# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address M.Ventura ;Departamento de Qu\'imica Inorg\'anica Universidad de Alcal\'a Campus Universitario 28871 Alcal\'a de Henares Spain ; 'C.Ramirez de Arellano' ;Departamento de Qu\'imica Org\'anica Universidad de Valencia 46100 Valencia Spain ; M.E.G.Mosquera ;Departamento de Qu\'imica Inorg\'anica Universidad de Alcal\'a Campus Universitario 28871 Alcal\'a de Henares Spain ; G.Jimenez ;Departamento de Qu\'imica Inorg\'anica Universidad de Alcal\'a Campus Universitario 28871 Alcal\'a de Henares Spain ; ; T.Cuenca ; ;Departamento de Qu\'imica Inorg\'anica Universidad de Alcal\'a Campus Universitario 28871 Alcal\'a de Henares Spain ; _publ_contact_author_address ;Departamento de Qu\'imica Org\'anica Universidad de Valencia 46100 Valencia Spain ; _publ_contact_author_email carmen.ramirezdearellano@uv.es _publ_contact_author_fax '+34 963544939' _publ_contact_author_phone '+34 963543046' #TrackingRef 'Compunds1&5_obm01global.cif' _publ_contact_author_name 'Carmen Ramirez de Arellano' _publ_section_title ; Synthesis and Structural Characterization of Novel Tetranuclear Organotitanoxanes ; #TrackingRef 'Compunds1&5_obm01global.cif' #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Marta E. G. Mosquera Departamento de Qu\'imica Inorg\'anica Facultad de Farmacia Universidad de Alcal\'a Campus Universitario 28871 Alcal\'a de Henares Spain ; _publ_contact_letter ; Alcal\'a 25/01/2010 Please receive the CIF for compound 5 submitted to be published in Inorg. Chem. Thank you very much. Dr. Marta E. G. Mosquera. ; data_comp1_obm01 _database_code_depnum_ccdc_archive 'CCDC 795475' loop_ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H36 Cl2 O3 Si2 Ti2' _chemical_formula_weight 571.39 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' O O 0.0106 0.0060 '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' Cl Cl 0.1484 0.1585 '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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.842(3) _cell_length_b 14.871(4) _cell_length_c 16.541(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2666.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9102 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 29.00 _exptl_crystal_description lath _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.910 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.825 _exptl_absorpt_correction_T_max 0.956 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38708 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 29.05 _reflns_number_total 6749 _reflns_number_gt 6676 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL v6.14 (Bruker 2000-2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0387P)^2^+2.0249P] 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 0.05(2) _refine_ls_number_reflns 6749 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.244 _refine_ls_restrained_S_all 1.244 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 1.02329(4) 0.49198(3) 0.89933(3) 0.00962(9) Uani 1 1 d . . . Ti2 Ti 0.91819(4) 0.58353(3) 1.06747(3) 0.00979(10) Uani 1 1 d . . . Cl1 Cl 1.07347(6) 0.57184(4) 0.78484(4) 0.01577(13) Uani 1 1 d . . . Cl2 Cl 1.03135(6) 0.66211(5) 1.16135(4) 0.01888(14) Uani 1 1 d . . . Si1 Si 0.99728(6) 0.37074(5) 1.08672(4) 0.01121(14) Uani 1 1 d . . . Si2 Si 0.72163(6) 0.50104(5) 0.90785(4) 0.01244(14) Uani 1 1 d . . . O1 O 0.92773(18) 0.46801(12) 1.10231(11) 0.0141(4) Uani 1 1 d . . . O2 O 0.86156(17) 0.46635(13) 0.88326(11) 0.0140(4) Uani 1 1 d . . . O3 O 1.01692(16) 0.57751(12) 0.97777(10) 0.0110(3) Uani 1 1 d . . . C1 C 1.0802(2) 0.37690(17) 0.98647(15) 0.0116(5) Uani 1 1 d . . . C2 C 1.0515(2) 0.33330(17) 0.91096(16) 0.0143(5) Uani 1 1 d . . . C3 C 1.1361(3) 0.36278(18) 0.85203(16) 0.0154(5) Uani 1 1 d . . . C4 C 1.2229(2) 0.42144(18) 0.89009(15) 0.0138(5) Uani 1 1 d . . . C5 C 1.1908(2) 0.42947(17) 0.97263(15) 0.0128(5) Uani 1 1 d . . . C6 C 0.7362(2) 0.58122(18) 0.99542(15) 0.0127(5) Uani 1 1 d . . . C7 C 0.7837(2) 0.67166(18) 0.98884(16) 0.0133(5) Uani 1 1 d . . . C8 C 0.7815(2) 0.71207(17) 1.06549(16) 0.0133(5) Uani 1 1 d . . . C9 C 0.7308(2) 0.64904(18) 1.12177(16) 0.0140(5) Uani 1 1 d . . . C10 C 0.7012(2) 0.56971(18) 1.07897(15) 0.0134(5) Uani 1 1 d . . . C12 C 0.9496(3) 0.26671(18) 0.89628(17) 0.0166(5) Uani 1 1 d . . . H12A H 0.9546 0.2445 0.8406 0.025 Uiso 1 1 calc R . . H12B H 0.8697 0.2961 0.9047 0.025 Uiso 1 1 calc R . . H12C H 0.9580 0.2162 0.9339 0.025 Uiso 1 1 calc R . . C13 C 1.1418(3) 0.3343(2) 0.76421(17) 0.0215(6) Uani 1 1 d . . . H13A H 1.2265 0.3170 0.7505 0.032 Uiso 1 1 calc R . . H13B H 1.1160 0.3845 0.7298 0.032 Uiso 1 1 calc R . . H13C H 1.0867 0.2830 0.7555 0.032 Uiso 1 1 calc R . . C14 C 1.3318(3) 0.4622(2) 0.84672(18) 0.0197(6) Uani 1 1 d . . . H14A H 1.3728 0.5055 0.8823 0.030 Uiso 1 1 calc R . . H14B H 1.3032 0.4929 0.7977 0.030 Uiso 1 1 calc R . . H14C H 1.3900 0.4146 0.8319 0.030 Uiso 1 1 calc R . . C15 C 1.2609(3) 0.48097(19) 1.03548(17) 0.0166(5) Uani 1 1 d . . . H15A H 1.3062 0.4389 1.0701 0.025 Uiso 1 1 calc R . . H15B H 1.2032 0.5160 1.0685 0.025 Uiso 1 1 calc R . . H15C H 1.3193 0.5218 1.0090 0.025 Uiso 1 1 calc R . . C17 C 0.8286(3) 0.71693(18) 0.91249(16) 0.0167(5) Uani 1 1 d . . . H17A H 0.7599 0.7489 0.8868 0.025 Uiso 1 1 calc R . . H17B H 0.8608 0.6714 0.8752 0.025 Uiso 1 1 calc R . . H17C H 0.8941 0.7598 0.9259 0.025 Uiso 1 1 calc R . . C18 C 0.8190(3) 0.80643(19) 1.08532(18) 0.0214(6) Uani 1 1 d . . . H18A H 0.8906 0.8233 1.0525 0.032 Uiso 1 1 calc R . . H18B H 0.8406 0.8104 1.1428 0.032 Uiso 1 1 calc R . . H18C H 0.7505 0.8474 1.0737 0.032 Uiso 1 1 calc R . . C19 C 0.7101(3) 0.6688(2) 1.20964(17) 0.0214(6) Uani 1 1 d . . . H19A H 0.6671 0.6181 1.2349 0.032 Uiso 1 1 calc R . . H19B H 0.6599 0.7233 1.2150 0.032 Uiso 1 1 calc R . . H19C H 0.7897 0.6779 1.2364 0.032 Uiso 1 1 calc R . . C20 C 0.6428(3) 0.48776(19) 1.11663(17) 0.0196(6) Uani 1 1 d . . . H20A H 0.6503 0.4913 1.1756 0.029 Uiso 1 1 calc R . . H20B H 0.6849 0.4336 1.0971 0.029 Uiso 1 1 calc R . . H20C H 0.5555 0.4851 1.1016 0.029 Uiso 1 1 calc R . . C21 C 0.8784(3) 0.28087(18) 1.09067(19) 0.0193(5) Uani 1 1 d . . . H21A H 0.8369 0.2824 1.1433 0.029 Uiso 1 1 calc R . . H21B H 0.9179 0.2222 1.0832 0.029 Uiso 1 1 calc R . . H21C H 0.8178 0.2906 1.0476 0.029 Uiso 1 1 calc R . . C22 C 1.1084(3) 0.35061(19) 1.16997(16) 0.0185(6) Uani 1 1 d . . . H22A H 1.1546 0.4059 1.1809 0.028 Uiso 1 1 calc R . . H22B H 1.1658 0.3028 1.1543 0.028 Uiso 1 1 calc R . . H22C H 1.0636 0.3325 1.2188 0.028 Uiso 1 1 calc R . . C23 C 0.6275(3) 0.40016(19) 0.93328(18) 0.0195(6) Uani 1 1 d . . . H23A H 0.6119 0.3653 0.8841 0.029 Uiso 1 1 calc R . . H23B H 0.5488 0.4193 0.9568 0.029 Uiso 1 1 calc R . . H23C H 0.6722 0.3629 0.9723 0.029 Uiso 1 1 calc R . . C24 C 0.6510(3) 0.5591(2) 0.81999(17) 0.0205(6) Uani 1 1 d . . . H24A H 0.7129 0.5973 0.7938 0.031 Uiso 1 1 calc R . . H24B H 0.5820 0.5963 0.8385 0.031 Uiso 1 1 calc R . . H24C H 0.6210 0.5143 0.7812 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.00975(19) 0.00983(19) 0.00928(19) 0.00018(16) -0.00023(15) 0.00088(16) Ti2 0.0121(2) 0.00777(19) 0.0094(2) 0.00005(16) 0.00005(16) 0.00071(17) Cl1 0.0175(3) 0.0181(3) 0.0117(3) 0.0043(2) 0.0017(2) 0.0013(2) Cl2 0.0187(3) 0.0207(3) 0.0172(3) -0.0061(2) -0.0054(2) -0.0001(3) Si1 0.0131(3) 0.0095(3) 0.0110(3) 0.0021(2) 0.0000(2) 0.0007(2) Si2 0.0106(3) 0.0145(3) 0.0122(3) -0.0011(3) -0.0019(2) 0.0005(3) O1 0.0175(9) 0.0103(8) 0.0145(9) 0.0023(7) 0.0030(7) 0.0028(7) O2 0.0105(8) 0.0175(9) 0.0142(9) -0.0035(7) -0.0013(7) -0.0002(7) O3 0.0123(8) 0.0083(8) 0.0126(8) -0.0008(7) 0.0014(7) -0.0010(7) C1 0.0115(11) 0.0086(10) 0.0146(11) 0.0010(9) -0.0001(10) 0.0024(10) C2 0.0172(12) 0.0106(11) 0.0152(12) -0.0007(10) -0.0033(10) 0.0037(9) C3 0.0159(12) 0.0140(12) 0.0163(13) -0.0013(10) -0.0002(10) 0.0084(10) C4 0.0124(11) 0.0139(11) 0.0153(12) 0.0037(10) 0.0020(9) 0.0051(10) C5 0.0119(11) 0.0117(12) 0.0147(12) 0.0014(9) -0.0017(9) 0.0031(10) C6 0.0100(11) 0.0125(11) 0.0155(12) 0.0030(10) -0.0012(9) 0.0006(9) C7 0.0121(11) 0.0133(12) 0.0145(12) 0.0017(10) -0.0010(9) 0.0047(9) C8 0.0145(12) 0.0104(11) 0.0149(12) -0.0005(10) 0.0008(10) 0.0058(9) C9 0.0126(11) 0.0165(13) 0.0129(12) -0.0017(10) 0.0014(9) 0.0036(10) C10 0.0111(11) 0.0175(12) 0.0115(11) 0.0004(9) -0.0003(9) 0.0019(10) C12 0.0205(13) 0.0138(12) 0.0153(12) -0.0031(10) -0.0038(10) -0.0015(10) C13 0.0241(15) 0.0251(15) 0.0153(13) -0.0051(11) -0.0004(11) 0.0040(12) C14 0.0144(12) 0.0202(14) 0.0246(14) 0.0036(11) 0.0030(11) 0.0044(11) C15 0.0142(12) 0.0166(13) 0.0190(13) 0.0020(10) -0.0056(10) -0.0003(10) C17 0.0201(13) 0.0157(12) 0.0143(12) 0.0022(10) 0.0023(10) 0.0023(10) C18 0.0283(15) 0.0141(13) 0.0217(14) -0.0029(11) 0.0003(12) 0.0039(11) C19 0.0237(14) 0.0242(15) 0.0162(13) -0.0047(11) 0.0067(11) 0.0018(12) C20 0.0190(13) 0.0198(13) 0.0199(13) 0.0001(11) 0.0039(10) -0.0049(11) C21 0.0184(13) 0.0138(12) 0.0256(14) 0.0024(11) 0.0032(11) -0.0018(10) C22 0.0231(14) 0.0200(14) 0.0126(12) 0.0030(10) -0.0019(10) 0.0041(11) C23 0.0153(12) 0.0202(13) 0.0230(14) -0.0032(11) -0.0017(11) -0.0021(11) C24 0.0193(14) 0.0256(15) 0.0165(13) -0.0013(11) -0.0082(10) 0.0027(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O2 1.814(2) . ? Ti1 O3 1.8182(18) . ? Ti1 Cl1 2.3005(9) . ? Ti1 C1 2.321(3) . ? Ti1 C5 2.373(3) . ? Ti1 C2 2.387(3) . ? Ti1 C3 2.408(3) . ? Ti1 C4 2.410(3) . ? Ti1 Ti2 3.2995(9) . ? Ti2 O1 1.8150(19) . ? Ti2 O3 1.8318(18) . ? Ti2 Cl2 2.2983(9) . ? Ti2 C6 2.306(3) . ? Ti2 C7 2.353(3) . ? Ti2 C10 2.369(3) . ? Ti2 C8 2.419(3) . ? Ti2 C9 2.426(3) . ? Si1 O1 1.6515(19) . ? Si1 C22 1.854(3) . ? Si1 C21 1.858(3) . ? Si1 C1 1.888(3) . ? Si2 O2 1.653(2) . ? Si2 C24 1.855(3) . ? Si2 C23 1.863(3) . ? Si2 C6 1.883(3) . ? C1 C2 1.441(4) . ? C1 C5 1.449(4) . ? C2 C3 1.409(4) . ? C2 C12 1.503(4) . ? C3 C4 1.429(4) . ? C3 C13 1.514(4) . ? C4 C5 1.414(4) . ? C4 C14 1.508(4) . ? C5 C15 1.499(4) . ? C6 C10 1.443(4) . ? C6 C7 1.444(4) . ? C7 C8 1.403(4) . ? C7 C17 1.512(4) . ? C8 C9 1.431(4) . ? C8 C18 1.497(4) . ? C9 C10 1.413(4) . ? C9 C19 1.500(4) . ? C10 C20 1.508(4) . ? 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 O2 Ti1 O3 102.41(8) . . ? O2 Ti1 Cl1 102.50(7) . . ? O3 Ti1 Cl1 103.61(6) . . ? O2 Ti1 C1 101.13(9) . . ? O3 Ti1 C1 94.75(9) . . ? Cl1 Ti1 C1 145.99(7) . . ? O2 Ti1 C5 137.07(9) . . ? O3 Ti1 C5 86.48(9) . . ? Cl1 Ti1 C5 116.21(7) . . ? C1 Ti1 C5 35.95(9) . . ? O2 Ti1 C2 85.86(9) . . ? O3 Ti1 C2 129.70(9) . . ? Cl1 Ti1 C2 123.12(7) . . ? C1 Ti1 C2 35.62(9) . . ? C5 Ti1 C2 58.24(9) . . ? O2 Ti1 C3 106.00(9) . . ? O3 Ti1 C3 144.02(9) . . ? Cl1 Ti1 C3 91.40(7) . . ? C1 Ti1 C3 58.56(9) . . ? C5 Ti1 C3 57.65(9) . . ? C2 Ti1 C3 34.16(9) . . ? O2 Ti1 C4 140.12(9) . . ? O3 Ti1 C4 112.57(9) . . ? Cl1 Ti1 C4 87.71(7) . . ? C1 Ti1 C4 58.64(9) . . ? C5 Ti1 C4 34.38(9) . . ? C2 Ti1 C4 57.31(9) . . ? C3 Ti1 C4 34.52(9) . . ? O2 Ti1 Ti2 82.90(6) . . ? O3 Ti1 Ti2 25.41(6) . . ? Cl1 Ti1 Ti2 124.23(3) . . ? C1 Ti1 Ti2 82.68(7) . . ? C5 Ti1 Ti2 89.73(7) . . ? C2 Ti1 Ti2 112.59(7) . . ? C3 Ti1 Ti2 141.12(7) . . ? C4 Ti1 Ti2 122.90(6) . . ? O1 Ti2 O3 100.23(8) . . ? O1 Ti2 Cl2 103.67(7) . . ? O3 Ti2 Cl2 105.08(6) . . ? O1 Ti2 C6 101.47(9) . . ? O3 Ti2 C6 94.63(9) . . ? Cl2 Ti2 C6 144.46(7) . . ? O1 Ti2 C7 137.57(9) . . ? O3 Ti2 C7 86.66(9) . . ? Cl2 Ti2 C7 114.91(7) . . ? C6 Ti2 C7 36.10(9) . . ? O1 Ti2 C10 87.08(9) . . ? O3 Ti2 C10 129.88(9) . . ? Cl2 Ti2 C10 121.33(7) . . ? C6 Ti2 C10 35.93(9) . . ? C7 Ti2 C10 58.48(9) . . ? O1 Ti2 C8 141.92(9) . . ? O3 Ti2 C8 112.69(9) . . ? Cl2 Ti2 C8 86.24(7) . . ? C6 Ti2 C8 58.69(9) . . ? C7 Ti2 C8 34.17(9) . . ? C10 Ti2 C8 57.40(9) . . ? O1 Ti2 C9 108.08(9) . . ? O3 Ti2 C9 144.01(9) . . ? Cl2 Ti2 C9 89.59(7) . . ? C6 Ti2 C9 58.70(9) . . ? C7 Ti2 C9 57.44(9) . . ? C10 Ti2 C9 34.25(9) . . ? C8 Ti2 C9 34.35(9) . . ? O1 Ti2 Ti1 81.80(6) . . ? O3 Ti2 Ti1 25.21(6) . . ? Cl2 Ti2 Ti1 126.51(3) . . ? C6 Ti2 Ti1 81.59(7) . . ? C7 Ti2 Ti1 88.74(7) . . ? C10 Ti2 Ti1 112.01(6) . . ? C8 Ti2 Ti1 121.75(7) . . ? C9 Ti2 Ti1 140.10(7) . . ? O1 Si1 C22 108.79(12) . . ? O1 Si1 C21 107.93(12) . . ? C22 Si1 C21 107.97(14) . . ? O1 Si1 C1 108.18(10) . . ? C22 Si1 C1 110.51(12) . . ? C21 Si1 C1 113.34(13) . . ? O2 Si2 C24 109.33(12) . . ? O2 Si2 C23 107.89(12) . . ? C24 Si2 C23 108.99(14) . . ? O2 Si2 C6 108.06(11) . . ? C24 Si2 C6 110.03(13) . . ? C23 Si2 C6 112.47(13) . . ? Si1 O1 Ti2 143.65(12) . . ? Si2 O2 Ti1 141.76(12) . . ? Ti1 O3 Ti2 129.37(10) . . ? C2 C1 C5 106.5(2) . . ? C2 C1 Si1 129.5(2) . . ? C5 C1 Si1 123.97(19) . . ? C2 C1 Ti1 74.69(14) . . ? C5 C1 Ti1 73.99(14) . . ? Si1 C1 Ti1 117.03(12) . . ? C3 C2 C1 108.6(2) . . ? C3 C2 C12 124.9(2) . . ? C1 C2 C12 126.5(2) . . ? C3 C2 Ti1 73.73(15) . . ? C1 C2 Ti1 69.69(14) . . ? C12 C2 Ti1 122.96(17) . . ? C2 C3 C4 108.3(2) . . ? C2 C3 C13 127.1(3) . . ? C4 C3 C13 124.5(3) . . ? C2 C3 Ti1 72.11(15) . . ? C4 C3 Ti1 72.81(15) . . ? C13 C3 Ti1 123.74(18) . . ? C5 C4 C3 108.3(2) . . ? C5 C4 C14 128.2(3) . . ? C3 C4 C14 123.4(2) . . ? C5 C4 Ti1 71.40(14) . . ? C3 C4 Ti1 72.67(14) . . ? C14 C4 Ti1 123.93(18) . . ? C4 C5 C1 108.1(2) . . ? C4 C5 C15 126.0(2) . . ? C1 C5 C15 125.9(2) . . ? C4 C5 Ti1 74.23(14) . . ? C1 C5 Ti1 70.07(14) . . ? C15 C5 Ti1 122.85(17) . . ? C10 C6 C7 106.0(2) . . ? C10 C6 Si2 129.8(2) . . ? C7 C6 Si2 124.17(19) . . ? C10 C6 Ti2 74.44(14) . . ? C7 C6 Ti2 73.73(14) . . ? Si2 C6 Ti2 118.61(12) . . ? C8 C7 C6 108.9(2) . . ? C8 C7 C17 124.7(2) . . ? C6 C7 C17 126.3(2) . . ? C8 C7 Ti2 75.50(15) . . ? C6 C7 Ti2 70.16(14) . . ? C17 C7 Ti2 120.68(18) . . ? C7 C8 C9 108.3(2) . . ? C7 C8 C18 126.5(2) . . ? C9 C8 C18 125.2(2) . . ? C7 C8 Ti2 70.33(14) . . ? C9 C8 Ti2 73.07(14) . . ? C18 C8 Ti2 124.81(19) . . ? C10 C9 C8 108.0(2) . . ? C10 C9 C19 128.0(3) . . ? C8 C9 C19 124.0(3) . . ? C10 C9 Ti2 70.69(15) . . ? C8 C9 Ti2 72.57(14) . . ? C19 C9 Ti2 124.27(19) . . ? C9 C10 C6 108.7(2) . . ? C9 C10 C20 124.3(2) . . ? C6 C10 C20 127.0(2) . . ? C9 C10 Ti2 75.06(15) . . ? C6 C10 Ti2 69.63(14) . . ? C20 C10 Ti2 121.33(18) . . ? 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 O2 Ti1 Ti2 O1 83.28(9) . . . . ? O3 Ti1 Ti2 O1 -136.66(15) . . . . ? Cl1 Ti1 Ti2 O1 -176.40(7) . . . . ? C1 Ti1 Ti2 O1 -18.97(9) . . . . ? C5 Ti1 Ti2 O1 -54.32(9) . . . . ? C2 Ti1 Ti2 O1 0.79(9) . . . . ? C3 Ti1 Ti2 O1 -23.45(13) . . . . ? C4 Ti1 Ti2 O1 -63.90(10) . . . . ? O2 Ti1 Ti2 O3 -140.06(15) . . . . ? Cl1 Ti1 Ti2 O3 -39.74(13) . . . . ? C1 Ti1 Ti2 O3 117.69(15) . . . . ? C5 Ti1 Ti2 O3 82.34(15) . . . . ? C2 Ti1 Ti2 O3 137.45(15) . . . . ? C3 Ti1 Ti2 O3 113.21(17) . . . . ? C4 Ti1 Ti2 O3 72.76(15) . . . . ? O2 Ti1 Ti2 Cl2 -175.74(7) . . . . ? O3 Ti1 Ti2 Cl2 -35.69(13) . . . . ? Cl1 Ti1 Ti2 Cl2 -75.43(4) . . . . ? C1 Ti1 Ti2 Cl2 82.01(7) . . . . ? C5 Ti1 Ti2 Cl2 46.65(7) . . . . ? C2 Ti1 Ti2 Cl2 101.77(7) . . . . ? C3 Ti1 Ti2 Cl2 77.52(12) . . . . ? C4 Ti1 Ti2 Cl2 37.08(9) . . . . ? O2 Ti1 Ti2 C6 -19.68(9) . . . . ? O3 Ti1 Ti2 C6 120.38(15) . . . . ? Cl1 Ti1 Ti2 C6 80.64(7) . . . . ? C1 Ti1 Ti2 C6 -121.93(9) . . . . ? C5 Ti1 Ti2 C6 -157.28(9) . . . . ? C2 Ti1 Ti2 C6 -102.17(10) . . . . ? C3 Ti1 Ti2 C6 -126.41(13) . . . . ? C4 Ti1 Ti2 C6 -166.86(11) . . . . ? O2 Ti1 Ti2 C7 -55.23(9) . . . . ? O3 Ti1 Ti2 C7 84.83(15) . . . . ? Cl1 Ti1 Ti2 C7 45.09(7) . . . . ? C1 Ti1 Ti2 C7 -157.48(9) . . . . ? C5 Ti1 Ti2 C7 167.17(9) . . . . ? C2 Ti1 Ti2 C7 -137.72(10) . . . . ? C3 Ti1 Ti2 C7 -161.96(13) . . . . ? C4 Ti1 Ti2 C7 157.59(10) . . . . ? O2 Ti1 Ti2 C10 -0.18(10) . . . . ? O3 Ti1 Ti2 C10 139.88(15) . . . . ? Cl1 Ti1 Ti2 C10 100.14(8) . . . . ? C1 Ti1 Ti2 C10 -102.43(10) . . . . ? C5 Ti1 Ti2 C10 -137.78(10) . . . . ? C2 Ti1 Ti2 C10 -82.67(10) . . . . ? C3 Ti1 Ti2 C10 -106.91(13) . . . . ? C4 Ti1 Ti2 C10 -147.36(11) . . . . ? O2 Ti1 Ti2 C8 -64.51(10) . . . . ? O3 Ti1 Ti2 C8 75.55(15) . . . . ? Cl1 Ti1 Ti2 C8 35.81(8) . . . . ? C1 Ti1 Ti2 C8 -166.76(10) . . . . ? C5 Ti1 Ti2 C8 157.89(10) . . . . ? C2 Ti1 Ti2 C8 -147.00(10) . . . . ? C3 Ti1 Ti2 C8 -171.24(13) . . . . ? C4 Ti1 Ti2 C8 148.31(11) . . . . ? O2 Ti1 Ti2 C9 -25.16(12) . . . . ? O3 Ti1 Ti2 C9 114.89(17) . . . . ? Cl1 Ti1 Ti2 C9 75.15(11) . . . . ? C1 Ti1 Ti2 C9 -127.42(13) . . . . ? C5 Ti1 Ti2 C9 -162.77(13) . . . . ? C2 Ti1 Ti2 C9 -107.65(13) . . . . ? C3 Ti1 Ti2 C9 -131.90(15) . . . . ? C4 Ti1 Ti2 C9 -172.35(13) . . . . ? C22 Si1 O1 Ti2 107.2(2) . . . . ? C21 Si1 O1 Ti2 -135.9(2) . . . . ? C1 Si1 O1 Ti2 -12.9(2) . . . . ? O3 Ti2 O1 Si1 6.7(2) . . . . ? Cl2 Ti2 O1 Si1 -101.7(2) . . . . ? C6 Ti2 O1 Si1 103.6(2) . . . . ? C7 Ti2 O1 Si1 103.0(2) . . . . ? C10 Ti2 O1 Si1 136.7(2) . . . . ? C8 Ti2 O1 Si1 156.71(17) . . . . ? C9 Ti2 O1 Si1 164.20(19) . . . . ? Ti1 Ti2 O1 Si1 24.00(19) . . . . ? C24 Si2 O2 Ti1 105.5(2) . . . . ? C23 Si2 O2 Ti1 -136.1(2) . . . . ? C6 Si2 O2 Ti1 -14.3(2) . . . . ? O3 Ti1 O2 Si2 8.8(2) . . . . ? Cl1 Ti1 O2 Si2 -98.41(19) . . . . ? C1 Ti1 O2 Si2 106.2(2) . . . . ? C5 Ti1 O2 Si2 107.1(2) . . . . ? C2 Ti1 O2 Si2 138.6(2) . . . . ? C3 Ti1 O2 Si2 166.45(19) . . . . ? C4 Ti1 O2 Si2 159.96(16) . . . . ? Ti2 Ti1 O2 Si2 25.16(19) . . . . ? O2 Ti1 O3 Ti2 40.72(15) . . . . ? Cl1 Ti1 O3 Ti2 147.06(11) . . . . ? C1 Ti1 O3 Ti2 -61.80(14) . . . . ? C5 Ti1 O3 Ti2 -96.81(14) . . . . ? C2 Ti1 O3 Ti2 -54.25(17) . . . . ? C3 Ti1 O3 Ti2 -100.85(18) . . . . ? C4 Ti1 O3 Ti2 -119.73(13) . . . . ? O1 Ti2 O3 Ti1 43.65(14) . . . . ? Cl2 Ti2 O3 Ti1 150.95(11) . . . . ? C6 Ti2 O3 Ti1 -58.90(14) . . . . ? C7 Ti2 O3 Ti1 -94.14(14) . . . . ? C10 Ti2 O3 Ti1 -51.12(18) . . . . ? C8 Ti2 O3 Ti1 -116.81(13) . . . . ? C9 Ti2 O3 Ti1 -98.07(18) . . . . ? O1 Si1 C1 C2 -108.5(2) . . . . ? C22 Si1 C1 C2 132.5(2) . . . . ? C21 Si1 C1 C2 11.2(3) . . . . ? O1 Si1 C1 C5 71.9(2) . . . . ? C22 Si1 C1 C5 -47.1(2) . . . . ? C21 Si1 C1 C5 -168.4(2) . . . . ? O1 Si1 C1 Ti1 -16.37(16) . . . . ? C22 Si1 C1 Ti1 -135.38(14) . . . . ? C21 Si1 C1 Ti1 103.27(15) . . . . ? O2 Ti1 C1 C2 66.35(16) . . . . ? O3 Ti1 C1 C2 170.00(15) . . . . ? Cl1 Ti1 C1 C2 -67.0(2) . . . . ? C5 Ti1 C1 C2 -112.7(2) . . . . ? C3 Ti1 C1 C2 -35.71(15) . . . . ? C4 Ti1 C1 C2 -76.39(16) . . . . ? Ti2 Ti1 C1 C2 147.59(15) . . . . ? O2 Ti1 C1 C5 179.03(14) . . . . ? O3 Ti1 C1 C5 -77.32(15) . . . . ? Cl1 Ti1 C1 C5 45.7(2) . . . . ? C2 Ti1 C1 C5 112.7(2) . . . . ? C3 Ti1 C1 C5 76.97(16) . . . . ? C4 Ti1 C1 C5 36.29(14) . . . . ? Ti2 Ti1 C1 C5 -99.73(14) . . . . ? O2 Ti1 C1 Si1 -60.56(14) . . . . ? O3 Ti1 C1 Si1 43.09(14) . . . . ? Cl1 Ti1 C1 Si1 166.12(6) . . . . ? C5 Ti1 C1 Si1 120.4(2) . . . . ? C2 Ti1 C1 Si1 -126.9(2) . . . . ? C3 Ti1 C1 Si1 -162.62(18) . . . . ? C4 Ti1 C1 Si1 156.70(18) . . . . ? Ti2 Ti1 C1 Si1 20.68(12) . . . . ? C5 C1 C2 C3 -3.8(3) . . . . ? Si1 C1 C2 C3 176.56(19) . . . . ? Ti1 C1 C2 C3 63.92(18) . . . . ? C5 C1 C2 C12 175.7(2) . . . . ? Si1 C1 C2 C12 -4.0(4) . . . . ? Ti1 C1 C2 C12 -116.6(3) . . . . ? C5 C1 C2 Ti1 -67.69(17) . . . . ? Si1 C1 C2 Ti1 112.6(2) . . . . ? O2 Ti1 C2 C3 126.79(16) . . . . ? O3 Ti1 C2 C3 -130.51(16) . . . . ? Cl1 Ti1 C2 C3 24.55(18) . . . . ? C1 Ti1 C2 C3 -117.5(2) . . . . ? C5 Ti1 C2 C3 -77.95(17) . . . . ? C4 Ti1 C2 C3 -37.07(15) . . . . ? Ti2 Ti1 C2 C3 -152.68(14) . . . . ? O2 Ti1 C2 C1 -115.69(15) . . . . ? O3 Ti1 C2 C1 -12.99(19) . . . . ? Cl1 Ti1 C2 C1 142.07(13) . . . . ? C5 Ti1 C2 C1 39.57(14) . . . . ? C3 Ti1 C2 C1 117.5(2) . . . . ? C4 Ti1 C2 C1 80.45(16) . . . . ? Ti2 Ti1 C2 C1 -35.16(16) . . . . ? O2 Ti1 C2 C12 5.4(2) . . . . ? O3 Ti1 C2 C12 108.1(2) . . . . ? Cl1 Ti1 C2 C12 -96.8(2) . . . . ? C1 Ti1 C2 C12 121.1(3) . . . . ? C5 Ti1 C2 C12 160.7(3) . . . . ? C3 Ti1 C2 C12 -121.4(3) . . . . ? C4 Ti1 C2 C12 -158.5(3) . . . . ? Ti2 Ti1 C2 C12 85.9(2) . . . . ? C1 C2 C3 C4 2.9(3) . . . . ? C12 C2 C3 C4 -176.6(2) . . . . ? Ti1 C2 C3 C4 64.28(18) . . . . ? C1 C2 C3 C13 179.5(3) . . . . ? C12 C2 C3 C13 0.0(4) . . . . ? Ti1 C2 C3 C13 -119.2(3) . . . . ? C1 C2 C3 Ti1 -61.34(18) . . . . ? C12 C2 C3 Ti1 119.2(2) . . . . ? O2 Ti1 C3 C2 -56.20(17) . . . . ? O3 Ti1 C3 C2 84.6(2) . . . . ? Cl1 Ti1 C3 C2 -159.63(15) . . . . ? C1 Ti1 C3 C2 37.25(15) . . . . ? C5 Ti1 C3 C2 79.87(17) . . . . ? C4 Ti1 C3 C2 116.5(2) . . . . ? Ti2 Ti1 C3 C2 42.5(2) . . . . ? O2 Ti1 C3 C4 -172.65(15) . . . . ? O3 Ti1 C3 C4 -31.8(2) . . . . ? Cl1 Ti1 C3 C4 83.92(14) . . . . ? C1 Ti1 C3 C4 -79.20(16) . . . . ? C5 Ti1 C3 C4 -36.58(15) . . . . ? C2 Ti1 C3 C4 -116.5(2) . . . . ? Ti2 Ti1 C3 C4 -73.98(18) . . . . ? O2 Ti1 C3 C13 67.0(2) . . . . ? O3 Ti1 C3 C13 -152.2(2) . . . . ? Cl1 Ti1 C3 C13 -36.4(2) . . . . ? C1 Ti1 C3 C13 160.4(3) . . . . ? C5 Ti1 C3 C13 -157.0(3) . . . . ? C2 Ti1 C3 C13 123.2(3) . . . . ? C4 Ti1 C3 C13 -120.4(3) . . . . ? Ti2 Ti1 C3 C13 165.65(18) . . . . ? C2 C3 C4 C5 -0.9(3) . . . . ? C13 C3 C4 C5 -177.6(2) . . . . ? Ti1 C3 C4 C5 62.91(18) . . . . ? C2 C3 C4 C14 176.5(2) . . . . ? C13 C3 C4 C14 -0.1(4) . . . . ? Ti1 C3 C4 C14 -119.7(2) . . . . ? C2 C3 C4 Ti1 -63.82(18) . . . . ? C13 C3 C4 Ti1 119.5(3) . . . . ? O2 Ti1 C4 C5 -105.86(18) . . . . ? O3 Ti1 C4 C5 43.49(18) . . . . ? Cl1 Ti1 C4 C5 147.28(16) . . . . ? C1 Ti1 C4 C5 -37.98(15) . . . . ? C2 Ti1 C4 C5 -80.24(17) . . . . ? C3 Ti1 C4 C5 -116.9(2) . . . . ? Ti2 Ti1 C4 C5 17.14(18) . . . . ? O2 Ti1 C4 C3 11.1(2) . . . . ? O3 Ti1 C4 C3 160.41(15) . . . . ? Cl1 Ti1 C4 C3 -95.80(15) . . . . ? C1 Ti1 C4 C3 78.94(17) . . . . ? C5 Ti1 C4 C3 116.9(2) . . . . ? C2 Ti1 C4 C3 36.68(15) . . . . ? Ti2 Ti1 C4 C3 134.06(13) . . . . ? O2 Ti1 C4 C14 130.1(2) . . . . ? O3 Ti1 C4 C14 -80.5(2) . . . . ? Cl1 Ti1 C4 C14 23.3(2) . . . . ? C1 Ti1 C4 C14 -162.0(3) . . . . ? C5 Ti1 C4 C14 -124.0(3) . . . . ? C2 Ti1 C4 C14 155.7(3) . . . . ? C3 Ti1 C4 C14 119.1(3) . . . . ? Ti2 Ti1 C4 C14 -106.9(2) . . . . ? C3 C4 C5 C1 -1.4(3) . . . . ? C14 C4 C5 C1 -178.7(3) . . . . ? Ti1 C4 C5 C1 62.28(17) . . . . ? C3 C4 C5 C15 176.8(2) . . . . ? C14 C4 C5 C15 -0.5(4) . . . . ? Ti1 C4 C5 C15 -119.4(3) . . . . ? C3 C4 C5 Ti1 -63.73(18) . . . . ? C14 C4 C5 Ti1 119.0(3) . . . . ? C2 C1 C5 C4 3.2(3) . . . . ? Si1 C1 C5 C4 -177.12(18) . . . . ? Ti1 C1 C5 C4 -64.99(18) . . . . ? C2 C1 C5 C15 -175.1(2) . . . . ? Si1 C1 C5 C15 4.6(4) . . . . ? Ti1 C1 C5 C15 116.7(2) . . . . ? C2 C1 C5 Ti1 68.18(17) . . . . ? Si1 C1 C5 Ti1 -112.13(18) . . . . ? O2 Ti1 C5 C4 115.08(18) . . . . ? O3 Ti1 C5 C4 -140.45(17) . . . . ? Cl1 Ti1 C5 C4 -37.02(17) . . . . ? C1 Ti1 C5 C4 116.5(2) . . . . ? C2 Ti1 C5 C4 77.28(17) . . . . ? C3 Ti1 C5 C4 36.74(16) . . . . ? Ti2 Ti1 C5 C4 -165.68(15) . . . . ? O2 Ti1 C5 C1 -1.4(2) . . . . ? O3 Ti1 C5 C1 103.07(15) . . . . ? Cl1 Ti1 C5 C1 -153.49(13) . . . . ? C2 Ti1 C5 C1 -39.19(14) . . . . ? C3 Ti1 C5 C1 -79.74(16) . . . . ? C4 Ti1 C5 C1 -116.5(2) . . . . ? Ti2 Ti1 C5 C1 77.85(14) . . . . ? O2 Ti1 C5 C15 -121.9(2) . . . . ? O3 Ti1 C5 C15 -17.4(2) . . . . ? Cl1 Ti1 C5 C15 86.0(2) . . . . ? C1 Ti1 C5 C15 -120.5(3) . . . . ? C2 Ti1 C5 C15 -159.7(2) . . . . ? C3 Ti1 C5 C15 159.8(3) . . . . ? C4 Ti1 C5 C15 123.0(3) . . . . ? Ti2 Ti1 C5 C15 -42.7(2) . . . . ? O2 Si2 C6 C10 -109.3(2) . . . . ? C24 Si2 C6 C10 131.4(2) . . . . ? C23 Si2 C6 C10 9.7(3) . . . . ? O2 Si2 C6 C7 73.1(2) . . . . ? C24 Si2 C6 C7 -46.3(2) . . . . ? C23 Si2 C6 C7 -168.0(2) . . . . ? O2 Si2 C6 Ti2 -16.06(16) . . . . ? C24 Si2 C6 Ti2 -135.37(14) . . . . ? C23 Si2 C6 Ti2 102.92(15) . . . . ? O1 Ti2 C6 C10 68.37(17) . . . . ? O3 Ti2 C6 C10 169.81(16) . . . . ? Cl2 Ti2 C6 C10 -66.0(2) . . . . ? C7 Ti2 C6 C10 -112.3(2) . . . . ? C8 Ti2 C6 C10 -76.38(17) . . . . ? C9 Ti2 C6 C10 -35.94(15) . . . . ? Ti1 Ti2 C6 C10 148.17(16) . . . . ? O1 Ti2 C6 C7 -179.29(15) . . . . ? O3 Ti2 C6 C7 -77.85(15) . . . . ? Cl2 Ti2 C6 C7 46.4(2) . . . . ? C10 Ti2 C6 C7 112.3(2) . . . . ? C8 Ti2 C6 C7 35.96(14) . . . . ? C9 Ti2 C6 C7 76.40(16) . . . . ? Ti1 Ti2 C6 C7 -99.49(14) . . . . ? O1 Ti2 C6 Si2 -58.81(15) . . . . ? O3 Ti2 C6 Si2 42.62(14) . . . . ? Cl2 Ti2 C6 Si2 166.85(7) . . . . ? C7 Ti2 C6 Si2 120.5(2) . . . . ? C10 Ti2 C6 Si2 -127.2(2) . . . . ? C8 Ti2 C6 Si2 156.43(18) . . . . ? C9 Ti2 C6 Si2 -163.13(18) . . . . ? Ti1 Ti2 C6 Si2 20.99(12) . . . . ? C10 C6 C7 C8 1.9(3) . . . . ? Si2 C6 C7 C8 -179.98(18) . . . . ? Ti2 C6 C7 C8 -66.10(19) . . . . ? C10 C6 C7 C17 -177.9(2) . . . . ? Si2 C6 C7 C17 0.2(4) . . . . ? Ti2 C6 C7 C17 114.1(3) . . . . ? C10 C6 C7 Ti2 68.00(17) . . . . ? Si2 C6 C7 Ti2 -113.88(19) . . . . ? O1 Ti2 C7 C8 117.76(17) . . . . ? O3 Ti2 C7 C8 -140.72(16) . . . . ? Cl2 Ti2 C7 C8 -35.64(17) . . . . ? C6 Ti2 C7 C8 116.7(2) . . . . ? C10 Ti2 C7 C8 77.17(17) . . . . ? C9 Ti2 C7 C8 36.54(15) . . . . ? Ti1 Ti2 C7 C8 -165.87(15) . . . . ? O1 Ti2 C7 C6 1.0(2) . . . . ? O3 Ti2 C7 C6 102.56(15) . . . . ? Cl2 Ti2 C7 C6 -152.36(13) . . . . ? C10 Ti2 C7 C6 -39.55(15) . . . . ? C8 Ti2 C7 C6 -116.7(2) . . . . ? C9 Ti2 C7 C6 -80.18(16) . . . . ? Ti1 Ti2 C7 C6 77.41(14) . . . . ? O1 Ti2 C7 C17 -120.2(2) . . . . ? O3 Ti2 C7 C17 -18.7(2) . . . . ? Cl2 Ti2 C7 C17 86.4(2) . . . . ? C6 Ti2 C7 C17 -121.2(3) . . . . ? C10 Ti2 C7 C17 -160.8(2) . . . . ? C8 Ti2 C7 C17 122.0(3) . . . . ? C9 Ti2 C7 C17 158.6(2) . . . . ? Ti1 Ti2 C7 C17 -43.8(2) . . . . ? C6 C7 C8 C9 -1.0(3) . . . . ? C17 C7 C8 C9 178.8(2) . . . . ? Ti2 C7 C8 C9 -63.65(19) . . . . ? C6 C7 C8 C18 -178.0(2) . . . . ? C17 C7 C8 C18 1.8(4) . . . . ? Ti2 C7 C8 C18 119.3(3) . . . . ? C6 C7 C8 Ti2 62.66(17) . . . . ? C17 C7 C8 Ti2 -117.5(3) . . . . ? O1 Ti2 C8 C7 -104.51(19) . . . . ? O3 Ti2 C8 C7 43.24(18) . . . . ? Cl2 Ti2 C8 C7 148.02(15) . . . . ? C6 Ti2 C8 C7 -38.03(15) . . . . ? C10 Ti2 C8 C7 -80.64(17) . . . . ? C9 Ti2 C8 C7 -117.2(2) . . . . ? Ti1 Ti2 C8 C7 16.68(18) . . . . ? O1 Ti2 C8 C9 12.7(2) . . . . ? O3 Ti2 C8 C9 160.45(15) . . . . ? Cl2 Ti2 C8 C9 -94.77(15) . . . . ? C6 Ti2 C8 C9 79.18(17) . . . . ? C7 Ti2 C8 C9 117.2(2) . . . . ? C10 Ti2 C8 C9 36.57(15) . . . . ? Ti1 Ti2 C8 C9 133.89(14) . . . . ? O1 Ti2 C8 C18 134.1(2) . . . . ? O3 Ti2 C8 C18 -78.1(2) . . . . ? Cl2 Ti2 C8 C18 26.7(2) . . . . ? C6 Ti2 C8 C18 -159.4(3) . . . . ? C7 Ti2 C8 C18 -121.4(3) . . . . ? C10 Ti2 C8 C18 158.0(3) . . . . ? C9 Ti2 C8 C18 121.4(3) . . . . ? Ti1 Ti2 C8 C18 -104.7(2) . . . . ? C7 C8 C9 C10 -0.3(3) . . . . ? C18 C8 C9 C10 176.7(3) . . . . ? Ti2 C8 C9 C10 -62.23(18) . . . . ? C7 C8 C9 C19 -178.1(3) . . . . ? C18 C8 C9 C19 -1.0(4) . . . . ? Ti2 C8 C9 C19 120.0(3) . . . . ? C7 C8 C9 Ti2 61.89(18) . . . . ? C18 C8 C9 Ti2 -121.0(3) . . . . ? O1 Ti2 C9 C10 -54.91(17) . . . . ? O3 Ti2 C9 C10 85.2(2) . . . . ? Cl2 Ti2 C9 C10 -159.17(15) . . . . ? C6 Ti2 C9 C10 37.74(15) . . . . ? C7 Ti2 C9 C10 80.55(17) . . . . ? C8 Ti2 C9 C10 116.9(2) . . . . ? Ti1 Ti2 C9 C10 44.1(2) . . . . ? O1 Ti2 C9 C8 -171.80(15) . . . . ? O3 Ti2 C9 C8 -31.7(2) . . . . ? Cl2 Ti2 C9 C8 83.94(15) . . . . ? C6 Ti2 C9 C8 -79.15(17) . . . . ? C7 Ti2 C9 C8 -36.34(15) . . . . ? C10 Ti2 C9 C8 -116.9(2) . . . . ? Ti1 Ti2 C9 C8 -72.80(18) . . . . ? O1 Ti2 C9 C19 68.5(2) . . . . ? O3 Ti2 C9 C19 -151.4(2) . . . . ? Cl2 Ti2 C9 C19 -35.8(2) . . . . ? C6 Ti2 C9 C19 161.1(3) . . . . ? C7 Ti2 C9 C19 -156.1(3) . . . . ? C10 Ti2 C9 C19 123.4(3) . . . . ? C8 Ti2 C9 C19 -119.7(3) . . . . ? Ti1 Ti2 C9 C19 167.46(18) . . . . ? C8 C9 C10 C6 1.5(3) . . . . ? C19 C9 C10 C6 179.2(3) . . . . ? Ti2 C9 C10 C6 -61.90(17) . . . . ? C8 C9 C10 C20 -178.6(2) . . . . ? C19 C9 C10 C20 -0.9(4) . . . . ? Ti2 C9 C10 C20 118.0(3) . . . . ? C8 C9 C10 Ti2 63.44(18) . . . . ? C19 C9 C10 Ti2 -118.9(3) . . . . ? C7 C6 C10 C9 -2.1(3) . . . . ? Si2 C6 C10 C9 179.9(2) . . . . ? Ti2 C6 C10 C9 65.40(19) . . . . ? C7 C6 C10 C20 178.0(2) . . . . ? Si2 C6 C10 C20 0.0(4) . . . . ? Ti2 C6 C10 C20 -114.5(3) . . . . ? C7 C6 C10 Ti2 -67.50(17) . . . . ? Si2 C6 C10 Ti2 114.5(2) . . . . ? O1 Ti2 C10 C9 128.84(16) . . . . ? O3 Ti2 C10 C9 -130.26(16) . . . . ? Cl2 Ti2 C10 C9 24.61(17) . . . . ? C6 Ti2 C10 C9 -117.0(2) . . . . ? C7 Ti2 C10 C9 -77.23(17) . . . . ? C8 Ti2 C10 C9 -36.69(15) . . . . ? Ti1 Ti2 C10 C9 -151.22(14) . . . . ? O1 Ti2 C10 C6 -114.18(16) . . . . ? O3 Ti2 C10 C6 -13.3(2) . . . . ? Cl2 Ti2 C10 C6 141.58(14) . . . . ? C7 Ti2 C10 C6 39.74(15) . . . . ? C8 Ti2 C10 C6 80.29(17) . . . . ? C9 Ti2 C10 C6 117.0(2) . . . . ? Ti1 Ti2 C10 C6 -34.24(17) . . . . ? O1 Ti2 C10 C20 7.5(2) . . . . ? O3 Ti2 C10 C20 108.4(2) . . . . ? Cl2 Ti2 C10 C20 -96.7(2) . . . . ? C6 Ti2 C10 C20 121.7(3) . . . . ? C7 Ti2 C10 C20 161.4(2) . . . . ? C8 Ti2 C10 C20 -158.0(2) . . . . ? C9 Ti2 C10 C20 -121.3(3) . . . . ? Ti1 Ti2 C10 C20 87.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.650 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.093 #===END data_comp5 _database_code_depnum_ccdc_archive 'CCDC 795476' #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H72 O8 Si4 Ti4' _chemical_formula_weight 1032.98 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.606(2) _cell_length_b 12.609(3) _cell_length_c 17.202(4) _cell_angle_alpha 84.349(18) _cell_angle_beta 82.941(16) _cell_angle_gamma 84.089(17) _cell_volume 2689.0(10) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 84 _cell_measurement_theta_max 19.034 _cell_measurement_theta_min 3.786 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_coefficient_mu 0.706 _exptl_absorpt_correction_T_min 0.797 _exptl_absorpt_correction_T_max 0.880 _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23097 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.1444 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.54 _reflns_number_total 12236 _reflns_number_gt 7097 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1024P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.056(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12236 _refine_ls_number_parameters 542 _refine_ls_number_restraints 304 _refine_ls_R_factor_all 0.1263 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.2140 _refine_ls_wR_factor_gt 0.1846 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 0.995 _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 C1 C 0.5046(6) -0.1173(5) -0.1264(5) 0.064(2) Uani 1 1 d . . . H1A H 0.5602 -0.0944 -0.1659 0.097 Uiso 1 1 calc R . . H1B H 0.4838 -0.1847 -0.1380 0.097 Uiso 1 1 calc R . . H1C H 0.5307 -0.1251 -0.0759 0.097 Uiso 1 1 calc R . . C2 C 0.2771(7) -0.0607(5) -0.0473(3) 0.065(2) Uani 1 1 d . . . H2A H 0.2157 -0.0088 -0.0463 0.098 Uiso 1 1 calc R . . H2B H 0.3041 -0.0684 0.0030 0.098 Uiso 1 1 calc R . . H2C H 0.2568 -0.1283 -0.0588 0.098 Uiso 1 1 calc R . . C3 C 0.5456(4) 0.4963(5) -0.3908(3) 0.0431(13) Uani 1 1 d . . . H3A H 0.5076 0.4496 -0.4159 0.065 Uiso 1 1 calc R . . H3B H 0.6195 0.4684 -0.3914 0.065 Uiso 1 1 calc R . . H3C H 0.5414 0.5662 -0.4185 0.065 Uiso 1 1 calc R . . C4 C 0.5622(4) 0.5980(4) -0.2407(4) 0.0428(13) Uani 1 1 d . . . H4A H 0.5333 0.6043 -0.1869 0.064 Uiso 1 1 calc R . . H4B H 0.5574 0.6673 -0.2693 0.064 Uiso 1 1 calc R . . H4C H 0.6360 0.5696 -0.2429 0.064 Uiso 1 1 calc R . . C5 C -0.0646(7) 0.3692(7) -0.0334(4) 0.085(3) Uani 1 1 d . . . H5A H -0.0105 0.3108 -0.0264 0.128 Uiso 1 1 calc R . . H5B H -0.1344 0.3442 -0.0195 0.128 Uiso 1 1 calc R . . H5C H -0.0556 0.4240 -0.0004 0.128 Uiso 1 1 calc R . . C6 C -0.1587(5) 0.5388(7) -0.1484(6) 0.084(3) Uani 1 1 d . . . H6A H -0.1498 0.5914 -0.1135 0.127 Uiso 1 1 calc R . . H6B H -0.2278 0.5122 -0.1347 0.127 Uiso 1 1 calc R . . H6C H -0.1535 0.5709 -0.2016 0.127 Uiso 1 1 calc R . . C7 C 0.1160(5) 0.1056(5) -0.5448(3) 0.0438(13) Uani 1 1 d . . . H7A H 0.0875 0.0453 -0.5138 0.066 Uiso 1 1 calc R . . H7B H 0.1699 0.0808 -0.5850 0.066 Uiso 1 1 calc R . . H7C H 0.0592 0.1484 -0.5688 0.066 Uiso 1 1 calc R . . C8 C 0.2291(5) 0.3027(5) -0.5482(3) 0.0485(14) Uani 1 1 d . . . H8A H 0.2617 0.3489 -0.5188 0.073 Uiso 1 1 calc R . . H8B H 0.1706 0.3425 -0.5721 0.073 Uiso 1 1 calc R . . H8C H 0.2814 0.2750 -0.5883 0.073 Uiso 1 1 calc R . . C11 C 0.2872(4) 0.1020(4) -0.4319(3) 0.0271(9) Uani 1 1 d U . . C12 C 0.2770(4) -0.0081(4) -0.3981(3) 0.0284(10) Uani 1 1 d U . . C13 C 0.3770(4) -0.0542(4) -0.3763(3) 0.0342(11) Uani 1 1 d U . . C14 C 0.4530(4) 0.0250(4) -0.3940(3) 0.0326(10) Uani 1 1 d U . . C15 C 0.3992(4) 0.1204(4) -0.4288(3) 0.0271(10) Uani 1 1 d U . . C16 C 0.1751(5) -0.0665(5) -0.3877(3) 0.0455(14) Uani 1 1 d U . . H16A H 0.1172 -0.0195 -0.4066 0.068 Uiso 1 1 calc R . . H16B H 0.1571 -0.0883 -0.3330 0.068 Uiso 1 1 calc R . . H16C H 0.1871 -0.1284 -0.4171 0.068 Uiso 1 1 calc R . . C17 C 0.3991(5) -0.1666(4) -0.3381(3) 0.0476(14) Uani 1 1 d U . . H17A H 0.4732 -0.1786 -0.3291 0.071 Uiso 1 1 calc R . . H17B H 0.3835 -0.2175 -0.3720 0.071 Uiso 1 1 calc R . . H17C H 0.3545 -0.1747 -0.2888 0.071 Uiso 1 1 calc R . . C18 C 0.5716(4) 0.0117(5) -0.3814(3) 0.0468(14) Uani 1 1 d U . . H18A H 0.6029 0.0776 -0.3983 0.070 Uiso 1 1 calc R . . H18B H 0.6081 -0.0442 -0.4114 0.070 Uiso 1 1 calc R . . H18C H 0.5784 -0.0066 -0.3266 0.070 Uiso 1 1 calc R . . C19 C 0.4525(4) 0.2208(4) -0.4544(3) 0.0379(12) Uani 1 1 d U . . H19A H 0.4018 0.2743 -0.4760 0.057 Uiso 1 1 calc R . . H19B H 0.5119 0.2062 -0.4936 0.057 Uiso 1 1 calc R . . H19C H 0.4780 0.2464 -0.4100 0.057 Uiso 1 1 calc R . . C21 C 0.4290(4) 0.1192(4) -0.1060(3) 0.0285(10) Uani 1 1 d U . . C22 C 0.3701(4) 0.1999(4) -0.0595(3) 0.0295(10) Uani 1 1 d U . . C23 C 0.4369(4) 0.2825(4) -0.0538(3) 0.0323(10) Uani 1 1 d U . . C24 C 0.5394(4) 0.2548(4) -0.0954(3) 0.0334(11) Uani 1 1 d U . . C25 C 0.5358(4) 0.1560(4) -0.1285(3) 0.0319(10) Uani 1 1 d U . . C26 C 0.2550(4) 0.2018(5) -0.0213(3) 0.0469(14) Uani 1 1 d U . . H26A H 0.2243 0.1392 -0.0325 0.070 Uiso 1 1 calc R . . H26B H 0.2142 0.2646 -0.0419 0.070 Uiso 1 1 calc R . . H26C H 0.2536 0.2029 0.0345 0.070 Uiso 1 1 calc R . . C27 C 0.4031(6) 0.3796(5) -0.0066(4) 0.0533(16) Uani 1 1 d U . . H27A H 0.4614 0.4239 -0.0111 0.080 Uiso 1 1 calc R . . H27B H 0.3846 0.3557 0.0477 0.080 Uiso 1 1 calc R . . H27C H 0.3421 0.4199 -0.0268 0.080 Uiso 1 1 calc R . . C28 C 0.6353(5) 0.3191(5) -0.1021(4) 0.0497(15) Uani 1 1 d U . . H28A H 0.6945 0.2840 -0.1333 0.075 Uiso 1 1 calc R . . H28B H 0.6549 0.3250 -0.0506 0.075 Uiso 1 1 calc R . . H28C H 0.6175 0.3893 -0.1267 0.075 Uiso 1 1 calc R . . C29 C 0.6284(5) 0.1051(5) -0.1798(3) 0.0496(15) Uani 1 1 d U . . H29A H 0.6091 0.0395 -0.1957 0.074 Uiso 1 1 calc R . . H29B H 0.6896 0.0904 -0.1510 0.074 Uiso 1 1 calc R . . H29C H 0.6457 0.1530 -0.2256 0.074 Uiso 1 1 calc R . . C31 C 0.3357(4) 0.5600(4) -0.2808(3) 0.0251(9) Uani 1 1 d U . . C32 C 0.2655(4) 0.5686(4) -0.3422(3) 0.0293(10) Uani 1 1 d U . . C33 C 0.1658(4) 0.6257(4) -0.3150(3) 0.0324(10) Uani 1 1 d U . . C34 C 0.1743(4) 0.6562(4) -0.2381(3) 0.0346(11) Uani 1 1 d U . . C35 C 0.2770(4) 0.6143(4) -0.2164(3) 0.0292(10) Uani 1 1 d U . . C36 C 0.0904(5) 0.7217(5) -0.1877(4) 0.0496(15) Uani 1 1 d U . . H36A H 0.0282 0.7405 -0.2150 0.074 Uiso 1 1 calc R . . H36B H 0.1191 0.7858 -0.1771 0.074 Uiso 1 1 calc R . . H36C H 0.0707 0.6806 -0.1390 0.074 Uiso 1 1 calc R . . C37 C 0.3153(5) 0.6271(5) -0.1372(3) 0.0450(14) Uani 1 1 d U . . H37A H 0.3867 0.5928 -0.1356 0.067 Uiso 1 1 calc R . . H37B H 0.2680 0.5947 -0.0956 0.067 Uiso 1 1 calc R . . H37C H 0.3152 0.7018 -0.1305 0.067 Uiso 1 1 calc R . . C38 C 0.2871(4) 0.5271(5) -0.4227(3) 0.0422(13) Uani 1 1 d U . . H38A H 0.3582 0.4913 -0.4292 0.063 Uiso 1 1 calc R . . H38B H 0.2810 0.5859 -0.4624 0.063 Uiso 1 1 calc R . . H38C H 0.2358 0.4777 -0.4278 0.063 Uiso 1 1 calc R . . C39 C 0.0719(4) 0.6516(5) -0.3619(4) 0.0482(14) Uani 1 1 d U . . H39A H 0.0145 0.6904 -0.3314 0.072 Uiso 1 1 calc R . . H39B H 0.0478 0.5864 -0.3749 0.072 Uiso 1 1 calc R . . H39C H 0.0933 0.6945 -0.4094 0.072 Uiso 1 1 calc R . . C41 C -0.0647(4) 0.3186(4) -0.2075(3) 0.0326(11) Uani 1 1 d U . . C42 C -0.1083(4) 0.3339(4) -0.2821(3) 0.0344(11) Uani 1 1 d U . . C43 C -0.1168(4) 0.2322(5) -0.3091(3) 0.0403(12) Uani 1 1 d U . . C44 C -0.0771(4) 0.1520(4) -0.2542(3) 0.0397(12) Uani 1 1 d U . . C45 C -0.0459(4) 0.2031(4) -0.1908(3) 0.0366(11) Uani 1 1 d U . . C46 C -0.0002(5) 0.1426(6) -0.1202(4) 0.0610(18) Uani 1 1 d U . . H46A H 0.0146 0.1925 -0.0851 0.092 Uiso 1 1 calc R . . H46B H 0.0650 0.1008 -0.1373 0.092 Uiso 1 1 calc R . . H46C H -0.0513 0.0961 -0.0934 0.092 Uiso 1 1 calc R . . C47 C -0.0725(5) 0.0333(5) -0.2586(5) 0.0627(19) Uani 1 1 d U . . H47A H -0.0417 -0.0031 -0.2138 0.094 Uiso 1 1 calc R . . H47B H -0.0291 0.0141 -0.3059 0.094 Uiso 1 1 calc R . . H47C H -0.1438 0.0129 -0.2589 0.094 Uiso 1 1 calc R . . C48 C -0.1609(5) 0.2117(6) -0.3859(4) 0.0597(18) Uani 1 1 d U . . H48A H -0.1831 0.2789 -0.4132 0.089 Uiso 1 1 calc R . . H48B H -0.2212 0.1700 -0.3733 0.089 Uiso 1 1 calc R . . H48C H -0.1058 0.1736 -0.4187 0.089 Uiso 1 1 calc R . . C49 C -0.1399(5) 0.4385(5) -0.3283(4) 0.0539(16) Uani 1 1 d U . . H49A H -0.1285 0.4972 -0.2996 0.081 Uiso 1 1 calc R . . H49B H -0.2143 0.4419 -0.3361 0.081 Uiso 1 1 calc R . . H49C H -0.0969 0.4428 -0.3784 0.081 Uiso 1 1 calc R . . O1 O 0.1715(2) 0.1485(3) -0.27258(18) 0.0289(7) Uani 1 1 d . . . O2 O 0.1396(3) 0.3800(3) -0.30131(19) 0.0321(8) Uani 1 1 d . . . O3 O 0.3917(3) 0.2004(3) -0.27199(18) 0.0290(7) Uani 1 1 d . . . O4 O 0.2801(2) 0.3642(3) -0.17697(19) 0.0304(7) Uani 1 1 d . . . O5 O 0.3368(3) -0.0068(3) -0.21105(19) 0.0321(8) Uani 1 1 d . . . O6 O 0.4965(2) 0.3855(3) -0.23904(19) 0.0298(7) Uani 1 1 d . . . O7 O 0.0649(3) 0.4753(3) -0.1596(2) 0.0343(8) Uani 1 1 d . . . O8 O 0.0853(3) 0.2358(3) -0.41314(19) 0.0337(8) Uani 1 1 d . . . Si1 Si 0.38492(12) -0.01442(11) -0.12567(8) 0.0347(3) Uani 1 1 d . . . Si2 Si 0.48330(10) 0.50540(11) -0.28574(8) 0.0269(3) Uani 1 1 d . . . Si3 Si -0.05127(11) 0.42564(13) -0.13949(9) 0.0394(4) Uani 1 1 d . . . Si4 Si 0.17721(11) 0.18835(11) -0.48004(7) 0.0282(3) Uani 1 1 d . . . Ti1 Ti 0.31250(6) 0.09440(7) -0.29480(5) 0.0240(2) Uani 1 1 d . . . Ti2 Ti 0.40881(6) 0.28161(7) -0.19160(5) 0.0237(2) Uani 1 1 d . . . Ti3 Ti 0.18829(6) 0.45896(7) -0.23045(5) 0.0247(2) Uani 1 1 d . . . Ti4 Ti 0.07359(6) 0.25632(7) -0.30575(5) 0.0260(2) 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 0.077(5) 0.026(3) 0.099(6) -0.010(3) -0.050(4) 0.008(3) C2 0.122(6) 0.044(4) 0.032(3) 0.005(3) -0.002(3) -0.039(4) C3 0.033(3) 0.060(4) 0.036(3) -0.001(3) 0.001(2) -0.009(3) C4 0.033(3) 0.033(3) 0.064(4) -0.008(3) -0.011(3) -0.002(2) C5 0.103(6) 0.115(7) 0.047(4) -0.036(4) 0.027(4) -0.071(6) C6 0.033(3) 0.084(6) 0.147(8) -0.078(6) -0.006(4) 0.001(3) C7 0.044(3) 0.047(3) 0.042(3) -0.012(3) -0.015(2) 0.004(3) C8 0.054(3) 0.048(3) 0.042(3) 0.013(3) -0.009(3) -0.007(3) C11 0.032(2) 0.029(2) 0.021(2) -0.0057(18) -0.0032(18) -0.0028(19) C12 0.038(2) 0.026(2) 0.023(2) -0.0071(19) -0.0048(19) -0.004(2) C13 0.045(3) 0.029(2) 0.028(2) -0.011(2) -0.001(2) 0.002(2) C14 0.032(2) 0.040(3) 0.025(2) -0.009(2) -0.0014(19) 0.006(2) C15 0.027(2) 0.032(2) 0.022(2) -0.0069(19) 0.0007(18) -0.0019(19) C16 0.056(3) 0.043(3) 0.044(3) -0.008(3) -0.009(3) -0.024(3) C17 0.075(4) 0.027(3) 0.041(3) -0.009(2) -0.014(3) 0.008(3) C18 0.033(3) 0.066(4) 0.042(3) -0.020(3) -0.006(2) 0.009(3) C19 0.043(3) 0.040(3) 0.031(3) -0.003(2) -0.001(2) -0.012(2) C21 0.035(2) 0.027(2) 0.023(2) 0.0035(19) -0.0093(19) -0.001(2) C22 0.038(2) 0.031(2) 0.018(2) 0.0056(19) -0.0051(19) 0.000(2) C23 0.043(3) 0.032(3) 0.023(2) -0.004(2) -0.012(2) -0.002(2) C24 0.040(3) 0.033(3) 0.029(2) 0.006(2) -0.016(2) -0.010(2) C25 0.035(2) 0.034(3) 0.027(2) 0.002(2) -0.0087(19) 0.002(2) C26 0.041(3) 0.056(4) 0.038(3) 0.004(3) 0.006(2) 0.003(3) C27 0.088(5) 0.031(3) 0.043(3) -0.006(2) -0.017(3) 0.001(3) C28 0.046(3) 0.052(4) 0.055(4) 0.017(3) -0.025(3) -0.019(3) C29 0.046(3) 0.052(4) 0.046(3) -0.002(3) -0.004(3) 0.019(3) C31 0.029(2) 0.020(2) 0.027(2) 0.0006(18) -0.0055(18) -0.0076(18) C32 0.032(2) 0.026(2) 0.029(2) 0.0057(19) -0.0037(19) -0.0098(19) C33 0.031(2) 0.028(3) 0.036(3) 0.006(2) -0.003(2) -0.003(2) C34 0.034(2) 0.025(2) 0.042(3) 0.003(2) 0.002(2) -0.004(2) C35 0.033(2) 0.022(2) 0.033(2) -0.003(2) -0.0009(19) -0.0072(19) C36 0.047(3) 0.039(3) 0.058(4) -0.012(3) 0.005(3) 0.006(3) C37 0.056(3) 0.048(3) 0.035(3) -0.011(3) -0.002(2) -0.018(3) C38 0.040(3) 0.056(4) 0.031(3) -0.006(2) -0.003(2) -0.009(3) C39 0.033(3) 0.045(3) 0.064(4) 0.009(3) -0.011(3) 0.001(2) C41 0.017(2) 0.044(3) 0.037(3) -0.011(2) 0.0041(18) -0.003(2) C42 0.019(2) 0.041(3) 0.044(3) -0.010(2) -0.001(2) -0.001(2) C43 0.027(2) 0.052(3) 0.045(3) -0.015(2) -0.001(2) -0.008(2) C44 0.028(2) 0.039(3) 0.052(3) -0.011(2) 0.008(2) -0.010(2) C45 0.025(2) 0.044(3) 0.038(3) 0.000(2) 0.005(2) -0.007(2) C46 0.051(4) 0.081(5) 0.041(3) 0.012(3) 0.010(3) 0.009(3) C47 0.051(4) 0.038(3) 0.096(5) -0.013(3) 0.016(4) -0.015(3) C48 0.040(3) 0.086(5) 0.060(4) -0.027(4) -0.011(3) -0.013(3) C49 0.040(3) 0.047(3) 0.069(4) 0.000(3) -0.004(3) 0.012(3) O1 0.0283(16) 0.0320(18) 0.0261(16) -0.0032(14) -0.0034(13) -0.0013(14) O2 0.0283(17) 0.0333(19) 0.0349(18) -0.0063(15) -0.0008(14) -0.0045(14) O3 0.0340(17) 0.0289(18) 0.0250(16) -0.0021(14) -0.0059(14) -0.0054(14) O4 0.0241(16) 0.0341(19) 0.0325(18) -0.0027(15) -0.0003(13) -0.0035(14) O5 0.0394(19) 0.0293(18) 0.0289(17) -0.0018(14) -0.0089(14) -0.0043(15) O6 0.0227(15) 0.0310(18) 0.0350(18) 0.0009(15) -0.0028(13) -0.0033(14) O7 0.0272(17) 0.037(2) 0.040(2) -0.0143(16) 0.0019(14) -0.0036(15) O8 0.0340(18) 0.037(2) 0.0300(18) -0.0041(15) -0.0075(14) 0.0010(15) Si1 0.0520(9) 0.0248(7) 0.0297(7) 0.0022(6) -0.0160(6) -0.0063(6) Si2 0.0248(6) 0.0260(7) 0.0295(7) 0.0005(5) -0.0018(5) -0.0056(5) Si3 0.0271(7) 0.0519(10) 0.0412(8) -0.0207(7) 0.0066(6) -0.0095(7) Si4 0.0314(7) 0.0297(7) 0.0242(6) -0.0015(5) -0.0067(5) -0.0021(6) Ti1 0.0261(4) 0.0235(4) 0.0227(4) -0.0028(3) -0.0038(3) -0.0010(3) Ti2 0.0246(4) 0.0221(4) 0.0248(4) -0.0006(3) -0.0050(3) -0.0024(3) Ti3 0.0218(4) 0.0231(4) 0.0288(4) -0.0025(3) -0.0018(3) -0.0019(3) Ti4 0.0221(4) 0.0289(5) 0.0274(4) -0.0051(4) -0.0027(3) -0.0022(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 Si1 1.885(6) . ? C2 Si1 1.887(6) . ? C3 Si2 1.890(5) . ? C4 Si2 1.887(5) . ? C5 Si3 1.886(8) . ? C6 Si3 1.872(8) . ? C7 Si4 1.880(5) . ? C8 Si4 1.885(6) . ? C11 C15 1.461(6) . ? C11 C12 1.464(7) . ? C11 Si4 1.895(5) . ? C11 Ti1 2.409(5) . ? C12 C13 1.410(7) . ? C12 C16 1.528(7) . ? C12 Ti1 2.408(4) . ? C13 C14 1.439(7) . ? C13 C17 1.516(7) . ? C13 Ti1 2.462(5) . ? C14 C15 1.433(7) . ? C14 C18 1.528(7) . ? C14 Ti1 2.459(5) . ? C15 C19 1.498(7) . ? C15 Ti1 2.433(4) . ? C21 C22 1.444(7) . ? C21 C25 1.464(7) . ? C21 Si1 1.900(5) . ? C21 Ti2 2.412(5) . ? C22 C23 1.423(7) . ? C22 C26 1.517(7) . ? C22 Ti2 2.415(4) . ? C23 C24 1.426(7) . ? C23 C27 1.530(7) . ? C23 Ti2 2.441(5) . ? C24 C25 1.427(7) . ? C24 C28 1.511(7) . ? C24 Ti2 2.452(5) . ? C25 C29 1.503(7) . ? C25 Ti2 2.411(5) . ? C31 C32 1.448(7) . ? C31 C35 1.444(7) . ? C31 Si2 1.912(5) . ? C31 Ti3 2.387(4) . ? C32 C33 1.432(7) . ? C32 C38 1.513(7) . ? C32 Ti3 2.418(5) . ? C33 C34 1.433(7) . ? C33 C39 1.504(7) . ? C33 Ti3 2.448(5) . ? C34 C35 1.427(7) . ? C34 C36 1.513(7) . ? C34 Ti3 2.467(5) . ? C35 C37 1.529(7) . ? C35 Ti3 2.399(5) . ? C41 C42 1.446(7) . ? C41 C45 1.458(8) . ? C41 Si3 1.904(5) . ? C41 Ti4 2.402(5) . ? C42 C43 1.424(8) . ? C42 C49 1.514(8) . ? C42 Ti4 2.401(5) . ? C43 C44 1.410(8) . ? C43 C48 1.548(8) . ? C43 Ti4 2.458(5) . ? C44 C45 1.434(8) . ? C44 C47 1.501(8) . ? C44 Ti4 2.449(5) . ? C45 C46 1.511(8) . ? C45 Ti4 2.418(5) . ? O1 Ti4 1.837(3) . ? O1 Ti1 1.845(3) . ? O2 Ti3 1.845(3) . ? O2 Ti4 1.854(3) . ? O3 Ti1 1.847(3) . ? O3 Ti2 1.845(3) . ? O4 Ti3 1.836(3) . ? O4 Ti2 1.840(3) . ? O5 Si1 1.647(3) . ? O5 Ti1 1.861(3) . ? O6 Si2 1.643(4) . ? O6 Ti2 1.863(3) . ? O7 Si3 1.636(3) . ? O7 Ti3 1.862(3) . ? O8 Si4 1.640(4) . ? O8 Ti4 1.876(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 C11 C12 105.5(4) . . ? C15 C11 Si4 130.3(4) . . ? C12 C11 Si4 123.7(3) . . ? C15 C11 Ti1 73.3(3) . . ? C12 C11 Ti1 72.3(2) . . ? Si4 C11 Ti1 125.1(2) . . ? C13 C12 C11 109.5(4) . . ? C13 C12 C16 124.2(5) . . ? C11 C12 C16 126.3(5) . . ? C13 C12 Ti1 75.3(3) . . ? C11 C12 Ti1 72.3(2) . . ? C16 C12 Ti1 119.1(3) . . ? C12 C13 C14 108.3(4) . . ? C12 C13 C17 125.6(5) . . ? C14 C13 C17 126.1(5) . . ? C12 C13 Ti1 71.1(3) . . ? C14 C13 Ti1 72.9(3) . . ? C17 C13 Ti1 120.2(3) . . ? C13 C14 C15 108.1(4) . . ? C13 C14 C18 127.3(5) . . ? C15 C14 C18 124.5(5) . . ? C13 C14 Ti1 73.1(3) . . ? C15 C14 Ti1 72.0(3) . . ? C18 C14 Ti1 122.2(3) . . ? C14 C15 C11 108.6(4) . . ? C14 C15 C19 123.5(4) . . ? C11 C15 C19 127.9(5) . . ? C14 C15 Ti1 74.0(3) . . ? C11 C15 Ti1 71.5(2) . . ? C19 C15 Ti1 119.2(3) . . ? C22 C21 C25 105.5(4) . . ? C22 C21 Si1 128.1(4) . . ? C25 C21 Si1 126.1(4) . . ? C22 C21 Ti2 72.7(3) . . ? C25 C21 Ti2 72.3(3) . . ? Si1 C21 Ti2 124.5(2) . . ? C23 C22 C21 109.6(4) . . ? C23 C22 C26 122.8(5) . . ? C21 C22 C26 127.6(5) . . ? C23 C22 Ti2 74.0(3) . . ? C21 C22 Ti2 72.5(2) . . ? C26 C22 Ti2 119.9(3) . . ? C22 C23 C24 108.0(4) . . ? C22 C23 C27 124.4(5) . . ? C24 C23 C27 127.5(5) . . ? C22 C23 Ti2 72.0(3) . . ? C24 C23 Ti2 73.5(3) . . ? C27 C23 Ti2 122.9(4) . . ? C23 C24 C25 108.4(4) . . ? C23 C24 C28 125.4(5) . . ? C25 C24 C28 126.2(5) . . ? C23 C24 Ti2 72.6(3) . . ? C25 C24 Ti2 71.4(3) . . ? C28 C24 Ti2 122.3(3) . . ? C24 C25 C21 108.6(4) . . ? C24 C25 C29 123.1(5) . . ? C21 C25 C29 128.4(5) . . ? C24 C25 Ti2 74.5(3) . . ? C21 C25 Ti2 72.4(3) . . ? C29 C25 Ti2 117.7(3) . . ? C32 C31 C35 106.6(4) . . ? C32 C31 Si2 128.1(4) . . ? C35 C31 Si2 124.8(3) . . ? C32 C31 Ti3 73.6(2) . . ? C35 C31 Ti3 72.9(3) . . ? Si2 C31 Ti3 124.7(2) . . ? C33 C32 C31 108.5(4) . . ? C33 C32 C38 122.7(4) . . ? C31 C32 C38 128.7(5) . . ? C33 C32 Ti3 74.1(3) . . ? C31 C32 Ti3 71.3(2) . . ? C38 C32 Ti3 120.8(3) . . ? C32 C33 C34 108.0(4) . . ? C32 C33 C39 124.8(5) . . ? C34 C33 C39 127.2(5) . . ? C32 C33 Ti3 71.7(3) . . ? C34 C33 Ti3 73.8(3) . . ? C39 C33 Ti3 122.0(3) . . ? C35 C34 C33 108.1(4) . . ? C35 C34 C36 125.1(5) . . ? C33 C34 C36 126.9(5) . . ? C35 C34 Ti3 70.4(3) . . ? C33 C34 Ti3 72.3(3) . . ? C36 C34 Ti3 123.2(4) . . ? C34 C35 C31 108.8(4) . . ? C34 C35 C37 123.9(5) . . ? C31 C35 C37 127.3(4) . . ? C34 C35 Ti3 75.6(3) . . ? C31 C35 Ti3 72.0(2) . . ? C37 C35 Ti3 118.8(3) . . ? C42 C41 C45 105.4(4) . . ? C42 C41 Si3 127.2(4) . . ? C45 C41 Si3 127.1(4) . . ? C42 C41 Ti4 72.4(3) . . ? C45 C41 Ti4 73.0(3) . . ? Si3 C41 Ti4 124.8(2) . . ? C43 C42 C41 109.3(5) . . ? C43 C42 C49 122.8(5) . . ? C41 C42 C49 127.9(5) . . ? C43 C42 Ti4 75.2(3) . . ? C41 C42 Ti4 72.5(3) . . ? C49 C42 Ti4 118.0(3) . . ? C44 C43 C42 108.5(5) . . ? C44 C43 C48 125.2(5) . . ? C42 C43 C48 126.3(6) . . ? C44 C43 Ti4 72.9(3) . . ? C42 C43 Ti4 70.8(3) . . ? C48 C43 Ti4 121.8(4) . . ? C43 C44 C45 108.2(5) . . ? C43 C44 C47 126.5(6) . . ? C45 C44 C47 125.2(6) . . ? C43 C44 Ti4 73.7(3) . . ? C45 C44 Ti4 71.7(3) . . ? C47 C44 Ti4 122.6(4) . . ? C44 C45 C41 108.6(5) . . ? C44 C45 C46 123.6(5) . . ? C41 C45 C46 127.8(5) . . ? C44 C45 Ti4 74.0(3) . . ? C41 C45 Ti4 71.8(3) . . ? C46 C45 Ti4 119.7(4) . . ? Ti4 O1 Ti1 141.38(19) . . ? Ti3 O2 Ti4 141.2(2) . . ? Ti1 O3 Ti2 141.39(18) . . ? Ti3 O4 Ti2 141.65(19) . . ? Si1 O5 Ti1 138.8(2) . . ? Si2 O6 Ti2 138.3(2) . . ? Si3 O7 Ti3 138.7(2) . . ? Si4 O8 Ti4 137.4(2) . . ? O5 Si1 C1 109.0(3) . . ? O5 Si1 C2 107.7(3) . . ? C1 Si1 C2 108.7(4) . . ? O5 Si1 C21 111.28(19) . . ? C1 Si1 C21 108.7(3) . . ? C2 Si1 C21 111.4(3) . . ? O6 Si2 C4 109.2(2) . . ? O6 Si2 C3 108.2(2) . . ? C4 Si2 C3 106.9(3) . . ? O6 Si2 C31 110.90(18) . . ? C4 Si2 C31 110.1(2) . . ? C3 Si2 C31 111.4(2) . . ? O7 Si3 C6 107.8(3) . . ? O7 Si3 C41 111.31(19) . . ? C6 Si3 C41 111.4(3) . . ? O7 Si3 C5 108.3(3) . . ? C6 Si3 C5 106.9(4) . . ? C41 Si3 C5 111.0(3) . . ? O8 Si4 C8 109.3(2) . . ? O8 Si4 C7 110.3(2) . . ? C8 Si4 C7 104.8(3) . . ? O8 Si4 C11 110.43(19) . . ? C8 Si4 C11 112.9(2) . . ? C7 Si4 C11 108.9(2) . . ? O3 Ti1 O1 104.43(15) . . ? O3 Ti1 O5 99.89(15) . . ? O1 Ti1 O5 104.51(15) . . ? O3 Ti1 C12 143.83(15) . . ? O1 Ti1 C12 94.67(16) . . ? O5 Ti1 C12 104.70(16) . . ? O3 Ti1 C11 113.30(15) . . ? O1 Ti1 C11 89.55(15) . . ? O5 Ti1 C11 139.48(16) . . ? C12 Ti1 C11 35.39(16) . . ? O3 Ti1 C15 86.34(15) . . ? O1 Ti1 C15 118.92(15) . . ? O5 Ti1 C15 133.11(16) . . ? C12 Ti1 C15 57.50(16) . . ? C11 Ti1 C15 35.13(15) . . ? O3 Ti1 C14 93.79(16) . . ? O1 Ti1 C14 146.97(16) . . ? O5 Ti1 C14 99.05(17) . . ? C12 Ti1 C14 56.65(17) . . ? C11 Ti1 C14 57.73(16) . . ? C15 Ti1 C14 34.07(17) . . ? O3 Ti1 C13 126.63(16) . . ? O1 Ti1 C13 126.14(17) . . ? O5 Ti1 C13 84.31(16) . . ? C12 Ti1 C13 33.64(17) . . ? C11 Ti1 C13 57.60(17) . . ? C15 Ti1 C13 56.74(17) . . ? C14 Ti1 C13 34.01(17) . . ? O4 Ti2 O3 103.89(15) . . ? O4 Ti2 O6 99.89(15) . . ? O3 Ti2 O6 104.49(14) . . ? O4 Ti2 C21 116.66(16) . . ? O3 Ti2 C21 89.05(15) . . ? O6 Ti2 C21 136.77(15) . . ? O4 Ti2 C25 144.98(16) . . ? O3 Ti2 C25 97.12(16) . . ? O6 Ti2 C25 101.58(16) . . ? C21 Ti2 C25 35.35(16) . . ? O4 Ti2 C22 88.07(16) . . ? O3 Ti2 C22 116.29(16) . . ? O6 Ti2 C22 135.21(16) . . ? C21 Ti2 C22 34.82(16) . . ? C25 Ti2 C22 57.34(17) . . ? O4 Ti2 C23 91.90(16) . . ? O3 Ti2 C23 146.76(16) . . ? O6 Ti2 C23 101.26(16) . . ? C21 Ti2 C23 57.72(16) . . ? C25 Ti2 C23 56.94(17) . . ? C22 Ti2 C23 34.07(16) . . ? O4 Ti2 C24 123.54(17) . . ? O3 Ti2 C24 130.00(17) . . ? O6 Ti2 C24 83.59(15) . . ? C21 Ti2 C24 57.70(16) . . ? C25 Ti2 C24 34.12(17) . . ? C22 Ti2 C24 56.52(17) . . ? C23 Ti2 C24 33.88(17) . . ? O4 Ti3 O2 104.95(16) . . ? O4 Ti3 O7 104.18(15) . . ? O2 Ti3 O7 99.93(14) . . ? O4 Ti3 C31 89.24(15) . . ? O2 Ti3 C31 115.63(15) . . ? O7 Ti3 C31 137.35(16) . . ? O4 Ti3 C35 95.44(16) . . ? O2 Ti3 C35 144.74(16) . . ? O7 Ti3 C35 102.57(16) . . ? C31 Ti3 C35 35.11(16) . . ? O4 Ti3 C32 117.65(16) . . ? O2 Ti3 C32 87.38(16) . . ? O7 Ti3 C32 134.08(17) . . ? C31 Ti3 C32 35.07(16) . . ? C35 Ti3 C32 57.52(16) . . ? O4 Ti3 C33 146.97(15) . . ? O2 Ti3 C33 92.64(17) . . ? O7 Ti3 C33 99.90(17) . . ? C31 Ti3 C33 57.80(16) . . ? C35 Ti3 C33 57.03(17) . . ? C32 Ti3 C33 34.21(16) . . ? O4 Ti3 C34 127.80(17) . . ? O2 Ti3 C34 124.79(17) . . ? O7 Ti3 C34 83.51(16) . . ? C31 Ti3 C34 57.46(16) . . ? C35 Ti3 C34 34.06(17) . . ? C32 Ti3 C34 56.62(17) . . ? C33 Ti3 C34 33.90(17) . . ? O1 Ti4 O2 103.92(15) . . ? O1 Ti4 O8 100.20(15) . . ? O2 Ti4 O8 104.90(15) . . ? O1 Ti4 C42 144.31(17) . . ? O2 Ti4 C42 97.07(16) . . ? O8 Ti4 C42 101.87(17) . . ? O1 Ti4 C41 116.38(17) . . ? O2 Ti4 C41 88.56(16) . . ? O8 Ti4 C41 136.79(16) . . ? C42 Ti4 C41 35.05(18) . . ? O1 Ti4 C45 87.42(17) . . ? O2 Ti4 C45 115.97(17) . . ? O8 Ti4 C45 135.26(17) . . ? C42 Ti4 C45 57.29(19) . . ? C41 Ti4 C45 35.21(18) . . ? O1 Ti4 C44 91.82(17) . . ? O2 Ti4 C44 146.47(16) . . ? O8 Ti4 C44 101.07(17) . . ? C42 Ti4 C44 56.61(18) . . ? C41 Ti4 C44 57.92(17) . . ? C45 Ti4 C44 34.27(18) . . ? O1 Ti4 C43 123.19(18) . . ? O2 Ti4 C43 129.97(18) . . ? O8 Ti4 C43 83.89(17) . . ? C42 Ti4 C43 34.05(18) . . ? C41 Ti4 C43 57.57(17) . . ? C45 Ti4 C43 56.40(18) . . ? C44 Ti4 C43 33.4(2) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.658 _refine_diff_density_min -0.782 _refine_diff_density_rms 0.129