Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr P.C.McGowan' _publ_contact_author_address ; Department of Chemistry University of Leeds Leeds LS2 9JT UK ; _publ_contact_author_email P.C.McGowan@chemistry.leeds.ac.uk _publ_contact_author_phone '+44 (0)113 34 36404' _publ_section_title ; Functionalised Cyclopentadienyl Titanium Compounds as Potential Anticancer Drugs ; loop_ _publ_author_name _publ_author_address 'P. C. McGowan' ;Department of Chemistry University of Leeds Leeds, LS2 9JT, UK ; 'Olivia R. Allen' ;Department of Chemistry University of Leeds Leeds, LS2 9JT, UK ; 'Andrew L. Gott' '' 'John A. Hartley' '' 'Janet M. Hartley' '' ; R.J.Knox ; '' data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 649314' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H22 Br3 N Ti' _chemical_formula_weight 515.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/a _symmetry_space_group_name_Hall '-P 2yab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 13.1375(2) _cell_length_b 6.68350(10) _cell_length_c 21.3776(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.7930(10) _cell_angle_gamma 90.00 _cell_volume 1837.43(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 37748 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.865 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 6.983 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.119 _exptl_absorpt_correction_T_max 0.870 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV. See R.H. Blessing, Acta Cryst (1995), A51, 33-38. ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data since the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree range. The crystal temperature was held constant using an Oxford Cryosystems Cryostream 600 system. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe x-ray _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 ; Nonius KappaCCD area-detector diffractometer ; _diffrn_radiation_detector 'CCD plate' _diffrn_measurement_method ; phi and omega scans to fill the asymmetric unit ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28374 _diffrn_reflns_av_R_equivalents 0.1066 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3605 _reflns_number_gt 3129 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 2001)' _computing_publication_material ; local program ; _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^)+(0.0813P)^2^+3.9664P] 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_number_reflns 3605 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1385 _refine_ls_wR_factor_gt 0.1307 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Br1 Br 0.81641(4) 0.43644(7) 0.69417(3) 0.0389(2) Uani 1 1 d . . . Br2 Br 0.53902(4) 0.42059(7) 0.61115(3) 0.0414(2) Uani 1 1 d . . . Ti1 Ti 0.67565(6) 0.68130(11) 0.64920(3) 0.0251(2) Uani 1 1 d . . . C6 C 0.5765(4) 0.9190(7) 0.6895(2) 0.0333(11) Uani 1 1 d . . . H6 H 0.5305 0.9968 0.6589 0.040 Uiso 1 1 calc R . . C7 C 0.6837(4) 0.9612(7) 0.7154(2) 0.0368(11) Uani 1 1 d . . . H7 H 0.7212 1.0752 0.7062 0.044 Uiso 1 1 calc R . . C1 C 0.7724(5) 0.9098(9) 0.5993(3) 0.0462(13) Uani 1 1 d . . . H1 H 0.8191 0.9985 0.6257 0.055 Uiso 1 1 calc R . . C2 C 0.6659(5) 0.9452(8) 0.5737(3) 0.0458(14) Uani 1 1 d . . . H2 H 0.6290 1.0644 0.5787 0.055 Uiso 1 1 calc R . . C8 C 0.7236(4) 0.8045(7) 0.7569(2) 0.0318(10) Uani 1 1 d . . . H8 H 0.7935 0.7928 0.7797 0.038 Uiso 1 1 calc R . . C3 C 0.7055(6) 0.6368(9) 0.5433(3) 0.0569(18) Uani 1 1 d . . . H3 H 0.6992 0.5075 0.5244 0.068 Uiso 1 1 calc R . . C9 C 0.5526(4) 0.7399(7) 0.7180(2) 0.0290(9) Uani 1 1 d . . . H9 H 0.4861 0.6783 0.7106 0.035 Uiso 1 1 calc R . . C4 C 0.7960(5) 0.7218(9) 0.5790(3) 0.0488(14) Uani 1 1 d . . . H4 H 0.8628 0.6609 0.5879 0.059 Uiso 1 1 calc R . . C5 C 0.6249(5) 0.7790(10) 0.5404(2) 0.0528(15) Uani 1 1 d . . . H5 H 0.5546 0.7620 0.5191 0.063 Uiso 1 1 calc R . . C10 C 0.6422(4) 0.6657(7) 0.7593(2) 0.0284(9) Uani 1 1 d . . . Br3 Br 0.87496(4) 0.98417(9) 0.90888(2) 0.0431(2) Uani 1 1 d . . . C11 C 0.6496(4) 0.4905(7) 0.8034(2) 0.0293(9) Uani 1 1 d . . . H11 H 0.7130 0.4115 0.8001 0.035 Uiso 1 1 calc R . . N1 N 0.5790(3) 0.2552(6) 0.90292(18) 0.0309(8) Uani 1 1 d . . . H1A H 0.5195 0.3277 0.9055 0.037 Uiso 1 1 calc R . . C12 C 0.5555(4) 0.3518(7) 0.7892(2) 0.0321(10) Uani 1 1 d . . . H12A H 0.4921 0.4290 0.7915 0.038 Uiso 1 1 calc R . . H12B H 0.5476 0.2987 0.7452 0.038 Uiso 1 1 calc R . . C13 C 0.6613(4) 0.5658(7) 0.8728(2) 0.0323(10) Uani 1 1 d . . . H13A H 0.7237 0.6520 0.8837 0.039 Uiso 1 1 calc R . . H13B H 0.5999 0.6480 0.8762 0.039 Uiso 1 1 calc R . . C14 C 0.5662(4) 0.1786(7) 0.8360(2) 0.0345(10) Uani 1 1 d . . . H14A H 0.5035 0.0928 0.8257 0.041 Uiso 1 1 calc R . . H14B H 0.6273 0.0964 0.8321 0.041 Uiso 1 1 calc R . . C15 C 0.6711(4) 0.3950(8) 0.9202(2) 0.0360(11) Uani 1 1 d . . . H15A H 0.6745 0.4490 0.9637 0.043 Uiso 1 1 calc R . . H15B H 0.7361 0.3203 0.9201 0.043 Uiso 1 1 calc R . . C16 C 0.5880(5) 0.0886(8) 0.9498(3) 0.0429(12) Uani 1 1 d . . . H16A H 0.5963 0.1436 0.9930 0.051 Uiso 1 1 calc R . . H16B H 0.6486 0.0062 0.9470 0.051 Uiso 1 1 calc R . . H16C H 0.5250 0.0062 0.9403 0.051 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 Br1 0.0361(3) 0.0371(3) 0.0459(3) 0.0043(2) 0.0137(2) 0.00115(18) Br2 0.0428(3) 0.0380(3) 0.0434(4) -0.0055(2) 0.0089(2) -0.00427(19) Ti1 0.0292(4) 0.0247(4) 0.0234(4) -0.0012(3) 0.0100(3) -0.0008(3) C6 0.045(3) 0.027(2) 0.033(3) -0.0019(18) 0.019(2) 0.0032(18) C7 0.058(3) 0.026(2) 0.034(3) -0.0084(19) 0.027(2) -0.010(2) C1 0.056(4) 0.049(3) 0.038(3) 0.006(2) 0.022(3) -0.015(2) C2 0.070(4) 0.039(3) 0.036(3) 0.012(2) 0.030(3) 0.011(3) C8 0.041(3) 0.038(2) 0.020(2) -0.0061(18) 0.0131(19) -0.0086(19) C3 0.109(5) 0.041(3) 0.035(3) -0.009(2) 0.048(3) -0.008(3) C9 0.033(2) 0.030(2) 0.029(2) -0.0026(18) 0.0164(19) 0.0014(18) C4 0.052(3) 0.059(3) 0.045(3) 0.018(3) 0.032(3) 0.013(3) C5 0.049(3) 0.083(4) 0.022(3) 0.015(3) 0.000(2) -0.012(3) C10 0.035(2) 0.033(2) 0.021(2) -0.0058(17) 0.0130(18) -0.0039(18) Br3 0.0368(3) 0.0600(4) 0.0337(3) -0.0014(2) 0.0098(2) -0.0129(2) C11 0.033(2) 0.032(2) 0.025(2) -0.0001(18) 0.0106(19) 0.0002(18) N1 0.035(2) 0.0298(19) 0.031(2) 0.0028(16) 0.0157(16) -0.0011(15) C12 0.040(3) 0.031(2) 0.027(2) -0.0005(18) 0.011(2) -0.0077(19) C13 0.036(3) 0.036(2) 0.026(2) -0.0037(18) 0.010(2) -0.0109(19) C14 0.049(3) 0.030(2) 0.027(2) -0.0025(18) 0.013(2) -0.0027(19) C15 0.037(3) 0.044(3) 0.027(2) -0.002(2) 0.009(2) -0.009(2) C16 0.059(3) 0.041(3) 0.033(3) 0.008(2) 0.017(2) -0.004(2) _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 Br1 Ti1 2.5090(9) . ? Br2 Ti1 2.5145(9) . ? Ti1 C6 2.328(4) . ? Ti1 C7 2.335(5) . ? Ti1 C1 2.375(5) . ? Ti1 C5 2.376(5) . ? Ti1 C2 2.377(5) . ? Ti1 C3 2.394(5) . ? Ti1 C8 2.405(4) . ? Ti1 C4 2.408(5) . ? Ti1 C9 2.429(4) . ? Ti1 C10 2.483(4) . ? C6 C9 1.408(6) . ? C6 C7 1.432(8) . ? C6 H6 0.9500 . ? C7 C8 1.403(7) . ? C7 H7 0.9500 . ? C1 C4 1.386(8) . ? C1 C2 1.415(9) . ? C1 H1 0.9500 . ? C2 C5 1.369(9) . ? C2 H2 0.9500 . ? C8 C10 1.425(6) . ? C8 H8 0.9500 . ? C3 C4 1.396(10) . ? C3 C5 1.415(9) . ? C3 H3 0.9500 . ? C9 C10 1.408(7) . ? C9 H9 0.9500 . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C10 C11 1.494(6) . ? C11 C12 1.526(6) . ? C11 C13 1.546(6) . ? C11 H11 1.0000 . ? N1 C16 1.486(6) . ? N1 C14 1.497(6) . ? N1 C15 1.514(6) . ? N1 H1A 0.9300 . ? C12 C14 1.517(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C15 1.514(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 C6 Ti1 C7 35.76(19) . . ? C6 Ti1 C1 96.8(2) . . ? C7 Ti1 C1 78.15(19) . . ? C6 Ti1 C5 96.2(2) . . ? C7 Ti1 C5 110.0(2) . . ? C1 Ti1 C5 56.8(2) . . ? C6 Ti1 C2 77.79(18) . . ? C7 Ti1 C2 78.87(19) . . ? C1 Ti1 C2 34.6(2) . . ? C5 Ti1 C2 33.5(2) . . ? C6 Ti1 C3 130.3(2) . . ? C7 Ti1 C3 132.61(19) . . ? C1 Ti1 C3 56.6(2) . . ? C5 Ti1 C3 34.5(2) . . ? C2 Ti1 C3 56.38(19) . . ? C6 Ti1 C8 57.93(18) . . ? C7 Ti1 C8 34.40(18) . . ? C1 Ti1 C8 98.63(18) . . ? C5 Ti1 C8 144.0(2) . . ? C2 Ti1 C8 111.33(18) . . ? C3 Ti1 C8 152.4(2) . . ? C6 Ti1 C4 129.95(19) . . ? C7 Ti1 C4 109.5(2) . . ? C1 Ti1 C4 33.7(2) . . ? C5 Ti1 C4 56.5(2) . . ? C2 Ti1 C4 56.23(19) . . ? C3 Ti1 C4 33.8(2) . . ? C8 Ti1 C4 118.8(2) . . ? C6 Ti1 C9 34.34(16) . . ? C7 Ti1 C9 57.12(16) . . ? C1 Ti1 C9 130.66(18) . . ? C5 Ti1 C9 117.41(19) . . ? C2 Ti1 C9 109.98(17) . . ? C3 Ti1 C9 148.3(2) . . ? C8 Ti1 C9 56.05(16) . . ? C4 Ti1 C9 164.24(19) . . ? C6 Ti1 C10 57.13(16) . . ? C7 Ti1 C10 56.91(16) . . ? C1 Ti1 C10 131.85(18) . . ? C5 Ti1 C10 150.5(2) . . ? C2 Ti1 C10 132.82(17) . . ? C3 Ti1 C10 170.42(19) . . ? C8 Ti1 C10 33.85(15) . . ? C4 Ti1 C10 149.5(2) . . ? C9 Ti1 C10 33.30(16) . . ? C6 Ti1 Br1 136.68(13) . . ? C7 Ti1 Br1 110.59(15) . . ? C1 Ti1 Br1 99.86(16) . . ? C5 Ti1 Br1 126.26(17) . . ? C2 Ti1 Br1 132.64(15) . . ? C3 Ti1 Br1 91.77(18) . . ? C8 Ti1 Br1 80.10(12) . . ? C4 Ti1 Br1 77.62(14) . . ? C9 Ti1 Br1 113.74(11) . . ? C10 Ti1 Br1 82.47(11) . . ? C6 Ti1 Br2 100.16(13) . . ? C7 Ti1 Br2 133.80(13) . . ? C1 Ti1 Br2 135.46(15) . . ? C5 Ti1 Br2 80.50(15) . . ? C2 Ti1 Br2 111.01(17) . . ? C3 Ti1 Br2 81.49(17) . . ? C8 Ti1 Br2 125.24(11) . . ? C4 Ti1 Br2 113.12(17) . . ? C9 Ti1 Br2 77.78(11) . . ? C10 Ti1 Br2 91.40(11) . . ? Br1 Ti1 Br2 95.36(3) . . ? C9 C6 C7 106.8(4) . . ? C9 C6 Ti1 76.8(2) . . ? C7 C6 Ti1 72.4(3) . . ? C9 C6 H6 126.6 . . ? C7 C6 H6 126.6 . . ? Ti1 C6 H6 116.4 . . ? C8 C7 C6 108.0(4) . . ? C8 C7 Ti1 75.5(3) . . ? C6 C7 Ti1 71.8(3) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? Ti1 C7 H7 118.5 . . ? C4 C1 C2 107.3(5) . . ? C4 C1 Ti1 74.5(3) . . ? C2 C1 Ti1 72.8(3) . . ? C4 C1 H1 126.4 . . ? C2 C1 H1 126.4 . . ? Ti1 C1 H1 118.4 . . ? C5 C2 C1 108.6(5) . . ? C5 C2 Ti1 73.2(3) . . ? C1 C2 Ti1 72.6(3) . . ? C5 C2 H2 125.7 . . ? C1 C2 H2 125.7 . . ? Ti1 C2 H2 120.2 . . ? C7 C8 C10 108.8(4) . . ? C7 C8 Ti1 70.1(3) . . ? C10 C8 Ti1 76.1(2) . . ? C7 C8 H8 125.6 . . ? C10 C8 H8 125.6 . . ? Ti1 C8 H8 120.0 . . ? C4 C3 C5 107.3(5) . . ? C4 C3 Ti1 73.6(3) . . ? C5 C3 Ti1 72.1(3) . . ? C4 C3 H3 126.4 . . ? C5 C3 H3 126.4 . . ? Ti1 C3 H3 119.8 . . ? C6 C9 C10 109.8(4) . . ? C6 C9 Ti1 68.9(2) . . ? C10 C9 Ti1 75.4(2) . . ? C6 C9 H9 125.1 . . ? C10 C9 H9 125.1 . . ? Ti1 C9 H9 122.2 . . ? C1 C4 C3 108.7(5) . . ? C1 C4 Ti1 71.8(3) . . ? C3 C4 Ti1 72.6(3) . . ? C1 C4 H4 125.7 . . ? C3 C4 H4 125.7 . . ? Ti1 C4 H4 121.6 . . ? C2 C5 C3 108.1(5) . . ? C2 C5 Ti1 73.3(3) . . ? C3 C5 Ti1 73.4(3) . . ? C2 C5 H5 125.9 . . ? C3 C5 H5 125.9 . . ? Ti1 C5 H5 119.2 . . ? C9 C10 C8 106.6(4) . . ? C9 C10 C11 127.6(4) . . ? C8 C10 C11 125.4(4) . . ? C9 C10 Ti1 71.3(2) . . ? C8 C10 Ti1 70.1(2) . . ? C11 C10 Ti1 129.0(3) . . ? C10 C11 C12 113.9(4) . . ? C10 C11 C13 109.4(4) . . ? C12 C11 C13 107.8(4) . . ? C10 C11 H11 108.6 . . ? C12 C11 H11 108.6 . . ? C13 C11 H11 108.6 . . ? C16 N1 C14 111.5(4) . . ? C16 N1 C15 110.4(4) . . ? C14 N1 C15 111.9(3) . . ? C16 N1 H1A 107.6 . . ? C14 N1 H1A 107.6 . . ? C15 N1 H1A 107.6 . . ? C14 C12 C11 111.8(4) . . ? C14 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? C14 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C15 C13 C11 112.0(4) . . ? C15 C13 H13A 109.2 . . ? C11 C13 H13A 109.2 . . ? C15 C13 H13B 109.2 . . ? C11 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? N1 C14 C12 110.3(4) . . ? N1 C14 H14A 109.6 . . ? C12 C14 H14A 109.6 . . ? N1 C14 H14B 109.6 . . ? C12 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? C13 C15 N1 110.4(4) . . ? C13 C15 H15A 109.6 . . ? N1 C15 H15A 109.6 . . ? C13 C15 H15B 109.6 . . ? N1 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? N1 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.189 _refine_diff_density_min -0.948 _refine_diff_density_rms 0.141 # Attachment 'cmpd_6.CIF' data_compound_6 _database_code_depnum_ccdc_archive 'CCDC 649315' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H37 Cl2 N Si2 Ti' _chemical_formula_sum 'C22 H37 Cl2 N Si2 Ti' _chemical_formula_weight 490.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3621(2) _cell_length_b 14.6464(2) _cell_length_c 18.2020(4) _cell_angle_alpha 107.8770(10) _cell_angle_beta 94.8930(10) _cell_angle_gamma 102.2810(10) _cell_volume 2535.02(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 22426 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.652 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.693 _exptl_absorpt_correction_T_max 0.932 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV. See R.H. Blessing, Acta Cryst (1995), A51, 33-38. ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data since the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree range. The crystal temperature was held constant using an Oxford Cryosystems Cryostream 600 system. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe x-ray _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 ; Nonius KappaCCD area-detector diffractometer ; _diffrn_radiation_detector 'CCD plate' _diffrn_measurement_method ; phi and omega scans to fill the asymmetric unit ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 39825 _diffrn_reflns_av_R_equivalents 0.0651 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9936 _reflns_number_gt 6881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material 'local program' _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^)+(0.0378P)^2^+1.2994P] 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_number_reflns 9936 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1051 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 0.41608(4) 0.09332(3) 0.25903(2) 0.02146(11) Uani 1 1 d . . . Ti2 Ti 0.42737(4) -0.40860(3) 0.25510(2) 0.02197(11) Uani 1 1 d . . . Cl1 Cl 0.50810(6) 0.24997(4) 0.24730(4) 0.03085(15) Uani 1 1 d . . . Cl2 Cl 0.20767(6) 0.12548(4) 0.28425(4) 0.02951(15) Uani 1 1 d . . . Cl3 Cl 0.51749(7) -0.25251(4) 0.24157(4) 0.03438(16) Uani 1 1 d . . . Cl4 Cl 0.21300(6) -0.37974(5) 0.26807(4) 0.03374(16) Uani 1 1 d . . . Si1 Si 0.79158(7) 0.10000(5) 0.31304(4) 0.02702(17) Uani 1 1 d . . . Si2 Si 0.26070(7) -0.04348(5) 0.39087(4) 0.02624(17) Uani 1 1 d . . . Si3 Si 0.26131(7) -0.54196(5) 0.38757(4) 0.02700(17) Uani 1 1 d . . . Si4 Si 0.79889(7) -0.38976(5) 0.32115(4) 0.02958(17) Uani 1 1 d . . . N1 N 0.1138(2) 0.14565(15) -0.04360(12) 0.0317(5) Uani 1 1 d . . . N2 N 0.2524(2) -0.36101(16) -0.07696(13) 0.0337(5) Uani 1 1 d . . . C1 C 0.6167(2) 0.09609(17) 0.33629(14) 0.0232(5) Uani 1 1 d . . . C2 C 0.5158(2) 0.01067(17) 0.33353(14) 0.0234(5) Uani 1 1 d . . . H2 H 0.5203 -0.0560 0.3104 0.028 Uiso 1 1 calc R . . C3 C 0.4086(2) 0.03921(17) 0.36995(14) 0.0234(5) Uani 1 1 d . . . C4 C 0.4467(2) 0.14527(17) 0.39912(14) 0.0253(5) Uani 1 1 d . . . H4 H 0.3954 0.1864 0.4274 0.030 Uiso 1 1 calc R . . C5 C 0.5710(2) 0.17863(17) 0.37944(14) 0.0246(5) Uani 1 1 d . . . H5 H 0.6180 0.2462 0.3928 0.030 Uiso 1 1 calc R . . C6 C 0.9062(3) 0.1977(2) 0.39732(17) 0.0463(8) Uani 1 1 d . . . H6A H 0.9988 0.2026 0.3880 0.056 Uiso 1 1 calc R . . H6B H 0.8959 0.1807 0.4449 0.056 Uiso 1 1 calc R . . H6C H 0.8847 0.2613 0.4037 0.056 Uiso 1 1 calc R . . C7 C 0.8208(3) 0.1310(2) 0.22352(16) 0.0397(7) Uani 1 1 d . . . H7A H 0.9133 0.1319 0.2155 0.048 Uiso 1 1 calc R . . H7B H 0.8053 0.1963 0.2294 0.048 Uiso 1 1 calc R . . H7C H 0.7593 0.0810 0.1783 0.048 Uiso 1 1 calc R . . C8 C 0.8231(3) -0.0235(2) 0.3035(2) 0.0477(8) Uani 1 1 d . . . H8A H 0.9135 -0.0237 0.2916 0.057 Uiso 1 1 calc R . . H8B H 0.7574 -0.0750 0.2612 0.057 Uiso 1 1 calc R . . H8C H 0.8149 -0.0367 0.3528 0.057 Uiso 1 1 calc R . . C9 C 0.1756(3) 0.0375(2) 0.45895(18) 0.0442(7) Uani 1 1 d . . . H9A H 0.0978 -0.0035 0.4708 0.053 Uiso 1 1 calc R . . H9B H 0.1462 0.0822 0.4345 0.053 Uiso 1 1 calc R . . H9C H 0.2380 0.0766 0.5075 0.053 Uiso 1 1 calc R . . C10 C 0.3337(3) -0.11993(19) 0.43981(17) 0.0378(7) Uani 1 1 d . . . H10A H 0.2615 -0.1652 0.4523 0.045 Uiso 1 1 calc R . . H10B H 0.3937 -0.0764 0.4881 0.045 Uiso 1 1 calc R . . H10C H 0.3842 -0.1584 0.4047 0.045 Uiso 1 1 calc R . . C11 C 0.1411(3) -0.12730(19) 0.30170(16) 0.0359(6) Uani 1 1 d . . . H11A H 0.0670 -0.1679 0.3168 0.043 Uiso 1 1 calc R . . H11B H 0.1873 -0.1705 0.2672 0.043 Uiso 1 1 calc R . . H11C H 0.1059 -0.0876 0.2741 0.043 Uiso 1 1 calc R . . C12 C 0.4728(3) 0.04467(18) 0.12929(14) 0.0275(6) Uani 1 1 d . . . H12 H 0.5458 0.0856 0.1169 0.033 Uiso 1 1 calc R . . C13 C 0.4815(3) -0.02866(17) 0.16233(14) 0.0299(6) Uani 1 1 d . . . H13 H 0.5608 -0.0472 0.1750 0.036 Uiso 1 1 calc R . . C14 C 0.3513(3) -0.07066(17) 0.17361(14) 0.0299(6) Uani 1 1 d . . . H14 H 0.3278 -0.1208 0.1965 0.036 Uiso 1 1 calc R . . C15 C 0.2631(3) -0.02395(17) 0.14441(14) 0.0272(6) Uani 1 1 d . . . H15 H 0.1690 -0.0387 0.1433 0.033 Uiso 1 1 calc R . . C16 C 0.3367(2) 0.04793(17) 0.11723(14) 0.0247(5) Uani 1 1 d . . . C17 C 0.2849(2) 0.11273(18) 0.07779(14) 0.0264(6) Uani 1 1 d . . . H17 H 0.3396 0.1824 0.1044 0.032 Uiso 1 1 calc R . . C18 C 0.3037(3) 0.0826(2) -0.00775(15) 0.0388(7) Uani 1 1 d . . . H18A H 0.3996 0.0873 -0.0111 0.047 Uiso 1 1 calc R . . H18B H 0.2532 0.0129 -0.0352 0.047 Uiso 1 1 calc R . . C19 C 0.1387(3) 0.1123(2) 0.08151(16) 0.0363(7) Uani 1 1 d . . . H19A H 0.1267 0.1379 0.1369 0.044 Uiso 1 1 calc R . . H19B H 0.0828 0.0434 0.0585 0.044 Uiso 1 1 calc R . . C20 C 0.0928(3) 0.1760(2) 0.03741(16) 0.0398(7) Uani 1 1 d . . . H20A H -0.0035 0.1717 0.0389 0.048 Uiso 1 1 calc R . . H20B H 0.1425 0.2461 0.0640 0.048 Uiso 1 1 calc R . . C21 C 0.2546(3) 0.1494(2) -0.04730(18) 0.0440(7) Uani 1 1 d . . . H21A H 0.3085 0.2185 -0.0215 0.053 Uiso 1 1 calc R . . H21B H 0.2674 0.1285 -0.1027 0.053 Uiso 1 1 calc R . . C22 C 0.0709(3) 0.2096(2) -0.08291(17) 0.0411(7) Uani 1 1 d . . . H22A H 0.0858 0.1882 -0.1374 0.049 Uiso 1 1 calc R . . H22B H 0.1226 0.2782 -0.0562 0.049 Uiso 1 1 calc R . . H22C H -0.0245 0.2053 -0.0816 0.049 Uiso 1 1 calc R . . C23 C 0.6219(2) -0.39707(17) 0.34074(14) 0.0246(5) Uani 1 1 d . . . C24 C 0.5231(2) -0.48413(17) 0.33706(14) 0.0231(5) Uani 1 1 d . . . H24 H 0.5325 -0.5499 0.3166 0.028 Uiso 1 1 calc R . . C25 C 0.4102(2) -0.45884(17) 0.36798(14) 0.0228(5) Uani 1 1 d . . . C26 C 0.4418(2) -0.35231(17) 0.39503(14) 0.0264(6) Uani 1 1 d . . . H26 H 0.3856 -0.3129 0.4197 0.032 Uiso 1 1 calc R . . C27 C 0.5680(2) -0.31628(17) 0.37916(14) 0.0262(6) Uani 1 1 d . . . H27 H 0.6118 -0.2482 0.3920 0.031 Uiso 1 1 calc R . . C28 C 0.9069(3) -0.2834(2) 0.40301(17) 0.0477(8) Uani 1 1 d . . . H28A H 1.0006 -0.2764 0.3956 0.057 Uiso 1 1 calc R . . H28B H 0.8964 -0.2952 0.4526 0.057 Uiso 1 1 calc R . . H28C H 0.8807 -0.2226 0.4041 0.057 Uiso 1 1 calc R . . C29 C 0.8355(3) -0.5075(2) 0.3242(2) 0.0494(8) Uani 1 1 d . . . H29A H 0.9270 -0.5077 0.3143 0.059 Uiso 1 1 calc R . . H29B H 0.7722 -0.5637 0.2841 0.059 Uiso 1 1 calc R . . H29C H 0.8268 -0.5134 0.3759 0.059 Uiso 1 1 calc R . . C30 C 0.8304(3) -0.3698(2) 0.22762(16) 0.0395(7) Uani 1 1 d . . . H30A H 0.9243 -0.3671 0.2223 0.047 Uiso 1 1 calc R . . H30B H 0.8110 -0.3072 0.2274 0.047 Uiso 1 1 calc R . . H30C H 0.7725 -0.4246 0.1838 0.047 Uiso 1 1 calc R . . C31 C 0.3313(3) -0.61659(19) 0.43956(17) 0.0376(7) Uani 1 1 d . . . H31A H 0.2580 -0.6616 0.4514 0.045 Uiso 1 1 calc R . . H31B H 0.3891 -0.5722 0.4884 0.045 Uiso 1 1 calc R . . H31C H 0.3837 -0.6553 0.4062 0.045 Uiso 1 1 calc R . . C32 C 0.1738(3) -0.4593(2) 0.45272(17) 0.0429(7) Uani 1 1 d . . . H32A H 0.0951 -0.4996 0.4644 0.052 Uiso 1 1 calc R . . H32B H 0.1454 -0.4159 0.4265 0.052 Uiso 1 1 calc R . . H32C H 0.2347 -0.4189 0.5015 0.052 Uiso 1 1 calc R . . C33 C 0.1446(3) -0.62689(19) 0.29777(16) 0.0349(6) Uani 1 1 d . . . H33A H 0.0698 -0.6675 0.3124 0.042 Uiso 1 1 calc R . . H33B H 0.1922 -0.6700 0.2644 0.042 Uiso 1 1 calc R . . H33C H 0.1101 -0.5879 0.2692 0.042 Uiso 1 1 calc R . . C34 C 0.4993(2) -0.46116(18) 0.13010(14) 0.0262(6) Uani 1 1 d . . . H34 H 0.5736 -0.4203 0.1187 0.031 Uiso 1 1 calc R . . C35 C 0.5063(3) -0.53146(17) 0.16686(14) 0.0286(6) Uani 1 1 d . . . H35 H 0.5855 -0.5472 0.1839 0.034 Uiso 1 1 calc R . . C36 C 0.3747(3) -0.57490(17) 0.17413(14) 0.0277(6) Uani 1 1 d . . . H36 H 0.3494 -0.6241 0.1978 0.033 Uiso 1 1 calc R . . C37 C 0.2878(3) -0.53201(17) 0.13992(14) 0.0265(6) Uani 1 1 d . . . H37 H 0.1931 -0.5485 0.1358 0.032 Uiso 1 1 calc R . . C38 C 0.3638(2) -0.46054(17) 0.11268(14) 0.0242(5) Uani 1 1 d . . . C39 C 0.3095(2) -0.40020(18) 0.06952(14) 0.0263(6) Uani 1 1 d . . . H39 H 0.2736 -0.3501 0.1072 0.032 Uiso 1 1 calc R . . C40 C 0.1953(3) -0.4665(2) 0.00333(16) 0.0335(6) Uani 1 1 d . . . H40A H 0.2271 -0.5207 -0.0316 0.040 Uiso 1 1 calc R . . H40B H 0.1208 -0.4968 0.0258 0.040 Uiso 1 1 calc R . . C41 C 0.4173(3) -0.34530(19) 0.03471(15) 0.0319(6) Uani 1 1 d . . . H41A H 0.4863 -0.2962 0.0776 0.038 Uiso 1 1 calc R . . H41B H 0.4612 -0.3933 0.0020 0.038 Uiso 1 1 calc R . . C42 C 0.3594(3) -0.2926(2) -0.01465(16) 0.0382(7) Uani 1 1 d . . . H42A H 0.3238 -0.2399 0.0191 0.046 Uiso 1 1 calc R . . H42B H 0.4313 -0.2609 -0.0380 0.046 Uiso 1 1 calc R . . C43 C 0.1446(3) -0.4086(2) -0.04394(17) 0.0395(7) Uani 1 1 d . . . H43A H 0.0724 -0.4540 -0.0868 0.047 Uiso 1 1 calc R . . H43B H 0.1067 -0.3575 -0.0099 0.047 Uiso 1 1 calc R . . C44 C 0.2024(3) -0.3075(2) -0.12413(18) 0.0494(8) Uani 1 1 d . . . H44A H 0.2764 -0.2757 -0.1453 0.059 Uiso 1 1 calc R . . H44B H 0.1639 -0.2568 -0.0915 0.059 Uiso 1 1 calc R . . H44C H 0.1335 -0.3540 -0.1673 0.059 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 0.0226(2) 0.0196(2) 0.0218(2) 0.00657(18) 0.00292(19) 0.00540(18) Ti2 0.0234(2) 0.0193(2) 0.0225(3) 0.00666(18) 0.00169(19) 0.00541(18) Cl1 0.0391(4) 0.0233(3) 0.0290(4) 0.0110(3) 0.0018(3) 0.0036(3) Cl2 0.0283(3) 0.0338(3) 0.0284(4) 0.0094(3) 0.0045(3) 0.0133(3) Cl3 0.0481(4) 0.0225(3) 0.0297(4) 0.0102(3) 0.0018(3) 0.0026(3) Cl4 0.0299(4) 0.0395(4) 0.0350(4) 0.0118(3) 0.0043(3) 0.0169(3) Si1 0.0222(4) 0.0324(4) 0.0272(4) 0.0129(3) 0.0022(3) 0.0048(3) Si2 0.0247(4) 0.0273(4) 0.0294(4) 0.0131(3) 0.0063(3) 0.0061(3) Si3 0.0245(4) 0.0281(4) 0.0293(4) 0.0125(3) 0.0039(3) 0.0044(3) Si4 0.0224(4) 0.0361(4) 0.0271(4) 0.0101(3) 0.0007(3) 0.0029(3) N1 0.0344(13) 0.0330(12) 0.0262(12) 0.0095(10) -0.0011(10) 0.0083(10) N2 0.0334(13) 0.0470(14) 0.0301(13) 0.0222(11) 0.0086(11) 0.0144(11) C1 0.0240(13) 0.0247(13) 0.0220(13) 0.0113(10) 0.0018(11) 0.0042(10) C2 0.0264(13) 0.0222(12) 0.0224(13) 0.0081(10) 0.0019(11) 0.0080(10) C3 0.0243(13) 0.0255(13) 0.0220(13) 0.0097(10) 0.0022(11) 0.0073(10) C4 0.0282(14) 0.0247(13) 0.0217(14) 0.0056(10) 0.0003(11) 0.0082(11) C5 0.0271(14) 0.0222(13) 0.0221(14) 0.0077(10) -0.0014(11) 0.0023(10) C6 0.0268(16) 0.064(2) 0.0365(18) 0.0089(15) 0.0026(13) -0.0006(14) C7 0.0280(15) 0.0594(19) 0.0339(17) 0.0221(14) 0.0038(13) 0.0069(13) C8 0.0337(17) 0.0507(19) 0.070(2) 0.0302(17) 0.0139(16) 0.0170(14) C9 0.0416(18) 0.0439(17) 0.0505(19) 0.0160(14) 0.0210(15) 0.0122(14) C10 0.0385(17) 0.0369(16) 0.0430(18) 0.0233(13) 0.0045(14) 0.0062(13) C11 0.0305(15) 0.0345(15) 0.0414(17) 0.0170(13) 0.0014(13) 0.0006(12) C12 0.0295(14) 0.0306(14) 0.0211(14) 0.0060(11) 0.0051(11) 0.0085(11) C13 0.0350(15) 0.0284(14) 0.0233(14) 0.0011(11) 0.0036(12) 0.0131(12) C14 0.0389(16) 0.0202(13) 0.0247(14) 0.0016(11) 0.0029(12) 0.0047(11) C15 0.0260(14) 0.0228(13) 0.0269(14) 0.0023(11) 0.0019(11) 0.0040(11) C16 0.0276(14) 0.0253(13) 0.0174(13) 0.0022(10) 0.0015(11) 0.0072(11) C17 0.0258(14) 0.0281(13) 0.0223(14) 0.0065(11) -0.0005(11) 0.0049(11) C18 0.0415(17) 0.0563(18) 0.0288(16) 0.0187(14) 0.0120(13) 0.0249(14) C19 0.0331(16) 0.0527(18) 0.0288(16) 0.0166(13) 0.0053(12) 0.0178(13) C20 0.0367(17) 0.0509(18) 0.0367(17) 0.0156(14) 0.0048(13) 0.0204(14) C21 0.0440(18) 0.065(2) 0.0376(18) 0.0293(15) 0.0138(15) 0.0228(15) C22 0.0430(18) 0.0384(16) 0.0407(18) 0.0161(14) -0.0047(14) 0.0077(13) C23 0.0225(13) 0.0260(13) 0.0224(14) 0.0068(10) -0.0013(11) 0.0041(10) C24 0.0246(13) 0.0232(12) 0.0211(13) 0.0082(10) -0.0006(10) 0.0058(10) C25 0.0243(13) 0.0233(13) 0.0196(13) 0.0068(10) 0.0004(10) 0.0054(10) C26 0.0299(14) 0.0259(13) 0.0214(14) 0.0052(10) 0.0011(11) 0.0084(11) C27 0.0295(14) 0.0227(13) 0.0229(14) 0.0074(10) -0.0020(11) 0.0022(11) C28 0.0330(17) 0.061(2) 0.0340(18) 0.0074(15) 0.0023(14) -0.0060(14) C29 0.0304(17) 0.058(2) 0.067(2) 0.0266(17) 0.0064(16) 0.0167(14) C30 0.0241(15) 0.0566(19) 0.0329(17) 0.0138(14) 0.0024(13) 0.0025(13) C31 0.0370(16) 0.0341(15) 0.0408(17) 0.0182(13) 0.0005(13) 0.0011(12) C32 0.0368(17) 0.0476(18) 0.0460(19) 0.0141(14) 0.0177(14) 0.0119(14) C33 0.0283(15) 0.0344(15) 0.0405(17) 0.0158(13) 0.0021(13) 0.0014(12) C34 0.0257(14) 0.0308(14) 0.0197(13) 0.0052(11) 0.0040(11) 0.0068(11) C35 0.0304(15) 0.0265(14) 0.0238(14) 0.0009(11) -0.0007(11) 0.0101(11) C36 0.0350(15) 0.0214(13) 0.0215(14) 0.0035(10) -0.0035(11) 0.0047(11) C37 0.0269(14) 0.0245(13) 0.0241(14) 0.0047(11) -0.0004(11) 0.0047(11) C38 0.0267(14) 0.0245(13) 0.0196(13) 0.0052(10) 0.0032(11) 0.0061(10) C39 0.0293(14) 0.0298(14) 0.0218(14) 0.0101(11) 0.0053(11) 0.0091(11) C40 0.0256(14) 0.0445(16) 0.0334(16) 0.0202(13) 0.0024(12) 0.0051(12) C41 0.0318(15) 0.0348(15) 0.0278(15) 0.0139(12) 0.0015(12) 0.0019(12) C42 0.0500(18) 0.0358(16) 0.0325(17) 0.0177(13) 0.0101(14) 0.0079(13) C43 0.0308(16) 0.0600(19) 0.0374(17) 0.0269(15) 0.0064(13) 0.0156(14) C44 0.053(2) 0.073(2) 0.0436(19) 0.0377(17) 0.0165(16) 0.0290(17) _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 C14 2.341(2) . ? Ti1 C13 2.353(2) . ? Ti1 Cl2 2.3591(7) . ? Ti1 Cl1 2.3714(7) . ? Ti1 C2 2.382(2) . ? Ti1 C3 2.386(2) . ? Ti1 C1 2.394(2) . ? Ti1 C4 2.398(2) . ? Ti1 C5 2.410(2) . ? Ti1 C12 2.411(2) . ? Ti1 C15 2.428(2) . ? Ti1 C16 2.476(2) . ? Ti2 C36 2.344(2) . ? Ti2 C35 2.359(2) . ? Ti2 Cl4 2.3656(7) . ? Ti2 Cl3 2.3740(7) . ? Ti2 C24 2.380(2) . ? Ti2 C23 2.383(2) . ? Ti2 C25 2.394(2) . ? Ti2 C27 2.404(2) . ? Ti2 C34 2.405(2) . ? Ti2 C26 2.405(2) . ? Ti2 C37 2.408(2) . ? Ti2 C38 2.453(2) . ? Si1 C6 1.852(3) . ? Si1 C7 1.852(3) . ? Si1 C8 1.865(3) . ? Si1 C1 1.889(2) . ? Si2 C9 1.857(3) . ? Si2 C11 1.861(3) . ? Si2 C10 1.865(3) . ? Si2 C3 1.885(2) . ? Si3 C33 1.859(3) . ? Si3 C32 1.861(3) . ? Si3 C31 1.863(3) . ? Si3 C25 1.884(2) . ? Si4 C28 1.857(3) . ? Si4 C30 1.857(3) . ? Si4 C29 1.859(3) . ? Si4 C23 1.885(2) . ? N1 C20 1.453(3) . ? N1 C21 1.456(3) . ? N1 C22 1.456(3) . ? N2 C44 1.459(3) . ? N2 C42 1.461(3) . ? N2 C43 1.462(3) . ? C1 C5 1.424(3) . ? C1 C2 1.434(3) . ? C2 C3 1.415(3) . ? C2 H2 0.9500 . ? C3 C4 1.431(3) . ? C4 C5 1.394(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.397(3) . ? C12 C16 1.421(3) . ? C12 H12 0.9500 . ? C13 C14 1.419(3) . ? C13 H13 0.9500 . ? C14 C15 1.411(3) . ? C14 H14 0.9500 . ? C15 C16 1.406(3) . ? C15 H15 0.9500 . ? C16 C17 1.508(3) . ? C17 C19 1.521(3) . ? C17 C18 1.524(3) . ? C17 H17 1.0000 . ? C18 C21 1.522(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.525(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C27 1.428(3) . ? C23 C24 1.435(3) . ? C24 C25 1.412(3) . ? C24 H24 0.9500 . ? C25 C26 1.438(3) . ? C26 C27 1.392(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.400(3) . ? C34 C38 1.415(3) . ? C34 H34 0.9500 . ? C35 C36 1.413(3) . ? C35 H35 0.9500 . ? C36 C37 1.406(3) . ? C36 H36 0.9500 . ? C37 C38 1.413(3) . ? C37 H37 0.9500 . ? C38 C39 1.509(3) . ? C39 C40 1.532(3) . ? C39 C41 1.532(3) . ? C39 H39 1.0000 . ? C40 C43 1.515(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.514(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? 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 C14 Ti1 C13 35.18(9) . . ? C14 Ti1 Cl2 101.78(7) . . ? C13 Ti1 Cl2 133.86(7) . . ? C14 Ti1 Cl1 135.39(7) . . ? C13 Ti1 Cl1 108.47(7) . . ? Cl2 Ti1 Cl1 95.00(3) . . ? C14 Ti1 C2 78.65(9) . . ? C13 Ti1 C2 77.53(9) . . ? Cl2 Ti1 C2 118.20(6) . . ? Cl1 Ti1 C2 127.86(6) . . ? C14 Ti1 C3 91.24(9) . . ? C13 Ti1 C3 106.08(8) . . ? Cl2 Ti1 C3 84.29(6) . . ? Cl1 Ti1 C3 131.70(6) . . ? C2 Ti1 C3 34.53(8) . . ? C14 Ti1 C1 102.36(9) . . ? C13 Ti1 C1 83.17(9) . . ? Cl2 Ti1 C1 135.75(6) . . ? Cl1 Ti1 C1 93.15(6) . . ? C2 Ti1 C1 34.95(8) . . ? C3 Ti1 C1 58.74(8) . . ? C14 Ti1 C4 126.04(9) . . ? C13 Ti1 C4 133.89(9) . . ? Cl2 Ti1 C4 78.34(6) . . ? Cl1 Ti1 C4 97.61(6) . . ? C2 Ti1 C4 56.55(8) . . ? C3 Ti1 C4 34.81(8) . . ? C1 Ti1 C4 57.48(8) . . ? C14 Ti1 C5 134.27(9) . . ? C13 Ti1 C5 117.08(9) . . ? Cl2 Ti1 C5 106.45(6) . . ? Cl1 Ti1 C5 77.04(6) . . ? C2 Ti1 C5 56.45(8) . . ? C3 Ti1 C5 57.39(8) . . ? C1 Ti1 C5 34.48(8) . . ? C4 Ti1 C5 33.72(8) . . ? C14 Ti1 C12 57.30(9) . . ? C13 Ti1 C12 34.08(8) . . ? Cl2 Ti1 C12 122.92(6) . . ? Cl1 Ti1 C12 78.84(6) . . ? C2 Ti1 C12 108.96(8) . . ? C3 Ti1 C12 140.08(8) . . ? C1 Ti1 C12 101.32(8) . . ? C4 Ti1 C12 158.53(9) . . ? C5 Ti1 C12 126.29(8) . . ? C14 Ti1 C15 34.37(8) . . ? C13 Ti1 C15 56.88(9) . . ? Cl2 Ti1 C15 77.41(6) . . ? Cl1 Ti1 C15 114.50(6) . . ? C2 Ti1 C15 111.42(8) . . ? C3 Ti1 C15 112.39(8) . . ? C1 Ti1 C15 136.25(8) . . ? C4 Ti1 C15 141.00(8) . . ? C5 Ti1 C15 167.80(8) . . ? C12 Ti1 C15 55.94(9) . . ? C14 Ti1 C16 56.85(8) . . ? C13 Ti1 C16 56.60(8) . . ? Cl2 Ti1 C16 89.23(6) . . ? Cl1 Ti1 C16 82.69(6) . . ? C2 Ti1 C16 132.31(8) . . ? C3 Ti1 C16 145.36(8) . . ? C1 Ti1 C16 134.96(8) . . ? C4 Ti1 C16 167.56(8) . . ? C5 Ti1 C16 155.23(8) . . ? C12 Ti1 C16 33.78(8) . . ? C15 Ti1 C16 33.31(8) . . ? C36 Ti2 C35 34.97(8) . . ? C36 Ti2 Cl4 102.15(7) . . ? C35 Ti2 Cl4 133.82(7) . . ? C36 Ti2 Cl3 136.09(7) . . ? C35 Ti2 Cl3 109.38(7) . . ? Cl4 Ti2 Cl3 93.77(3) . . ? C36 Ti2 C24 78.11(8) . . ? C35 Ti2 C24 76.71(9) . . ? Cl4 Ti2 C24 119.63(6) . . ? Cl3 Ti2 C24 127.78(6) . . ? C36 Ti2 C23 102.17(8) . . ? C35 Ti2 C23 82.89(8) . . ? Cl4 Ti2 C23 136.64(6) . . ? Cl3 Ti2 C23 92.96(6) . . ? C24 Ti2 C23 35.06(8) . . ? C36 Ti2 C25 90.40(8) . . ? C35 Ti2 C25 104.96(8) . . ? Cl4 Ti2 C25 85.77(6) . . ? Cl3 Ti2 C25 131.79(6) . . ? C24 Ti2 C25 34.41(8) . . ? C23 Ti2 C25 58.77(8) . . ? C36 Ti2 C27 134.03(8) . . ? C35 Ti2 C27 117.17(9) . . ? Cl4 Ti2 C27 106.53(6) . . ? Cl3 Ti2 C27 76.97(6) . . ? C24 Ti2 C27 56.60(8) . . ? C23 Ti2 C27 34.72(8) . . ? C25 Ti2 C27 57.39(8) . . ? C36 Ti2 C34 57.17(9) . . ? C35 Ti2 C34 34.17(8) . . ? Cl4 Ti2 C34 122.34(6) . . ? Cl3 Ti2 C34 79.68(6) . . ? C24 Ti2 C34 108.21(8) . . ? C23 Ti2 C34 101.00(8) . . ? C25 Ti2 C34 139.05(8) . . ? C27 Ti2 C34 126.66(8) . . ? C36 Ti2 C26 125.27(9) . . ? C35 Ti2 C26 133.19(9) . . ? Cl4 Ti2 C26 79.02(6) . . ? Cl3 Ti2 C26 97.70(6) . . ? C24 Ti2 C26 56.60(8) . . ? C23 Ti2 C26 57.63(8) . . ? C25 Ti2 C26 34.87(8) . . ? C27 Ti2 C26 33.65(8) . . ? C34 Ti2 C26 158.49(9) . . ? C36 Ti2 C37 34.39(8) . . ? C35 Ti2 C37 56.96(9) . . ? Cl4 Ti2 C37 77.18(6) . . ? Cl3 Ti2 C37 115.19(6) . . ? C24 Ti2 C37 110.91(8) . . ? C23 Ti2 C37 136.10(8) . . ? C25 Ti2 C37 111.65(8) . . ? C27 Ti2 C37 167.35(8) . . ? C34 Ti2 C37 56.11(8) . . ? C26 Ti2 C37 140.23(8) . . ? C36 Ti2 C38 57.17(8) . . ? C35 Ti2 C38 56.92(8) . . ? Cl4 Ti2 C38 88.60(6) . . ? Cl3 Ti2 C38 82.99(6) . . ? C24 Ti2 C38 131.95(8) . . ? C23 Ti2 C38 134.74(8) . . ? C25 Ti2 C38 145.02(8) . . ? C27 Ti2 C38 155.48(8) . . ? C34 Ti2 C38 33.84(8) . . ? C26 Ti2 C38 167.62(8) . . ? C37 Ti2 C38 33.78(8) . . ? C6 Si1 C7 108.19(14) . . ? C6 Si1 C8 110.41(15) . . ? C7 Si1 C8 110.07(14) . . ? C6 Si1 C1 106.35(12) . . ? C7 Si1 C1 114.23(11) . . ? C8 Si1 C1 107.53(12) . . ? C9 Si2 C11 110.77(13) . . ? C9 Si2 C10 110.33(13) . . ? C11 Si2 C10 108.99(13) . . ? C9 Si2 C3 107.59(12) . . ? C11 Si2 C3 113.82(11) . . ? C10 Si2 C3 105.19(11) . . ? C33 Si3 C32 110.63(13) . . ? C33 Si3 C31 109.25(12) . . ? C32 Si3 C31 110.44(13) . . ? C33 Si3 C25 113.97(11) . . ? C32 Si3 C25 106.65(12) . . ? C31 Si3 C25 105.77(11) . . ? C28 Si4 C30 108.47(13) . . ? C28 Si4 C29 110.08(15) . . ? C30 Si4 C29 110.88(14) . . ? C28 Si4 C23 106.22(12) . . ? C30 Si4 C23 115.01(12) . . ? C29 Si4 C23 106.04(12) . . ? C20 N1 C21 110.1(2) . . ? C20 N1 C22 110.5(2) . . ? C21 N1 C22 109.8(2) . . ? C44 N2 C42 109.6(2) . . ? C44 N2 C43 110.8(2) . . ? C42 N2 C43 110.4(2) . . ? C5 C1 C2 104.9(2) . . ? C5 C1 Si1 125.92(17) . . ? C2 C1 Si1 127.30(17) . . ? C5 C1 Ti1 73.35(13) . . ? C2 C1 Ti1 72.06(13) . . ? Si1 C1 Ti1 131.08(12) . . ? C3 C2 C1 110.7(2) . . ? C3 C2 Ti1 72.90(13) . . ? C1 C2 Ti1 72.99(13) . . ? C3 C2 H2 124.6 . . ? C1 C2 H2 124.6 . . ? Ti1 C2 H2 121.1 . . ? C2 C3 C4 105.4(2) . . ? C2 C3 Si2 127.37(17) . . ? C4 C3 Si2 126.49(18) . . ? C2 C3 Ti1 72.57(13) . . ? C4 C3 Ti1 73.04(13) . . ? Si2 C3 Ti1 126.56(12) . . ? C5 C4 C3 109.2(2) . . ? C5 C4 Ti1 73.60(14) . . ? C3 C4 Ti1 72.15(13) . . ? C5 C4 H4 125.4 . . ? C3 C4 H4 125.4 . . ? Ti1 C4 H4 120.5 . . ? C4 C5 C1 109.7(2) . . ? C4 C5 Ti1 72.68(14) . . ? C1 C5 Ti1 72.16(13) . . ? C4 C5 H5 125.2 . . ? C1 C5 H5 125.2 . . ? Ti1 C5 H5 121.6 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C16 108.8(2) . . ? C13 C12 Ti1 70.71(14) . . ? C16 C12 Ti1 75.64(14) . . ? C13 C12 H12 125.6 . . ? C16 C12 H12 125.6 . . ? Ti1 C12 H12 119.8 . . ? C12 C13 C14 108.1(2) . . ? C12 C13 Ti1 75.21(14) . . ? C14 C13 Ti1 71.94(13) . . ? C12 C13 H13 126.0 . . ? C14 C13 H13 126.0 . . ? Ti1 C13 H13 118.8 . . ? C15 C14 C13 107.2(2) . . ? C15 C14 Ti1 76.18(14) . . ? C13 C14 Ti1 72.88(13) . . ? C15 C14 H14 126.4 . . ? C13 C14 H14 126.4 . . ? Ti1 C14 H14 116.7 . . ? C16 C15 C14 109.1(2) . . ? C16 C15 Ti1 75.23(14) . . ? C14 C15 Ti1 69.45(14) . . ? C16 C15 H15 125.4 . . ? C14 C15 H15 125.4 . . ? Ti1 C15 H15 121.5 . . ? C15 C16 C12 106.8(2) . . ? C15 C16 C17 128.2(2) . . ? C12 C16 C17 125.0(2) . . ? C15 C16 Ti1 71.45(14) . . ? C12 C16 Ti1 70.58(13) . . ? C17 C16 Ti1 125.92(15) . . ? C16 C17 C19 114.5(2) . . ? C16 C17 C18 110.4(2) . . ? C19 C17 C18 108.5(2) . . ? C16 C17 H17 107.7 . . ? C19 C17 H17 107.7 . . ? C18 C17 H17 107.7 . . ? C21 C18 C17 110.6(2) . . ? C21 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? C21 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C17 C19 C20 111.2(2) . . ? C17 C19 H19A 109.4 . . ? C20 C19 H19A 109.4 . . ? C17 C19 H19B 109.4 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? N1 C20 C19 112.4(2) . . ? N1 C20 H20A 109.1 . . ? C19 C20 H20A 109.1 . . ? N1 C20 H20B 109.1 . . ? C19 C20 H20B 109.1 . . ? H20A C20 H20B 107.9 . . ? N1 C21 C18 111.7(2) . . ? N1 C21 H21A 109.3 . . ? C18 C21 H21A 109.3 . . ? N1 C21 H21B 109.3 . . ? C18 C21 H21B 109.3 . . ? H21A C21 H21B 107.9 . . ? N1 C22 H22A 109.5 . . ? N1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C27 C23 C24 104.8(2) . . ? C27 C23 Si4 126.86(18) . . ? C24 C23 Si4 126.96(18) . . ? C27 C23 Ti2 73.43(14) . . ? C24 C23 Ti2 72.34(13) . . ? Si4 C23 Ti2 129.08(12) . . ? C25 C24 C23 110.9(2) . . ? C25 C24 Ti2 73.34(13) . . ? C23 C24 Ti2 72.60(13) . . ? C25 C24 H24 124.6 . . ? C23 C24 H24 124.6 . . ? Ti2 C24 H24 121.1 . . ? C24 C25 C26 105.5(2) . . ? C24 C25 Si3 128.43(17) . . ? C26 C25 Si3 125.28(18) . . ? C24 C25 Ti2 72.25(13) . . ? C26 C25 Ti2 72.98(13) . . ? Si3 C25 Ti2 127.41(12) . . ? C27 C26 C25 109.0(2) . . ? C27 C26 Ti2 73.13(14) . . ? C25 C26 Ti2 72.15(13) . . ? C27 C26 H26 125.5 . . ? C25 C26 H26 125.5 . . ? Ti2 C26 H26 120.9 . . ? C26 C27 C23 109.8(2) . . ? C26 C27 Ti2 73.22(14) . . ? C23 C27 Ti2 71.85(13) . . ? C26 C27 H27 125.1 . . ? C23 C27 H27 125.1 . . ? Ti2 C27 H27 121.5 . . ? Si4 C28 H28A 109.5 . . ? Si4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si4 C29 H29A 109.5 . . ? Si4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si4 C30 H30A 109.5 . . ? Si4 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si4 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si3 C31 H31A 109.5 . . ? Si3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si3 C32 H32A 109.5 . . ? Si3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si3 C33 H33A 109.5 . . ? Si3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C38 109.2(2) . . ? C35 C34 Ti2 71.12(14) . . ? C38 C34 Ti2 74.96(14) . . ? C35 C34 H34 125.4 . . ? C38 C34 H34 125.4 . . ? Ti2 C34 H34 120.2 . . ? C34 C35 C36 107.8(2) . . ? C34 C35 Ti2 74.71(13) . . ? C36 C35 Ti2 71.96(13) . . ? C34 C35 H35 126.1 . . ? C36 C35 H35 126.1 . . ? Ti2 C35 H35 119.1 . . ? C37 C36 C35 107.5(2) . . ? C37 C36 Ti2 75.28(14) . . ? C35 C36 Ti2 73.07(13) . . ? C37 C36 H36 126.3 . . ? C35 C36 H36 126.3 . . ? Ti2 C36 H36 117.5 . . ? C36 C37 C38 109.2(2) . . ? C36 C37 Ti2 70.33(14) . . ? C38 C37 Ti2 74.86(14) . . ? C36 C37 H37 125.4 . . ? C38 C37 H37 125.4 . . ? Ti2 C37 H37 121.0 . . ? C37 C38 C34 106.3(2) . . ? C37 C38 C39 126.4(2) . . ? C34 C38 C39 127.2(2) . . ? C37 C38 Ti2 71.36(14) . . ? C34 C38 Ti2 71.20(14) . . ? C39 C38 Ti2 124.91(16) . . ? C38 C39 C40 110.7(2) . . ? C38 C39 C41 112.3(2) . . ? C40 C39 C41 108.6(2) . . ? C38 C39 H39 108.4 . . ? C40 C39 H39 108.4 . . ? C41 C39 H39 108.4 . . ? C43 C40 C39 111.7(2) . . ? C43 C40 H40A 109.3 . . ? C39 C40 H40A 109.3 . . ? C43 C40 H40B 109.3 . . ? C39 C40 H40B 109.3 . . ? H40A C40 H40B 108.0 . . ? C42 C41 C39 111.9(2) . . ? C42 C41 H41A 109.2 . . ? C39 C41 H41A 109.2 . . ? C42 C41 H41B 109.2 . . ? C39 C41 H41B 109.2 . . ? H41A C41 H41B 107.9 . . ? N2 C42 C41 111.6(2) . . ? N2 C42 H42A 109.3 . . ? C41 C42 H42A 109.3 . . ? N2 C42 H42B 109.3 . . ? C41 C42 H42B 109.3 . . ? H42A C42 H42B 108.0 . . ? N2 C43 C40 111.0(2) . . ? N2 C43 H43A 109.4 . . ? C40 C43 H43A 109.4 . . ? N2 C43 H43B 109.4 . . ? C40 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? N2 C44 H44A 109.5 . . ? N2 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N2 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.346 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.064 # Attachment 'cmpd_10.CIF' data_compound_10 _database_code_depnum_ccdc_archive 'CCDC 649316' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H38 Cl2 N Si2 Ti, Cl' _chemical_formula_sum 'C22 H38 Cl3 N Si2 Ti' _chemical_formula_weight 526.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 monoclinic _symmetry_space_group_name_H-M P21 _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 6.648(1) _cell_length_b 12.313(3) _cell_length_c 16.448(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.44(3) _cell_angle_gamma 90.00 _cell_volume 1328.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 0.724 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8991 _exptl_absorpt_correction_T_max 0.9181 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV. See R.H. Blessing, Acta Cryst (1995), A51, 33-38. ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data since the entire data set is used to refine the cell, which is indexed from all observed reflections in a 10 degree range. The crystal temperature was held constant using an Oxford Cryosystems Cryostream 600 system. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe x-ray _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 ; Nonius KappaCCD area-detector diffractometer ; _diffrn_radiation_detector 'CCD plate' _diffrn_measurement_method ; phi and omega scans to fill the asymmetric unit ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 42257 _diffrn_reflns_av_R_equivalents 0.0880 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6086 _reflns_number_gt 5763 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction ; DENZO-SMN and COLLECT (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 2001)' _computing_publication_material ; local program ; _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^)+(0.0415P)^2^+0.2658P] 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 -0.020(19) _refine_ls_number_reflns 6086 _refine_ls_number_parameters 269 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.79451(5) 0.04619(3) 0.21480(2) 0.02696(8) Uani 1 1 d . . . Cl1 Cl 0.59448(8) 0.11417(4) 0.30976(3) 0.03429(11) Uani 1 1 d . . . C1 C 0.9448(3) -0.04350(18) 0.34043(14) 0.0351(4) Uani 1 1 d . . . H1 H 0.9404 -0.0118 0.3928 0.042 Uiso 1 1 calc R . . Cl2 Cl 0.50399(7) -0.03334(4) 0.13213(3) 0.03565(12) Uani 1 1 d . . . C2 C 1.0950(3) -0.0245(2) 0.29165(16) 0.0412(5) Uani 1 1 d . . . H2 H 1.2091 0.0224 0.3050 0.049 Uiso 1 1 calc R . . Cl3 Cl -0.24753(8) -0.45273(5) 0.48219(3) 0.03877(12) Uani 1 1 d . . . C3 C 1.0474(3) -0.08748(18) 0.21895(16) 0.0395(5) Uani 1 1 d . . . H3 H 1.1228 -0.0901 0.1747 0.047 Uiso 1 1 calc R . . C4 C 0.8679(3) -0.14541(17) 0.22451(14) 0.0338(4) Uani 1 1 d . . . H4 H 0.8028 -0.1952 0.1845 0.041 Uiso 1 1 calc R . . Si5 Si 0.83295(9) 0.35090(5) 0.28137(4) 0.03213(12) Uani 1 1 d . . . C5 C 0.7996(3) -0.11804(17) 0.29884(13) 0.0302(4) Uani 1 1 d . . . Si6 Si 0.72648(10) 0.08371(5) -0.02252(3) 0.03792(14) Uani 1 1 d . . . C6 C 0.6097(3) -0.15864(16) 0.32851(12) 0.0280(4) Uani 1 1 d . . . H6 H 0.4946 -0.1093 0.3059 0.034 Uiso 1 1 calc R . . C7 C 0.6327(3) -0.15641(18) 0.42280(12) 0.0342(4) Uani 1 1 d . . . H7A H 0.7528 -0.2003 0.4466 0.041 Uiso 1 1 calc R . . H7B H 0.6566 -0.0808 0.4424 0.041 Uiso 1 1 calc R . . C8 C 0.4442(4) -0.20082(18) 0.45249(13) 0.0365(5) Uani 1 1 d . . . H8A H 0.4670 -0.2020 0.5135 0.044 Uiso 1 1 calc R . . H8B H 0.3266 -0.1526 0.4335 0.044 Uiso 1 1 calc R . . N9 N 0.3971(3) -0.31280(14) 0.42043(10) 0.0297(3) Uani 1 1 d . . . H9 H 0.5096 -0.3561 0.4393 0.036 Uiso 1 1 calc R . . C9 C 0.2190(3) -0.3601(2) 0.45186(15) 0.0407(5) Uani 1 1 d . . . H9A H 0.2470 -0.3624 0.5122 0.061 Uiso 1 1 calc R . . H9B H 0.1944 -0.4340 0.4303 0.061 Uiso 1 1 calc R . . H9C H 0.0982 -0.3153 0.4338 0.061 Uiso 1 1 calc R . . C10 C 0.3657(3) -0.31458(17) 0.32837(12) 0.0314(4) Uani 1 1 d . . . H10A H 0.2472 -0.2685 0.3063 0.038 Uiso 1 1 calc R . . H10B H 0.3360 -0.3897 0.3086 0.038 Uiso 1 1 calc R . . C11 C 0.5545(3) -0.27304(16) 0.29695(13) 0.0318(4) Uani 1 1 d . . . H11A H 0.5290 -0.2727 0.2359 0.038 Uiso 1 1 calc R . . H11B H 0.6703 -0.3225 0.3154 0.038 Uiso 1 1 calc R . . C12 C 1.0406(3) 0.18297(17) 0.20149(13) 0.0321(4) Uani 1 1 d . . . H12 H 1.1607 0.1869 0.2416 0.038 Uiso 1 1 calc R . . C13 C 1.0161(3) 0.11886(18) 0.12873(12) 0.0324(4) Uani 1 1 d . . . H13 H 1.1178 0.0736 0.1121 0.039 Uiso 1 1 calc R . . C14 C 0.8159(3) 0.13322(17) 0.08503(12) 0.0305(4) Uani 1 1 d . . . C15 C 0.7168(3) 0.20685(17) 0.13386(13) 0.0312(4) Uani 1 1 d . . . H15 H 0.5789 0.2298 0.1208 0.037 Uiso 1 1 calc R . . C16 C 0.8566(3) 0.24025(16) 0.20475(13) 0.0297(4) Uani 1 1 d . . . C17 C 0.9845(4) 0.3135(2) 0.38303(14) 0.0407(5) Uani 1 1 d . . . H17A H 0.9574 0.3658 0.4249 0.061 Uiso 1 1 calc R . . H17B H 1.1301 0.3146 0.3792 0.061 Uiso 1 1 calc R . . H17C H 0.9458 0.2406 0.3985 0.061 Uiso 1 1 calc R . . C18 C 0.9574(4) 0.47182(19) 0.24112(15) 0.0432(5) Uani 1 1 d . . . H18A H 0.8886 0.4886 0.1852 0.065 Uiso 1 1 calc R . . H18B H 1.1013 0.4557 0.2401 0.065 Uiso 1 1 calc R . . H18C H 0.9473 0.5344 0.2771 0.065 Uiso 1 1 calc R . . C19 C 0.5615(4) 0.3885(2) 0.28337(16) 0.0439(5) Uani 1 1 d . . . H19A H 0.4979 0.4133 0.2285 0.066 Uiso 1 1 calc R . . H19B H 0.5565 0.4469 0.3235 0.066 Uiso 1 1 calc R . . H19C H 0.4878 0.3250 0.2991 0.066 Uiso 1 1 calc R . . C20 C 0.8614(4) 0.1735(2) -0.08814(15) 0.0473(6) Uani 1 1 d . . . H20A H 0.8141 0.2484 -0.0847 0.071 Uiso 1 1 calc R . . H20B H 0.8322 0.1488 -0.1455 0.071 Uiso 1 1 calc R . . H20C H 1.0087 0.1702 -0.0686 0.071 Uiso 1 1 calc R . . C21 C 0.4465(4) 0.1062(3) -0.05444(16) 0.0605(7) Uani 1 1 d . . . H21A H 0.3709 0.0526 -0.0272 0.091 Uiso 1 1 calc R . . H21B H 0.4107 0.0981 -0.1143 0.091 Uiso 1 1 calc R . . H21C H 0.4110 0.1795 -0.0385 0.091 Uiso 1 1 calc R . . C22 C 0.8061(6) -0.0605(2) -0.03256(17) 0.0580(7) Uani 1 1 d . . . H22A H 0.9529 -0.0673 -0.0128 0.087 Uiso 1 1 calc R . . H22B H 0.7758 -0.0825 -0.0905 0.087 Uiso 1 1 calc R . . H22C H 0.7315 -0.1073 0.0004 0.087 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 0.02414(15) 0.02757(16) 0.02922(17) 0.00030(13) 0.00455(12) -0.00101(14) Cl1 0.0352(2) 0.0323(2) 0.0376(2) -0.00111(19) 0.01256(19) -0.00083(19) C1 0.0286(9) 0.0354(10) 0.0380(10) 0.0046(9) -0.0044(8) -0.0036(8) Cl2 0.0280(2) 0.0433(3) 0.0349(2) 0.0006(2) 0.00267(19) -0.0064(2) C2 0.0251(10) 0.0375(11) 0.0583(13) 0.0105(11) -0.0011(9) -0.0004(9) Cl3 0.0348(2) 0.0357(2) 0.0441(3) 0.0084(2) 0.00163(19) 0.0039(2) C3 0.0322(11) 0.0329(11) 0.0568(13) 0.0076(10) 0.0167(10) 0.0063(9) C4 0.0325(10) 0.0282(10) 0.0422(11) 0.0019(8) 0.0104(9) 0.0030(8) Si5 0.0317(3) 0.0298(3) 0.0338(3) -0.0002(2) 0.0020(2) 0.0002(2) C5 0.0286(9) 0.0272(9) 0.0335(10) 0.0037(8) 0.0013(8) -0.0002(8) Si6 0.0444(3) 0.0394(3) 0.0293(3) 0.0005(2) 0.0041(2) -0.0008(3) C6 0.0275(9) 0.0250(9) 0.0311(9) 0.0017(7) 0.0038(7) -0.0014(7) C7 0.0409(11) 0.0311(10) 0.0308(10) -0.0067(8) 0.0063(8) -0.0061(9) C8 0.0473(12) 0.0312(10) 0.0328(10) -0.0047(8) 0.0124(9) -0.0006(9) N9 0.0297(8) 0.0296(8) 0.0298(8) 0.0031(7) 0.0050(7) 0.0018(7) C9 0.0363(11) 0.0447(13) 0.0433(11) 0.0076(10) 0.0133(9) -0.0016(9) C10 0.0311(10) 0.0322(10) 0.0299(9) -0.0001(8) 0.0022(8) -0.0049(8) C11 0.0355(10) 0.0318(10) 0.0284(9) -0.0050(8) 0.0058(8) -0.0063(8) C12 0.0272(10) 0.0312(10) 0.0371(10) 0.0054(8) 0.0032(8) -0.0019(8) C13 0.0298(9) 0.0344(10) 0.0342(10) 0.0053(8) 0.0091(8) 0.0007(8) C14 0.0310(10) 0.0311(10) 0.0301(9) 0.0041(8) 0.0072(8) 0.0005(8) C15 0.0284(9) 0.0301(10) 0.0347(10) 0.0067(8) 0.0042(8) 0.0008(8) C16 0.0315(9) 0.0274(9) 0.0302(10) 0.0043(7) 0.0046(8) -0.0032(8) C17 0.0437(12) 0.0410(12) 0.0356(10) 0.0000(9) 0.0007(9) 0.0007(10) C18 0.0467(13) 0.0341(11) 0.0479(12) 0.0009(10) 0.0049(10) -0.0061(10) C19 0.0368(12) 0.0421(12) 0.0523(13) -0.0055(10) 0.0059(10) 0.0068(10) C20 0.0561(15) 0.0514(14) 0.0357(11) 0.0079(10) 0.0117(10) -0.0003(12) C21 0.0476(14) 0.087(2) 0.0426(13) 0.0043(14) -0.0059(11) -0.0046(15) C22 0.093(2) 0.0411(13) 0.0439(13) -0.0060(11) 0.0237(14) 0.0001(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 C3 2.346(2) . ? Ti1 C2 2.349(2) . ? Ti1 Cl1 2.3642(8) . ? Ti1 C13 2.379(2) . ? Ti1 Cl2 2.3826(9) . ? Ti1 C12 2.383(2) . ? Ti1 C15 2.393(2) . ? Ti1 C4 2.409(2) . ? Ti1 C1 2.411(2) . ? Ti1 C14 2.413(2) . ? Ti1 C16 2.435(2) . ? Ti1 C5 2.447(2) . ? C1 C2 1.400(3) . ? C1 C5 1.423(3) . ? C1 H1 0.9500 . ? C2 C3 1.417(4) . ? C2 H2 0.9500 . ? C3 C4 1.406(3) . ? C3 H3 0.9500 . ? C4 C5 1.413(3) . ? C4 H4 0.9500 . ? Si5 C17 1.863(2) . ? Si5 C19 1.868(2) . ? Si5 C18 1.876(2) . ? Si5 C16 1.880(2) . ? C5 C6 1.511(3) . ? Si6 C22 1.868(3) . ? Si6 C21 1.870(3) . ? Si6 C20 1.873(3) . ? Si6 C14 1.873(2) . ? C6 C11 1.525(3) . ? C6 C7 1.534(3) . ? C6 H6 1.0000 . ? C7 C8 1.519(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N9 1.491(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N9 C9 1.486(3) . ? N9 C10 1.494(2) . ? N9 H9 0.9300 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.522(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C16 1.420(3) . ? C12 C13 1.420(3) . ? C12 H12 0.9500 . ? C13 C14 1.417(3) . ? C13 H13 0.9500 . ? C14 C15 1.440(3) . ? C15 C16 1.427(3) . ? C15 H15 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Ti1 C2 35.13(9) . . ? C3 Ti1 Cl1 135.01(6) . . ? C2 Ti1 Cl1 107.25(7) . . ? C3 Ti1 C13 76.72(8) . . ? C2 Ti1 C13 84.52(8) . . ? Cl1 Ti1 C13 136.91(6) . . ? C3 Ti1 Cl2 103.79(6) . . ? C2 Ti1 Cl2 133.87(7) . . ? Cl1 Ti1 Cl2 91.80(3) . . ? C13 Ti1 Cl2 109.76(5) . . ? C3 Ti1 C12 89.94(7) . . ? C2 Ti1 C12 77.01(8) . . ? Cl1 Ti1 C12 106.23(6) . . ? C13 Ti1 C12 34.71(7) . . ? Cl2 Ti1 C12 137.94(5) . . ? C3 Ti1 C15 133.19(8) . . ? C2 Ti1 C15 133.83(8) . . ? Cl1 Ti1 C15 88.94(5) . . ? C13 Ti1 C15 57.06(7) . . ? Cl2 Ti1 C15 86.65(6) . . ? C12 Ti1 C15 56.86(7) . . ? C3 Ti1 C4 34.36(7) . . ? C2 Ti1 C4 57.06(8) . . ? Cl1 Ti1 C4 115.64(5) . . ? C13 Ti1 C4 105.62(8) . . ? Cl2 Ti1 C4 76.81(6) . . ? C12 Ti1 C4 124.30(7) . . ? C15 Ti1 C4 150.37(8) . . ? C3 Ti1 C1 57.27(8) . . ? C2 Ti1 C1 34.17(8) . . ? Cl1 Ti1 C1 78.16(6) . . ? C13 Ti1 C1 118.19(7) . . ? Cl2 Ti1 C1 118.96(6) . . ? C12 Ti1 C1 102.03(7) . . ? C15 Ti1 C1 151.27(8) . . ? C4 Ti1 C1 56.19(8) . . ? C3 Ti1 C14 101.04(8) . . ? C2 Ti1 C14 118.18(8) . . ? Cl1 Ti1 C14 123.24(5) . . ? C13 Ti1 C14 34.38(7) . . ? Cl2 Ti1 C14 80.65(5) . . ? C12 Ti1 C14 57.59(7) . . ? C15 Ti1 C14 34.87(7) . . ? C4 Ti1 C14 116.93(7) . . ? C1 Ti1 C14 152.30(7) . . ? C3 Ti1 C16 124.18(8) . . ? C2 Ti1 C16 105.16(8) . . ? Cl1 Ti1 C16 79.48(5) . . ? C13 Ti1 C16 57.46(7) . . ? Cl2 Ti1 C16 119.68(5) . . ? C12 Ti1 C16 34.27(7) . . ? C15 Ti1 C16 34.37(7) . . ? C4 Ti1 C16 158.54(7) . . ? C1 Ti1 C16 117.17(7) . . ? C14 Ti1 C16 57.93(7) . . ? C3 Ti1 C5 57.33(7) . . ? C2 Ti1 C5 57.17(7) . . ? Cl1 Ti1 C5 82.91(5) . . ? C13 Ti1 C5 133.99(7) . . ? Cl2 Ti1 C5 85.28(5) . . ? C12 Ti1 C5 133.63(7) . . ? C15 Ti1 C5 168.32(7) . . ? C4 Ti1 C5 33.82(7) . . ? C1 Ti1 C5 34.06(7) . . ? C14 Ti1 C5 150.39(7) . . ? C16 Ti1 C5 149.61(7) . . ? C2 C1 C5 108.9(2) . . ? C2 C1 Ti1 70.52(13) . . ? C5 C1 Ti1 74.36(12) . . ? C2 C1 H1 125.6 . . ? C5 C1 H1 125.6 . . ? Ti1 C1 H1 121.2 . . ? C1 C2 C3 108.1(2) . . ? C1 C2 Ti1 75.31(13) . . ? C3 C2 Ti1 72.30(13) . . ? C1 C2 H2 125.9 . . ? C3 C2 H2 125.9 . . ? Ti1 C2 H2 118.4 . . ? C4 C3 C2 107.3(2) . . ? C4 C3 Ti1 75.29(12) . . ? C2 C3 Ti1 72.57(13) . . ? C4 C3 H3 126.4 . . ? C2 C3 H3 126.4 . . ? Ti1 C3 H3 117.8 . . ? C3 C4 C5 109.4(2) . . ? C3 C4 Ti1 70.35(12) . . ? C5 C4 Ti1 74.54(12) . . ? C3 C4 H4 125.3 . . ? C5 C4 H4 125.3 . . ? Ti1 C4 H4 121.4 . . ? C17 Si5 C19 115.28(12) . . ? C17 Si5 C18 107.93(11) . . ? C19 Si5 C18 107.01(12) . . ? C17 Si5 C16 109.29(10) . . ? C19 Si5 C16 112.25(11) . . ? C18 Si5 C16 104.39(10) . . ? C4 C5 C1 106.32(19) . . ? C4 C5 C6 127.19(18) . . ? C1 C5 C6 126.49(19) . . ? C4 C5 Ti1 71.64(12) . . ? C1 C5 Ti1 71.58(12) . . ? C6 C5 Ti1 121.39(13) . . ? C22 Si6 C21 113.53(16) . . ? C22 Si6 C20 109.90(13) . . ? C21 Si6 C20 107.45(13) . . ? C22 Si6 C14 110.01(11) . . ? C21 Si6 C14 111.35(12) . . ? C20 Si6 C14 104.14(11) . . ? C5 C6 C11 111.29(17) . . ? C5 C6 C7 111.77(17) . . ? C11 C6 C7 109.82(16) . . ? C5 C6 H6 107.9 . . ? C11 C6 H6 107.9 . . ? C7 C6 H6 107.9 . . ? C8 C7 C6 111.60(17) . . ? C8 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? C8 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? N9 C8 C7 110.83(17) . . ? N9 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? N9 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C9 N9 C8 111.89(17) . . ? C9 N9 C10 111.10(16) . . ? C8 N9 C10 110.98(15) . . ? C9 N9 H9 107.5 . . ? C8 N9 H9 107.5 . . ? C10 N9 H9 107.5 . . ? N9 C9 H9A 109.5 . . ? N9 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N9 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N9 C10 C11 110.70(16) . . ? N9 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? N9 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C10 C11 C6 111.15(17) . . ? C10 C11 H11A 109.4 . . ? C6 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? C6 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C16 C12 C13 109.12(18) . . ? C16 C12 Ti1 74.88(12) . . ? C13 C12 Ti1 72.50(12) . . ? C16 C12 H12 125.4 . . ? C13 C12 H12 125.4 . . ? Ti1 C12 H12 119.0 . . ? C14 C13 C12 109.04(19) . . ? C14 C13 Ti1 74.13(11) . . ? C12 C13 Ti1 72.79(11) . . ? C14 C13 H13 125.5 . . ? C12 C13 H13 125.5 . . ? Ti1 C13 H13 119.4 . . ? C13 C14 C15 105.85(18) . . ? C13 C14 Si6 124.38(16) . . ? C15 C14 Si6 128.93(15) . . ? C13 C14 Ti1 71.49(11) . . ? C15 C14 Ti1 71.80(11) . . ? Si6 C14 Ti1 129.43(10) . . ? C16 C15 C14 109.95(18) . . ? C16 C15 Ti1 74.43(11) . . ? C14 C15 Ti1 73.33(11) . . ? C16 C15 H15 125.0 . . ? C14 C15 H15 125.0 . . ? Ti1 C15 H15 118.9 . . ? C12 C16 C15 105.98(18) . . ? C12 C16 Si5 123.53(16) . . ? C15 C16 Si5 129.92(16) . . ? C12 C16 Ti1 70.85(12) . . ? C15 C16 Ti1 71.20(11) . . ? Si5 C16 Ti1 129.19(10) . . ? Si5 C17 H17A 109.5 . . ? Si5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si5 C18 H18A 109.5 . . ? Si5 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si5 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si5 C19 H19A 109.5 . . ? Si5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si6 C20 H20A 109.5 . . ? Si6 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si6 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si6 C21 H21A 109.5 . . ? Si6 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si6 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si6 C22 H22A 109.5 . . ? Si6 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si6 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? 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 C3 Ti1 C1 C2 38.35(14) . . . . ? Cl1 Ti1 C1 C2 -148.03(14) . . . . ? C13 Ti1 C1 C2 -10.79(17) . . . . ? Cl2 Ti1 C1 C2 126.52(13) . . . . ? C12 Ti1 C1 C2 -43.71(15) . . . . ? C15 Ti1 C1 C2 -83.0(2) . . . . ? C4 Ti1 C1 C2 79.71(15) . . . . ? C14 Ti1 C1 C2 -4.4(2) . . . . ? C16 Ti1 C1 C2 -76.53(16) . . . . ? C5 Ti1 C1 C2 117.1(2) . . . . ? C3 Ti1 C1 C5 -78.75(14) . . . . ? C2 Ti1 C1 C5 -117.1(2) . . . . ? Cl1 Ti1 C1 C5 94.87(12) . . . . ? C13 Ti1 C1 C5 -127.89(13) . . . . ? Cl2 Ti1 C1 C5 9.42(15) . . . . ? C12 Ti1 C1 C5 -160.81(13) . . . . ? C15 Ti1 C1 C5 159.92(14) . . . . ? C4 Ti1 C1 C5 -37.39(12) . . . . ? C14 Ti1 C1 C5 -121.46(17) . . . . ? C16 Ti1 C1 C5 166.37(12) . . . . ? C5 C1 C2 C3 -0.4(2) . . . . ? Ti1 C1 C2 C3 -65.40(16) . . . . ? C5 C1 C2 Ti1 64.96(15) . . . . ? C3 Ti1 C2 C1 -114.9(2) . . . . ? Cl1 Ti1 C2 C1 32.86(15) . . . . ? C13 Ti1 C2 C1 170.46(15) . . . . ? Cl2 Ti1 C2 C1 -77.27(16) . . . . ? C12 Ti1 C2 C1 136.08(15) . . . . ? C15 Ti1 C2 C1 138.60(14) . . . . ? C4 Ti1 C2 C1 -76.93(14) . . . . ? C14 Ti1 C2 C1 177.70(13) . . . . ? C16 Ti1 C2 C1 116.32(14) . . . . ? C5 Ti1 C2 C1 -36.39(13) . . . . ? Cl1 Ti1 C2 C3 147.75(12) . . . . ? C13 Ti1 C2 C3 -74.65(14) . . . . ? Cl2 Ti1 C2 C3 37.62(16) . . . . ? C12 Ti1 C2 C3 -109.03(14) . . . . ? C15 Ti1 C2 C3 -106.52(15) . . . . ? C4 Ti1 C2 C3 37.96(12) . . . . ? C1 Ti1 C2 C3 114.9(2) . . . . ? C14 Ti1 C2 C3 -67.41(15) . . . . ? C16 Ti1 C2 C3 -128.79(13) . . . . ? C5 Ti1 C2 C3 78.49(14) . . . . ? C1 C2 C3 C4 -0.5(3) . . . . ? Ti1 C2 C3 C4 -67.88(15) . . . . ? C1 C2 C3 Ti1 67.40(16) . . . . ? C2 Ti1 C3 C4 113.87(19) . . . . ? Cl1 Ti1 C3 C4 67.74(16) . . . . ? C13 Ti1 C3 C4 -146.64(15) . . . . ? Cl2 Ti1 C3 C4 -39.19(14) . . . . ? C12 Ti1 C3 C4 -179.04(14) . . . . ? C15 Ti1 C3 C4 -137.69(13) . . . . ? C1 Ti1 C3 C4 76.59(14) . . . . ? C14 Ti1 C3 C4 -122.15(14) . . . . ? C16 Ti1 C3 C4 179.28(12) . . . . ? C5 Ti1 C3 C4 35.85(12) . . . . ? Cl1 Ti1 C3 C2 -46.13(16) . . . . ? C13 Ti1 C3 C2 99.49(14) . . . . ? Cl2 Ti1 C3 C2 -153.06(12) . . . . ? C12 Ti1 C3 C2 67.10(14) . . . . ? C15 Ti1 C3 C2 108.45(15) . . . . ? C4 Ti1 C3 C2 -113.87(19) . . . . ? C1 Ti1 C3 C2 -37.28(13) . . . . ? C14 Ti1 C3 C2 123.98(13) . . . . ? C16 Ti1 C3 C2 65.42(16) . . . . ? C5 Ti1 C3 C2 -78.02(14) . . . . ? C2 C3 C4 C5 1.2(2) . . . . ? Ti1 C3 C4 C5 -64.80(15) . . . . ? C2 C3 C4 Ti1 66.04(15) . . . . ? C2 Ti1 C4 C3 -38.83(14) . . . . ? Cl1 Ti1 C4 C3 -133.47(13) . . . . ? C13 Ti1 C4 C3 33.76(15) . . . . ? Cl2 Ti1 C4 C3 140.92(14) . . . . ? C12 Ti1 C4 C3 1.17(17) . . . . ? C15 Ti1 C4 C3 83.2(2) . . . . ? C1 Ti1 C4 C3 -80.01(15) . . . . ? C14 Ti1 C4 C3 68.76(15) . . . . ? C16 Ti1 C4 C3 -1.6(3) . . . . ? C5 Ti1 C4 C3 -117.67(19) . . . . ? C3 Ti1 C4 C5 117.67(19) . . . . ? C2 Ti1 C4 C5 78.84(14) . . . . ? Cl1 Ti1 C4 C5 -15.80(13) . . . . ? C13 Ti1 C4 C5 151.43(12) . . . . ? Cl2 Ti1 C4 C5 -101.41(12) . . . . ? C12 Ti1 C4 C5 118.84(13) . . . . ? C15 Ti1 C4 C5 -159.15(13) . . . . ? C1 Ti1 C4 C5 37.66(12) . . . . ? C14 Ti1 C4 C5 -173.57(11) . . . . ? C16 Ti1 C4 C5 116.1(2) . . . . ? C3 C4 C5 C1 -1.5(2) . . . . ? Ti1 C4 C5 C1 -63.64(14) . . . . ? C3 C4 C5 C6 178.07(19) . . . . ? Ti1 C4 C5 C6 115.9(2) . . . . ? C3 C4 C5 Ti1 62.15(15) . . . . ? C2 C1 C5 C4 1.2(2) . . . . ? Ti1 C1 C5 C4 63.67(14) . . . . ? C2 C1 C5 C6 -178.4(2) . . . . ? Ti1 C1 C5 C6 -115.9(2) . . . . ? C2 C1 C5 Ti1 -62.50(15) . . . . ? C3 Ti1 C5 C4 -36.43(13) . . . . ? C2 Ti1 C5 C4 -78.48(14) . . . . ? Cl1 Ti1 C5 C4 165.68(12) . . . . ? C13 Ti1 C5 C4 -39.80(16) . . . . ? Cl2 Ti1 C5 C4 73.26(12) . . . . ? C12 Ti1 C5 C4 -88.63(15) . . . . ? C15 Ti1 C5 C4 119.6(4) . . . . ? C1 Ti1 C5 C4 -115.00(18) . . . . ? C14 Ti1 C5 C4 11.7(2) . . . . ? C16 Ti1 C5 C4 -139.48(14) . . . . ? C3 Ti1 C5 C1 78.56(14) . . . . ? C2 Ti1 C5 C1 36.51(14) . . . . ? Cl1 Ti1 C5 C1 -79.33(13) . . . . ? C13 Ti1 C5 C1 75.19(16) . . . . ? Cl2 Ti1 C5 C1 -171.74(13) . . . . ? C12 Ti1 C5 C1 26.36(18) . . . . ? C15 Ti1 C5 C1 -125.4(3) . . . . ? C4 Ti1 C5 C1 115.00(18) . . . . ? C14 Ti1 C5 C1 126.65(16) . . . . ? C16 Ti1 C5 C1 -24.5(2) . . . . ? C3 Ti1 C5 C6 -159.35(19) . . . . ? C2 Ti1 C5 C6 158.60(19) . . . . ? Cl1 Ti1 C5 C6 42.75(15) . . . . ? C13 Ti1 C5 C6 -162.73(14) . . . . ? Cl2 Ti1 C5 C6 -49.66(15) . . . . ? C12 Ti1 C5 C6 148.45(14) . . . . ? C15 Ti1 C5 C6 -3.3(5) . . . . ? C4 Ti1 C5 C6 -122.9(2) . . . . ? C1 Ti1 C5 C6 122.1(2) . . . . ? C14 Ti1 C5 C6 -111.27(18) . . . . ? C16 Ti1 C5 C6 97.60(19) . . . . ? C4 C5 C6 C11 30.4(3) . . . . ? C1 C5 C6 C11 -150.2(2) . . . . ? Ti1 C5 C6 C11 120.34(16) . . . . ? C4 C5 C6 C7 153.5(2) . . . . ? C1 C5 C6 C7 -27.0(3) . . . . ? Ti1 C5 C6 C7 -116.47(17) . . . . ? C5 C6 C7 C8 -178.10(17) . . . . ? C11 C6 C7 C8 -54.1(2) . . . . ? C6 C7 C8 N9 56.0(2) . . . . ? C7 C8 N9 C9 177.28(17) . . . . ? C7 C8 N9 C10 -58.0(2) . . . . ? C9 N9 C10 C11 -176.18(17) . . . . ? C8 N9 C10 C11 58.7(2) . . . . ? N9 C10 C11 C6 -57.3(2) . . . . ? C5 C6 C11 C10 178.84(16) . . . . ? C7 C6 C11 C10 54.5(2) . . . . ? C3 Ti1 C12 C16 -177.53(13) . . . . ? C2 Ti1 C12 C16 -144.58(14) . . . . ? Cl1 Ti1 C12 C16 -40.11(12) . . . . ? C13 Ti1 C12 C16 116.17(17) . . . . ? Cl2 Ti1 C12 C16 71.70(14) . . . . ? C15 Ti1 C12 C16 37.59(12) . . . . ? C4 Ti1 C12 C16 -178.19(11) . . . . ? C1 Ti1 C12 C16 -121.11(13) . . . . ? C14 Ti1 C12 C16 79.32(13) . . . . ? C5 Ti1 C12 C16 -135.84(12) . . . . ? C3 Ti1 C12 C13 66.30(13) . . . . ? C2 Ti1 C12 C13 99.25(14) . . . . ? Cl1 Ti1 C12 C13 -156.28(11) . . . . ? Cl2 Ti1 C12 C13 -44.47(15) . . . . ? C15 Ti1 C12 C13 -78.58(13) . . . . ? C4 Ti1 C12 C13 65.64(14) . . . . ? C1 Ti1 C12 C13 122.73(13) . . . . ? C14 Ti1 C12 C13 -36.84(12) . . . . ? C16 Ti1 C12 C13 -116.17(17) . . . . ? C5 Ti1 C12 C13 107.99(14) . . . . ? C16 C12 C13 C14 -0.7(2) . . . . ? Ti1 C12 C13 C14 65.82(15) . . . . ? C16 C12 C13 Ti1 -66.50(14) . . . . ? C3 Ti1 C13 C14 133.89(14) . . . . ? C2 Ti1 C13 C14 168.65(14) . . . . ? Cl1 Ti1 C13 C14 -81.86(14) . . . . ? Cl2 Ti1 C13 C14 33.79(13) . . . . ? C12 Ti1 C13 C14 -116.30(18) . . . . ? C15 Ti1 C13 C14 -38.33(12) . . . . ? C4 Ti1 C13 C14 115.09(13) . . . . ? C1 Ti1 C13 C14 174.71(12) . . . . ? C16 Ti1 C13 C14 -79.46(13) . . . . ? C5 Ti1 C13 C14 136.81(13) . . . . ? C3 Ti1 C13 C12 -109.81(13) . . . . ? C2 Ti1 C13 C12 -75.05(13) . . . . ? Cl1 Ti1 C13 C12 34.43(15) . . . . ? Cl2 Ti1 C13 C12 150.09(10) . . . . ? C15 Ti1 C13 C12 77.96(13) . . . . ? C4 Ti1 C13 C12 -128.61(12) . . . . ? C1 Ti1 C13 C12 -68.99(14) . . . . ? C14 Ti1 C13 C12 116.30(18) . . . . ? C16 Ti1 C13 C12 36.84(12) . . . . ? C5 Ti1 C13 C12 -106.90(14) . . . . ? C12 C13 C14 C15 -0.9(2) . . . . ? Ti1 C13 C14 C15 64.06(14) . . . . ? C12 C13 C14 Si6 169.43(15) . . . . ? Ti1 C13 C14 Si6 -125.63(15) . . . . ? C12 C13 C14 Ti1 -64.94(15) . . . . ? C22 Si6 C14 C13 47.5(2) . . . . ? C21 Si6 C14 C13 174.3(2) . . . . ? C20 Si6 C14 C13 -70.2(2) . . . . ? C22 Si6 C14 C15 -144.5(2) . . . . ? C21 Si6 C14 C15 -17.7(2) . . . . ? C20 Si6 C14 C15 97.8(2) . . . . ? C22 Si6 C14 Ti1 -46.17(17) . . . . ? C21 Si6 C14 Ti1 80.60(17) . . . . ? C20 Si6 C14 Ti1 -163.90(13) . . . . ? C3 Ti1 C14 C13 -45.61(14) . . . . ? C2 Ti1 C14 C13 -12.84(15) . . . . ? Cl1 Ti1 C14 C13 126.04(12) . . . . ? Cl2 Ti1 C14 C13 -147.96(13) . . . . ? C12 Ti1 C14 C13 37.21(13) . . . . ? C15 Ti1 C14 C13 114.41(18) . . . . ? C4 Ti1 C14 C13 -78.02(14) . . . . ? C1 Ti1 C14 C13 -10.1(2) . . . . ? C16 Ti1 C14 C13 77.98(14) . . . . ? C5 Ti1 C14 C13 -85.27(18) . . . . ? C3 Ti1 C14 C15 -160.02(12) . . . . ? C2 Ti1 C14 C15 -127.25(13) . . . . ? Cl1 Ti1 C14 C15 11.63(13) . . . . ? C13 Ti1 C14 C15 -114.41(18) . . . . ? Cl2 Ti1 C14 C15 97.63(11) . . . . ? C12 Ti1 C14 C15 -77.20(13) . . . . ? C4 Ti1 C14 C15 167.56(11) . . . . ? C1 Ti1 C14 C15 -124.48(17) . . . . ? C16 Ti1 C14 C15 -36.43(12) . . . . ? C5 Ti1 C14 C15 160.32(13) . . . . ? C3 Ti1 C14 Si6 74.11(14) . . . . ? C2 Ti1 C14 Si6 106.88(14) . . . . ? Cl1 Ti1 C14 Si6 -114.24(12) . . . . ? C13 Ti1 C14 Si6 119.7(2) . . . . ? Cl2 Ti1 C14 Si6 -28.24(12) . . . . ? C12 Ti1 C14 Si6 156.93(16) . . . . ? C15 Ti1 C14 Si6 -125.87(19) . . . . ? C4 Ti1 C14 Si6 41.69(15) . . . . ? C1 Ti1 C14 Si6 109.65(18) . . . . ? C16 Ti1 C14 Si6 -162.30(16) . . . . ? C5 Ti1 C14 Si6 34.5(2) . . . . ? C13 C14 C15 C16 2.1(2) . . . . ? Si6 C14 C15 C16 -167.57(15) . . . . ? Ti1 C14 C15 C16 66.00(14) . . . . ? C13 C14 C15 Ti1 -63.85(14) . . . . ? Si6 C14 C15 Ti1 126.43(17) . . . . ? C3 Ti1 C15 C16 -89.56(15) . . . . ? C2 Ti1 C15 C16 -40.40(17) . . . . ? Cl1 Ti1 C15 C16 72.76(12) . . . . ? C13 Ti1 C15 C16 -79.16(13) . . . . ? Cl2 Ti1 C15 C16 164.63(12) . . . . ? C12 Ti1 C15 C16 -37.47(12) . . . . ? C4 Ti1 C15 C16 -139.80(14) . . . . ? C1 Ti1 C15 C16 10.2(2) . . . . ? C14 Ti1 C15 C16 -116.95(17) . . . . ? C5 Ti1 C15 C16 118.4(3) . . . . ? C3 Ti1 C15 C14 27.38(17) . . . . ? C2 Ti1 C15 C14 76.55(16) . . . . ? Cl1 Ti1 C15 C14 -170.29(11) . . . . ? C13 Ti1 C15 C14 37.78(11) . . . . ? Cl2 Ti1 C15 C14 -78.42(11) . . . . ? C12 Ti1 C15 C14 79.47(13) . . . . ? C4 Ti1 C15 C14 -22.9(2) . . . . ? C1 Ti1 C15 C14 127.15(16) . . . . ? C16 Ti1 C15 C14 116.95(17) . . . . ? C5 Ti1 C15 C14 -124.7(3) . . . . ? C13 C12 C16 C15 2.0(2) . . . . ? Ti1 C12 C16 C15 -62.98(14) . . . . ? C13 C12 C16 Si5 -170.13(15) . . . . ? Ti1 C12 C16 Si5 124.91(15) . . . . ? C13 C12 C16 Ti1 64.95(14) . . . . ? C14 C15 C16 C12 -2.6(2) . . . . ? Ti1 C15 C16 C12 62.74(13) . . . . ? C14 C15 C16 Si5 168.86(15) . . . . ? Ti1 C15 C16 Si5 -125.84(17) . . . . ? C14 C15 C16 Ti1 -65.30(14) . . . . ? C17 Si5 C16 C12 -38.8(2) . . . . ? C19 Si5 C16 C12 -167.97(17) . . . . ? C18 Si5 C16 C12 76.48(19) . . . . ? C17 Si5 C16 C15 151.15(19) . . . . ? C19 Si5 C16 C15 21.9(2) . . . . ? C18 Si5 C16 C15 -93.6(2) . . . . ? C17 Si5 C16 Ti1 53.10(16) . . . . ? C19 Si5 C16 Ti1 -76.11(16) . . . . ? C18 Si5 C16 Ti1 168.34(13) . . . . ? C3 Ti1 C16 C12 2.98(16) . . . . ? C2 Ti1 C16 C12 35.81(14) . . . . ? Cl1 Ti1 C16 C12 141.01(12) . . . . ? C13 Ti1 C16 C12 -37.32(12) . . . . ? Cl2 Ti1 C16 C12 -132.95(11) . . . . ? C15 Ti1 C16 C12 -115.22(18) . . . . ? C4 Ti1 C16 C12 4.1(3) . . . . ? C1 Ti1 C16 C12 70.28(14) . . . . ? C14 Ti1 C16 C12 -78.25(13) . . . . ? C5 Ti1 C16 C12 85.40(18) . . . . ? C3 Ti1 C16 C15 118.20(13) . . . . ? C2 Ti1 C16 C15 151.03(13) . . . . ? Cl1 Ti1 C16 C15 -103.77(12) . . . . ? C13 Ti1 C16 C15 77.90(13) . . . . ? Cl2 Ti1 C16 C15 -17.73(13) . . . . ? C12 Ti1 C16 C15 115.22(18) . . . . ? C4 Ti1 C16 C15 119.3(2) . . . . ? C1 Ti1 C16 C15 -174.51(12) . . . . ? C14 Ti1 C16 C15 36.97(12) . . . . ? C5 Ti1 C16 C15 -159.39(13) . . . . ? C3 Ti1 C16 Si5 -115.13(14) . . . . ? C2 Ti1 C16 Si5 -82.31(15) . . . . ? Cl1 Ti1 C16 Si5 22.89(12) . . . . ? C13 Ti1 C16 Si5 -155.44(16) . . . . ? Cl2 Ti1 C16 Si5 108.94(12) . . . . ? C12 Ti1 C16 Si5 -118.12(19) . . . . ? C15 Ti1 C16 Si5 126.7(2) . . . . ? C4 Ti1 C16 Si5 -114.0(2) . . . . ? C1 Ti1 C16 Si5 -47.84(16) . . . . ? C14 Ti1 C16 Si5 163.63(16) . . . . ? C5 Ti1 C16 Si5 -32.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.424 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.067