19 164.7(9) . . ? C15 Ti2 C12 56.9(5) . . ? C16 Ti2 C12 133.8(9) . . ? C14 Ti2 C12 56.6(5) . . ? C17 Ti2 C12 141.5(10) . . ? C20 Ti2 C12 143.1(10) . . ? C11 Ti2 C12 33.5(4) . . ? C18 Ti2 C12 159.9(10) . . ? C13 Ti2 C12 33.3(4) . . ? C19 Ti2 C12 161.4(10) . . ? C15 Ti2 Sb6 106.3(9) . . ? C16 Ti2 Sb6 128.0(9) . . ? C14 Ti2 Sb6 136.2(7) . . ? C17 Ti2 Sb6 130.3(8) . . ? C20 Ti2 Sb6 93.0(9) . . ? C11 Ti2 Sb6 78.3(6) . . ? C18 Ti2 Sb6 96.5(8) . . ? C13 Ti2 Sb6 119.0(7) . . ? C19 Ti2 Sb6 76.3(7) . . ? C12 Ti2 Sb6 86.5(6) . . ? C15 Ti2 Sb5 137.9(7) . . ? C16 Ti2 Sb5 131.9(9) . . ? C14 Ti2 Sb5 116.8(8) . . ? C17 Ti2 Sb5 96.5(9) . . ? C20 Ti2 Sb5 133.9(9) . . ? C11 Ti2 Sb5 110.2(7) . . ? C18 Ti2 Sb5 80.1(6) . . ? C13 Ti2 Sb5 84.5(7) . . ? C19 Ti2 Sb5 100.4(9) . . ? C12 Ti2 Sb5 81.5(6) . . ? Sb6 Ti2 Sb5 74.61(13) . . ? C15 C11 C12 108.0 . . ? C15 C11 Ti2 68.4(13) . . ? C12 C11 Ti2 76.7(12) . . ? C11 C12 C13 108.0 . . ? C11 C12 Ti2 69.8(12) . . ? C13 C12 Ti2 71.5(11) . . ? C14 C13 C12 108.0 . . ? C14 C13 Ti2 68.1(12) . . ? C12 C13 Ti2 75.2(11) . . ? C13 C14 C15 108.0 . . ? C13 C14 Ti2 77.5(13) . . ? C15 C14 Ti2 71.2(12) . . ? C11 C15 C14 108.0 . . ? C11 C15 Ti2 76.6(12) . . ? C14 C15 Ti2 73.2(12) . . ? C17 C16 C20 108.0 . . ? C17 C16 Ti2 73.3(12) . . ? C20 C16 Ti2 75.3(13) . . ? C16 C17 C18 108.0 . . ? C16 C17 Ti2 71.2(12) . . ? C18 C17 Ti2 76.2(12) . . ? C19 C18 C17 108.0 . . ? C19 C18 Ti2 74.2(12) . . ? C17 C18 Ti2 69.3(11) . . ? C18 C19 C20 108.0 . . ? C18 C19 Ti2 72.1(12) . . ? C20 C19 Ti2 70.3(11) . . ? C19 C20 C16 108.0 . . ? C19 C20 Ti2 75.7(11) . . ? C16 C20 Ti2 69.6(12) . . ? C23 Ti3 C23 37.4(11) 7_665 . ? C23 Ti3 C28 108.2(9) 7_665 7_665 ? C23 Ti3 C28 96.7(10) . 7_665 ? C23 Ti3 C28 96.7(10) 7_665 . ? C23 Ti3 C28 108.2(9) . . ? C28 Ti3 C28 35.4(9) 7_665 . ? C23 Ti3 C22 34.8(5) 7_665 7_665 ? C23 Ti3 C22 58.3(9) . 7_665 ? C28 Ti3 C22 142.5(8) 7_665 7_665 ? C28 Ti3 C22 120.9(8) . 7_665 ? C23 Ti3 C22 58.3(9) 7_665 . ? C23 Ti3 C22 34.8(5) . . ? C28 Ti3 C22 120.9(8) 7_665 . ? C28 Ti3 C22 142.5(8) . . ? C22 Ti3 C22 54.8(9) 7_665 . ? C23 Ti3 C27 142.0(8) 7_665 7_665 ? C23 Ti3 C27 119.4(9) . 7_665 ? C28 Ti3 C27 34.4(5) 7_665 7_665 ? C28 Ti3 C27 57.1(9) . 7_665 ? C22 Ti3 C27 176.8(8) 7_665 7_665 ? C22 Ti3 C27 124.9(7) . 7_665 ? C23 Ti3 C27 119.4(9) 7_665 . ? C23 Ti3 C27 142.0(8) . . ? C28 Ti3 C27 57.1(9) 7_665 . ? C28 Ti3 C27 34.4(5) . . ? C22 Ti3 C27 124.9(7) 7_665 . ? C22 Ti3 C27 176.8(8) . . ? C27 Ti3 C27 55.1(11) 7_665 . ? C23 Ti3 C26 151.7(7) 7_665 . ? C23 Ti3 C26 151.7(7) . . ? C28 Ti3 C26 56.6(8) 7_665 . ? C28 Ti3 C26 56.6(9) . . ? C22 Ti3 C26 148.9(5) 7_665 . ? C22 Ti3 C26 148.9(5) . . ? C27 Ti3 C26 32.9(7) 7_665 . ? C27 Ti3 C26 32.9(7) . . ? C23 Ti3 C21 56.6(8) 7_665 . ? C23 Ti3 C21 56.6(8) . . ? C28 Ti3 C21 152.2(9) 7_665 . ? C28 Ti3 C21 152.2(9) . . ? C22 Ti3 C21 32.2(6) 7_665 . ? C22 Ti3 C21 32.2(6) . . ? C27 Ti3 C21 149.3(5) 7_665 . ? C27 Ti3 C21 149.3(5) . . ? C26 Ti3 C21 147.2(7) . . ? C23 Ti3 Sb6 133.3(8) 7_665 . ? C23 Ti3 Sb6 107.0(4) . . ? C28 Ti3 Sb6 104.4(6) 7_665 . ? C28 Ti3 Sb6 128.5(8) . . ? C22 Ti3 Sb6 109.4(5) 7_665 . ? C22 Ti3 Sb6 76.5(5) . . ? C27 Ti3 Sb6 73.1(5) 7_665 . ? C27 Ti3 Sb6 106.2(7) . . ? C26 Ti3 Sb6 74.9(2) . . ? C21 Ti3 Sb6 79.3(5) . . ? C23 Ti3 Sb6 107.0(5) 7_665 7_665 ? C23 Ti3 Sb6 133.3(7) . 7_665 ? C28 Ti3 Sb6 128.5(8) 7_665 7_665 ? C28 Ti3 Sb6 104.4(6) . 7_665 ? C22 Ti3 Sb6 76.5(5) 7_665 7_665 ? C22 Ti3 Sb6 109.4(5) . 7_665 ? C27 Ti3 Sb6 106.2(7) 7_665 7_665 ? C27 Ti3 Sb6 73.1(5) . 7_665 ? C26 Ti3 Sb6 74.9(2) . 7_665 ? C21 Ti3 Sb6 79.3(5) . 7_665 ? Sb6 Ti3 Sb6 75.84(18) . 7_665 ? C22 C21 C22 106.2(13) . 7_665 ? C22 C21 Ti3 67.8(12) . . ? C22 C21 Ti3 67.8(12) 7_665 . ? C21 C22 C23 109.4(12) . . ? C21 C22 Ti3 80.0(16) . . ? C23 C22 Ti3 63(2) . . ? C23 C23 C22 107.5(7) 7_665 . ? C23 C23 Ti3 71.3(5) 7_665 . ? C22 C23 Ti3 82(2) . . ? C27 C26 C27 106.6(13) . 7_665 ? C27 C26 Ti3 70.4(12) . . ? C27 C26 Ti3 70.4(12) 7_665 . ? C28 C27 C26 108.8(12) . . ? C28 C27 Ti3 67(2) . . ? C26 C27 Ti3 76.6(15) . . ? C28 C28 C27 107.9(9) 7_665 . ? C28 C28 Ti3 72.3(4) 7_665 . ? C27 C28 Ti3 79(2) . . ? Si1 C31 Sb5 118.9(19) . . ? C34 Si1 C33 114(2) . . ? C34 Si1 C32 109(2) . . ? C33 Si1 C32 107(2) . . ? C34 Si1 C31 111(2) . . ? C33 Si1 C31 111(3) . . ? C32 Si1 C31 104(2) . . ? C36 C35 C40 120.00(8) . . ? C37 C36 C35 120.00(7) . . ? C36 C37 C38 120.00(7) . . ? C39 C38 C37 120.00(7) . . ? C38 C39 C40 120.00(6) . . ? C39 C40 C35 120.00(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.192 _refine_diff_density_min -1.182 _refine_diff_density_rms 0.172 #===END #===END data_om20 _database_code_depnum_ccdc_archive 'CCDC 710426' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C57 H66 N3 Sb4 Ti3, 2.5(C6 H6)' _chemical_formula_sum 'C72 H81 N3 Sb4 Ti3' _chemical_formula_weight 1619.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 Rhombohedral _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 15.2155(14) _cell_length_b 15.2155(14) _cell_length_c 50.767(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10178.5(18) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 2.401 _cell_measurement_theta_max 12.498 _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4824 _exptl_absorpt_coefficient_mu 1.945 _exptl_absorpt_correction_type refdelF _exptl_absorpt_correction_T_min 0.3882 _exptl_absorpt_correction_T_max 0.8293 _exptl_absorpt_process_details 'Stuart & Walker, Acta Cryst A, 1983' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 197 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'random variation +/-2.0' _diffrn_reflns_number 6156 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 65 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5038 _reflns_number_gt 4220 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond, Crystal Impact' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; The remaining electron density is located close to one of the C6H6 rings (1.6A) and indicating a disordered ring system. A further treatment of this disordering does not lead to significant better results. 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^)+(0.0498P)^2^+32.9537P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00015(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5038 _refine_ls_number_parameters 251 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.3333 0.6667 0.542312(8) 0.02241(12) Uani 1 3 d S . . Sb2 Sb 0.475373(19) 0.801665(19) 0.579372(5) 0.02146(10) Uani 1 1 d . . . N1 N 0.7919(5) 1.0678(4) 0.60564(10) 0.084(2) Uani 1 1 d D . . C1 C 0.5955(3) 0.9144(3) 0.55452(8) 0.0272(8) Uani 1 1 d . . . C2 C 0.6805(3) 0.9970(3) 0.56582(9) 0.0327(9) Uani 1 1 d . . . C3 C 0.7544(4) 1.0707(4) 0.54952(11) 0.0479(13) Uani 1 1 d . . . H3 H 0.8117 1.1272 0.5572 0.058 Uiso 1 1 calc R . . C4 C 0.7464(4) 1.0633(4) 0.52259(11) 0.0517(14) Uani 1 1 d . . . H4 H 0.7976 1.1141 0.5118 0.062 Uiso 1 1 calc R . . C5 C 0.6631(4) 0.9810(4) 0.51129(9) 0.0402(11) Uani 1 1 d . . . H5 H 0.6573 0.9747 0.4927 0.048 Uiso 1 1 calc R . . C6 C 0.5885(3) 0.9084(3) 0.52709(8) 0.0318(9) Uani 1 1 d . . . H6 H 0.5309 0.8529 0.5191 0.038 Uiso 1 1 calc R . . C7 C 0.6909(4) 1.0058(4) 0.59588(10) 0.0466(13) Uani 1 1 d . . . H7A H 0.6485 1.0335 0.6025 0.056 Uiso 1 1 calc R . . H7B H 0.6631 0.9368 0.6033 0.056 Uiso 1 1 calc R . . C8 C 0.8500(7) 1.0146(7) 0.6011(2) 0.092(3) Uani 1 1 d D . . H8A H 0.8180 0.9503 0.6108 0.139 Uiso 1 1 calc R . . H8B H 0.9198 1.0573 0.6074 0.139 Uiso 1 1 calc R . . H8C H 0.8506 1.0013 0.5823 0.139 Uiso 1 1 calc R . . C9 C 0.7898(6) 1.0852(6) 0.63419(12) 0.088(3) Uani 1 1 d D . . H9A H 0.7457 1.1138 0.6376 0.132 Uiso 1 1 calc R . . H9B H 0.8587 1.1328 0.6403 0.132 Uiso 1 1 calc R . . H9C H 0.7636 1.0207 0.6436 0.132 Uiso 1 1 calc R . . Ti1 Ti 0.54112(5) 0.65640(6) 0.595317(13) 0.02393(17) Uani 1 1 d . . . C10 C 0.5939(5) 0.6878(6) 0.55068(10) 0.0554(16) Uani 1 1 d . . . H10 H 0.5620 0.7122 0.5391 0.066 Uiso 1 1 d R . . C11 C 0.6762(5) 0.7446(5) 0.56516(14) 0.0624(18) Uani 1 1 d . . . H11 H 0.7131 0.8167 0.5652 0.075 Uiso 1 1 d R . . C12 C 0.6988(4) 0.6832(6) 0.57946(12) 0.0602(18) Uani 1 1 d . . . H12 H 0.7545 0.7049 0.5912 0.072 Uiso 1 1 d R . . C13 C 0.6268(6) 0.5829(6) 0.57438(13) 0.071(2) Uani 1 1 d . . . H13 H 0.6220 0.5237 0.5821 0.085 Uiso 1 1 d R . . C14 C 0.5601(4) 0.5875(6) 0.55507(13) 0.066(2) Uani 1 1 d . . . H14 H 0.5045 0.5308 0.5469 0.080 Uiso 1 1 d R . . C15 C 0.4671(4) 0.6433(4) 0.63711(8) 0.0380(11) Uani 1 1 d . . . H15 H 0.4001 0.6326 0.6379 0.046 Uiso 1 1 d R . . C16 C 0.5557(4) 0.7366(4) 0.63707(9) 0.0414(11) Uani 1 1 d . . . H16 H 0.5601 0.8009 0.6383 0.050 Uiso 1 1 d R . . C17 C 0.6371(4) 0.7188(5) 0.63500(10) 0.0498(14) Uani 1 1 d . . . H17 H 0.7068 0.7693 0.6342 0.060 Uiso 1 1 d R . . C18 C 0.6000(5) 0.6155(5) 0.63411(10) 0.0520(15) Uani 1 1 d . . . H18 H 0.6388 0.5824 0.6328 0.062 Uiso 1 1 d R . . C19 C 0.4925(4) 0.5666(4) 0.63564(8) 0.0416(11) Uani 1 1 d . . . H19 H 0.4465 0.4955 0.6358 0.050 Uiso 1 1 d R . . C20 C 0.6951(4) 0.4348(4) 0.53158(10) 0.0447(12) Uani 1 1 d . . . H20 H 0.7145 0.5046 0.5316 0.054 Uiso 1 1 calc R . . C21 C 0.5933(4) 0.3614(4) 0.53159(10) 0.0443(12) Uani 1 1 d . . . H21 H 0.5429 0.3808 0.5316 0.053 Uiso 1 1 calc R . . C22 C 0.9002(14) 0.9694(13) 0.5242(5) 0.126(10) Uani 0.50 1 d P . . H22 H 0.8303 0.9489 0.5257 0.151 Uiso 0.50 1 calc PR . . C23 C 0.9732(13) 1.0697(14) 0.5230(5) 0.119(9) Uani 0.50 1 d P . . H23 H 0.9527 1.1190 0.5214 0.142 Uiso 0.50 1 calc PR . . C24 C 0.6392(16) 0.2908(14) 0.6035(2) 0.126(9) Uiso 0.50 1 d PG A -1 H24 H 0.6363 0.2772 0.5852 0.151 Uiso 0.50 1 calc PR A -1 C25 C 0.7037(16) 0.2748(17) 0.6197(4) 0.079(6) Uiso 0.25 1 d PG A -1 H25 H 0.7448 0.2502 0.6124 0.095 Uiso 0.25 1 calc PR A -1 C26 C 0.7080(17) 0.295(2) 0.6465(3) 0.077(6) Uiso 0.25 1 d PG A -1 H26 H 0.7520 0.2838 0.6575 0.092 Uiso 0.25 1 calc PR A -1 C27 C 0.6478(19) 0.3308(19) 0.6572(2) 0.155(8) Uiso 0.50 1 d PG A -1 H27 H 0.6508 0.3444 0.6755 0.187 Uiso 0.50 1 calc PR A -1 C28 C 0.5834(18) 0.3468(19) 0.6410(4) 0.077(6) Uiso 0.25 1 d PG A -1 H28 H 0.5423 0.3714 0.6483 0.092 Uiso 0.25 1 calc PR A -1 C29 C 0.5791(16) 0.3268(17) 0.6142(3) 0.079(6) Uiso 0.25 1 d PG A -1 H29 H 0.5351 0.3378 0.6032 0.095 Uiso 0.25 1 calc PR A -1 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 Sb1 0.02324(16) 0.02324(16) 0.0208(2) 0.000 0.000 0.01162(8) Sb2 0.02078(15) 0.02016(15) 0.02176(14) 0.00081(9) 0.00072(9) 0.00896(11) N1 0.069(4) 0.068(4) 0.049(3) 0.009(3) -0.010(3) -0.016(3) C1 0.024(2) 0.0207(19) 0.033(2) 0.0027(16) 0.0022(16) 0.0086(16) C2 0.028(2) 0.028(2) 0.032(2) 0.0007(17) 0.0040(17) 0.0059(18) C3 0.037(3) 0.036(3) 0.051(3) 0.004(2) 0.002(2) 0.003(2) C4 0.045(3) 0.039(3) 0.047(3) 0.017(2) 0.013(2) 0.003(2) C5 0.045(3) 0.043(3) 0.032(2) 0.013(2) 0.011(2) 0.021(2) C6 0.030(2) 0.029(2) 0.032(2) 0.0037(17) 0.0000(17) 0.0113(19) C7 0.033(3) 0.045(3) 0.039(3) 0.001(2) 0.001(2) 0.002(2) C8 0.075(5) 0.094(7) 0.111(7) 0.006(5) -0.005(5) 0.045(5) C9 0.082(5) 0.081(5) 0.050(4) -0.010(4) -0.021(4) 0.003(4) Ti1 0.0227(3) 0.0297(4) 0.0228(3) -0.0003(3) 0.0001(3) 0.0157(3) C10 0.074(4) 0.091(5) 0.035(3) 0.010(3) 0.019(3) 0.066(4) C11 0.059(4) 0.052(3) 0.071(4) 0.010(3) 0.041(3) 0.023(3) C12 0.032(3) 0.101(6) 0.055(3) -0.025(3) -0.003(2) 0.038(3) C13 0.113(6) 0.081(5) 0.065(4) 0.033(4) 0.054(4) 0.084(5) C14 0.026(3) 0.088(5) 0.061(4) -0.042(4) 0.014(2) 0.010(3) C15 0.037(2) 0.061(3) 0.021(2) -0.0003(19) 0.0007(17) 0.029(2) C16 0.057(3) 0.039(3) 0.025(2) -0.0051(18) -0.005(2) 0.022(2) C17 0.034(3) 0.072(4) 0.031(2) -0.003(2) -0.010(2) 0.018(3) C18 0.070(4) 0.084(4) 0.031(2) 0.002(3) -0.007(2) 0.060(4) C19 0.056(3) 0.043(3) 0.024(2) 0.0075(19) 0.001(2) 0.023(2) C20 0.052(3) 0.037(3) 0.042(3) -0.001(2) -0.001(2) 0.020(2) C21 0.043(3) 0.055(3) 0.043(3) -0.002(2) 0.004(2) 0.031(3) C22 0.064(10) 0.049(9) 0.25(3) 0.019(13) -0.051(14) 0.017(8) C23 0.056(10) 0.059(10) 0.25(3) -0.004(13) -0.030(13) 0.033(8) _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 Sb1 Sb2 2.8267(4) 2_665 ? Sb1 Sb2 2.8267(4) . ? Sb1 Sb2 2.8267(4) 3_565 ? Sb2 C1 2.177(4) . ? Sb2 Ti1 2.9584(8) . ? Sb2 Ti1 2.9676(8) 2_665 ? N1 C7 1.431(8) . ? N1 C9 1.477(7) . ? N1 C8 1.484(7) . ? C1 C6 1.396(6) . ? C1 C2 1.398(6) . ? C2 C3 1.395(7) . ? C2 C7 1.533(7) . ? C3 C4 1.372(8) . ? C4 C5 1.384(8) . ? C5 C6 1.378(6) . ? Ti1 C13 2.353(5) . ? Ti1 C15 2.363(4) . ? Ti1 C12 2.365(5) . ? Ti1 C19 2.365(5) . ? Ti1 C11 2.369(5) . ? Ti1 C10 2.371(5) . ? Ti1 C18 2.372(5) . ? Ti1 C14 2.379(5) . ? Ti1 C17 2.389(5) . ? Ti1 C16 2.400(5) . ? Ti1 Sb2 2.9676(8) 3_565 ? C10 C11 1.332(10) . ? C10 C14 1.363(10) . ? C11 C12 1.356(10) . ? C12 C13 1.387(10) . ? C13 C14 1.438(10) . ? C15 C16 1.385(7) . ? C15 C19 1.402(7) . ? C16 C17 1.398(8) . ? C17 C18 1.381(9) . ? C18 C19 1.421(8) . ? C20 C21 1.375(8) 3_665 ? C20 C21 1.384(8) . ? C21 C20 1.375(8) 2_655 ? C22 C23 1.30(2) 2_765 ? C22 C23 1.37(2) . ? C23 C22 1.30(2) 3_675 ? C24 C25 1.3900 . ? C24 C29 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? 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 Sb2 Sb1 Sb2 80.532(14) 2_665 . ? Sb2 Sb1 Sb2 80.532(14) 2_665 3_565 ? Sb2 Sb1 Sb2 80.532(14) . 3_565 ? C1 Sb2 Sb1 102.86(11) . . ? C1 Sb2 Ti1 106.41(11) . . ? Sb1 Sb2 Ti1 93.470(16) . . ? C1 Sb2 Ti1 107.62(11) . 2_665 ? Sb1 Sb2 Ti1 93.274(16) . 2_665 ? Ti1 Sb2 Ti1 142.79(3) . 2_665 ? C7 N1 C9 110.2(5) . . ? C7 N1 C8 108.9(6) . . ? C9 N1 C8 108.7(7) . . ? C6 C1 C2 118.3(4) . . ? C6 C1 Sb2 121.3(3) . . ? C2 C1 Sb2 120.3(3) . . ? C3 C2 C1 119.4(4) . . ? C3 C2 C7 120.9(4) . . ? C1 C2 C7 119.7(4) . . ? C4 C3 C2 121.5(5) . . ? C3 C4 C5 119.4(4) . . ? C6 C5 C4 119.9(4) . . ? C5 C6 C1 121.5(4) . . ? N1 C7 C2 115.6(4) . . ? C13 Ti1 C15 136.00(19) . . ? C13 Ti1 C12 34.2(3) . . ? C15 Ti1 C12 136.0(2) . . ? C13 Ti1 C19 101.8(2) . . ? C15 Ti1 C19 34.50(18) . . ? C12 Ti1 C19 113.1(2) . . ? C13 Ti1 C11 56.4(2) . . ? C15 Ti1 C11 150.5(2) . . ? C12 Ti1 C11 33.3(2) . . ? C19 Ti1 C11 145.0(2) . . ? C13 Ti1 C10 56.8(2) . . ? C15 Ti1 C10 166.87(18) . . ? C12 Ti1 C10 55.1(2) . . ? C19 Ti1 C10 156.9(2) . . ? C11 Ti1 C10 32.6(2) . . ? C13 Ti1 C18 83.0(2) . . ? C15 Ti1 C18 57.26(18) . . ? C12 Ti1 C18 81.0(2) . . ? C19 Ti1 C18 34.9(2) . . ? C11 Ti1 C18 110.5(3) . . ? C10 Ti1 C18 135.4(2) . . ? C13 Ti1 C14 35.4(3) . . ? C15 Ti1 C14 153.1(2) . . ? C12 Ti1 C14 56.5(2) . . ? C19 Ti1 C14 124.1(3) . . ? C11 Ti1 C14 55.4(2) . . ? C10 Ti1 C14 33.4(2) . . ? C18 Ti1 C14 116.9(3) . . ? C13 Ti1 C17 101.3(3) . . ? C15 Ti1 C17 56.44(18) . . ? C12 Ti1 C17 81.5(2) . . ? C19 Ti1 C17 56.8(2) . . ? C11 Ti1 C17 97.8(2) . . ? C10 Ti1 C17 130.4(2) . . ? C18 Ti1 C17 33.7(2) . . ? C14 Ti1 C17 135.6(2) . . ? C13 Ti1 C16 135.1(3) . . ? C15 Ti1 C16 33.80(18) . . ? C12 Ti1 C16 112.7(2) . . ? C19 Ti1 C16 56.78(18) . . ? C11 Ti1 C16 116.7(2) . . ? C10 Ti1 C16 143.7(2) . . ? C18 Ti1 C16 56.61(19) . . ? C14 Ti1 C16 169.1(2) . . ? C17 Ti1 C16 33.9(2) . . ? C13 Ti1 Sb2 134.92(15) . . ? C15 Ti1 Sb2 89.07(13) . . ? C12 Ti1 Sb2 118.1(2) . . ? C19 Ti1 Sb2 122.91(14) . . ? C11 Ti1 Sb2 85.52(18) . . ? C10 Ti1 Sb2 78.17(14) . . ? C18 Ti1 Sb2 137.44(15) . . ? C14 Ti1 Sb2 104.8(2) . . ? C17 Ti1 Sb2 107.54(16) . . ? C16 Ti1 Sb2 80.86(13) . . ? C13 Ti1 Sb2 103.9(2) . 3_565 ? C15 Ti1 Sb2 82.55(13) . 3_565 ? C12 Ti1 Sb2 134.70(16) . 3_565 ? C19 Ti1 Sb2 85.70(14) . 3_565 ? C11 Ti1 Sb2 123.9(2) . 3_565 ? C10 Ti1 Sb2 91.31(19) . 3_565 ? C18 Ti1 Sb2 118.82(18) . 3_565 ? C14 Ti1 Sb2 78.65(14) . 3_565 ? C17 Ti1 Sb2 138.29(14) . 3_565 ? C16 Ti1 Sb2 112.01(14) . 3_565 ? Sb2 Ti1 Sb2 76.139(19) . 3_565 ? C11 C10 C14 110.0(6) . . ? C11 C10 Ti1 73.6(3) . . ? C14 C10 Ti1 73.6(3) . . ? C10 C11 C12 109.2(6) . . ? C10 C11 Ti1 73.8(3) . . ? C12 C11 Ti1 73.2(3) . . ? C11 C12 C13 109.0(6) . . ? C11 C12 Ti1 73.5(3) . . ? C13 C12 Ti1 72.5(3) . . ? C12 C13 C14 105.2(6) . . ? C12 C13 Ti1 73.3(3) . . ? C14 C13 Ti1 73.3(3) . . ? C10 C14 C13 106.6(6) . . ? C10 C14 Ti1 73.0(3) . . ? C13 C14 Ti1 71.3(3) . . ? C16 C15 C19 108.7(5) . . ? C16 C15 Ti1 74.6(3) . . ? C19 C15 Ti1 72.8(3) . . ? C15 C16 C17 107.7(5) . . ? C15 C16 Ti1 71.6(3) . . ? C17 C16 Ti1 72.6(3) . . ? C18 C17 C16 109.0(5) . . ? C18 C17 Ti1 72.5(3) . . ? C16 C17 Ti1 73.5(3) . . ? C17 C18 C19 107.5(5) . . ? C17 C18 Ti1 73.8(3) . . ? C19 C18 Ti1 72.3(3) . . ? C15 C19 C18 107.0(5) . . ? C15 C19 Ti1 72.7(3) . . ? C18 C19 Ti1 72.8(3) . . ? C21 C20 C21 120.0(6) 3_665 . ? C20 C21 C20 120.0(6) 2_655 . ? C23 C22 C23 117(2) 2_765 . ? C22 C23 C22 122(2) 3_675 . ? C25 C24 C29 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C27 120.0 . . ? C26 C27 C28 120.0 . . ? C29 C28 C27 120.0 . . ? C28 C29 C24 120.0 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 2.161 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.118