# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Hayato Tsurugi' 'Haruki Nagae' 'Kazushi Mashima' _publ_contact_author_name 'Hayato Tsurugi' _publ_contact_author_email tsurugi@chem.es.osaka-u.ac.jp data_shelxl _database_code_depnum_ccdc_archive 'CCDC 811933' #TrackingRef '4126_web_deposit_cif_file_0_HayatoTsurugi_1297063279.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 3a _chemical_melting_point ? _chemical_formula_moiety 'C16 H17 Cl2 F6 N Si Ti' _chemical_formula_sum 'C16 H17 Cl2 F6 N Si Ti' _chemical_formula_weight 484.20 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 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 8.519(6) _cell_length_b 23.699(15) _cell_length_c 10.892(7) _cell_angle_alpha 90.00 _cell_angle_beta 110.026(7) _cell_angle_gamma 90.00 _cell_volume 2066(2) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 4144 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.784 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.7445 _exptl_absorpt_correction_T_max 0.8464 _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19168 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.45 _reflns_number_total 4645 _reflns_number_gt 3572 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ORTEP-III _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^)+(0.1235P)^2^+0.8152P] 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 4645 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.2014 _refine_ls_wR_factor_gt 0.1735 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _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 Ti1 Ti 0.85802(7) 0.05849(2) 0.65141(5) 0.0239(2) Uani 1 1 d . . . Cl1 Cl 1.08036(11) 0.10100(4) 0.62062(9) 0.0322(2) Uani 1 1 d . . . Cl2 Cl 0.68434(11) 0.03765(4) 0.44636(8) 0.0363(3) Uani 1 1 d . . . Si1 Si 0.65243(12) 0.17552(4) 0.60162(9) 0.0286(3) Uani 1 1 d . . . F1 F 0.3996(4) 0.05508(14) 0.9885(4) 0.0826(11) Uani 1 1 d . . . F2 F 0.3123(3) 0.13915(17) 0.9526(3) 0.0730(10) Uani 1 1 d . . . F3 F 0.4596(3) 0.11485(14) 1.1455(2) 0.0636(8) Uani 1 1 d . . . F4 F 1.1632(4) 0.1699(2) 1.1686(4) 0.1041(16) Uani 1 1 d . . . F5 F 1.0166(4) 0.18512(15) 1.2823(3) 0.0735(10) Uani 1 1 d . . . F6 F 1.0204(6) 0.24511(15) 1.1418(4) 0.1172(18) Uani 1 1 d . . . N1 N 0.7549(4) 0.11896(11) 0.7113(3) 0.0254(6) Uani 1 1 d . . . C1 C 0.7467(4) 0.12832(14) 0.8389(3) 0.0255(7) Uani 1 1 d . . . C2 C 0.6042(4) 0.11482(14) 0.8680(3) 0.0295(7) Uani 1 1 d . . . H1 H 0.4985 0.0952 0.7944 0.036 Uiso 1 1 d . . . C3 C 0.5993(4) 0.12448(15) 0.9925(3) 0.0319(7) Uani 1 1 d . . . C4 C 0.7331(4) 0.14864(15) 1.0898(3) 0.0306(7) Uani 1 1 d . . . H2 H 0.7301 0.1497 1.1776 0.037 Uiso 1 1 d . . . C5 C 0.8741(4) 0.16277(15) 1.0608(3) 0.0297(7) Uani 1 1 d . . . C6 C 0.8818(4) 0.15291(14) 0.9366(3) 0.0279(7) Uani 1 1 d . . . H3 H 0.9834 0.1632 0.9231 0.035 Uiso 1 1 d . . . C7 C 0.4452(5) 0.10842(19) 1.0215(4) 0.0421(9) Uani 1 1 d . . . C8 C 1.0172(5) 0.19119(17) 1.1617(4) 0.0384(9) Uani 1 1 d . . . C9 C 0.8203(5) 0.00454(15) 0.8191(4) 0.0365(8) Uani 1 1 d . . . H4 H 0.7380 0.0153 0.8628 0.045 Uiso 1 1 d . . . C10 C 0.9871(5) 0.02268(15) 0.8607(3) 0.0340(8) Uani 1 1 d . . . H5 H 1.0473 0.0527 0.9353 0.042 Uiso 1 1 d . . . C11 C 1.0639(5) -0.00426(16) 0.7801(4) 0.0378(9) Uani 1 1 d . . . H6 H 1.1904 -0.0002 0.7847 0.048 Uiso 1 1 d . . . C12 C 0.9441(5) -0.03721(15) 0.6892(4) 0.0392(9) Uani 1 1 d . . . H7 H 0.9674 -0.0586 0.6191 0.048 Uiso 1 1 d . . . C13 C 0.7924(5) -0.03186(16) 0.7120(4) 0.0404(9) Uani 1 1 d . . . H8 H 0.6810 -0.0530 0.6625 0.049 Uiso 1 1 d . . . C14 C 0.4253(5) 0.15860(18) 0.5336(4) 0.0422(9) Uani 1 1 d . . . H9 H 0.4108 0.1187 0.5084 0.051 Uiso 1 1 calc R . . H10 H 0.3718 0.1822 0.4566 0.051 Uiso 1 1 calc R . . H11 H 0.3739 0.1660 0.5998 0.051 Uiso 1 1 calc R . . C15 C 0.7350(5) 0.18529(17) 0.4658(4) 0.0411(9) Uani 1 1 d . . . H12 H 0.7744 0.1490 0.4445 0.049 Uiso 1 1 calc R . . H13 H 0.8279 0.2122 0.4924 0.049 Uiso 1 1 calc R . . H14 H 0.6461 0.1998 0.3888 0.049 Uiso 1 1 calc R . . C16 C 0.6888(5) 0.24198(15) 0.6991(4) 0.0370(8) Uani 1 1 d . . . H15 H 0.8187 0.2478 0.7405 0.045 Uiso 1 1 d . . . H16 H 0.6442 0.2368 0.7733 0.045 Uiso 1 1 d . . . H17 H 0.6419 0.2757 0.6425 0.045 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0243(4) 0.0281(3) 0.0200(3) -0.0010(2) 0.0083(3) -0.0016(2) Cl1 0.0292(5) 0.0350(5) 0.0364(5) -0.0003(3) 0.0163(4) -0.0036(3) Cl2 0.0340(5) 0.0474(5) 0.0242(4) -0.0063(3) 0.0056(4) -0.0015(4) Si1 0.0250(5) 0.0322(5) 0.0285(5) 0.0024(4) 0.0092(4) 0.0015(4) F1 0.081(2) 0.079(2) 0.118(3) -0.029(2) 0.073(2) -0.0397(18) F2 0.0292(14) 0.140(3) 0.0545(16) 0.0176(18) 0.0206(13) 0.0099(15) F3 0.0420(15) 0.125(3) 0.0300(13) -0.0062(14) 0.0198(11) -0.0181(15) F4 0.0309(16) 0.180(4) 0.092(3) -0.079(3) 0.0098(16) -0.0086(19) F5 0.0688(19) 0.115(3) 0.0347(14) -0.0217(15) 0.0153(13) -0.0399(18) F6 0.135(3) 0.0572(19) 0.093(3) 0.0130(17) -0.046(2) -0.055(2) N1 0.0258(14) 0.0303(14) 0.0215(13) 0.0009(10) 0.0098(11) -0.0016(11) C1 0.0283(17) 0.0275(15) 0.0214(15) -0.0009(12) 0.0092(13) 0.0001(13) C2 0.0282(18) 0.0323(17) 0.0286(17) -0.0020(13) 0.0105(14) -0.0037(13) C3 0.0258(18) 0.0421(19) 0.0287(18) -0.0012(14) 0.0106(14) -0.0013(14) C4 0.0297(19) 0.0407(19) 0.0218(16) -0.0039(13) 0.0094(14) 0.0022(14) C5 0.0267(18) 0.0332(17) 0.0280(17) -0.0074(13) 0.0076(14) -0.0027(13) C6 0.0256(17) 0.0306(17) 0.0291(17) -0.0017(13) 0.0114(14) -0.0021(13) C7 0.032(2) 0.067(3) 0.0301(19) -0.0073(17) 0.0148(16) -0.0101(18) C8 0.035(2) 0.049(2) 0.0308(19) -0.0097(16) 0.0110(16) -0.0083(17) C9 0.046(2) 0.0333(18) 0.037(2) 0.0098(15) 0.0231(18) 0.0021(16) C10 0.045(2) 0.0287(17) 0.0253(17) 0.0047(13) 0.0080(15) 0.0007(15) C11 0.037(2) 0.042(2) 0.0335(19) 0.0147(15) 0.0108(16) 0.0085(16) C12 0.055(3) 0.0297(18) 0.036(2) 0.0030(14) 0.0194(18) 0.0095(17) C13 0.047(2) 0.0294(18) 0.043(2) 0.0059(15) 0.0125(18) -0.0055(16) C14 0.030(2) 0.047(2) 0.044(2) -0.0041(17) 0.0057(18) -0.0015(16) C15 0.044(2) 0.046(2) 0.035(2) 0.0173(16) 0.0163(18) 0.0102(17) C16 0.035(2) 0.0300(18) 0.044(2) 0.0007(15) 0.0113(17) 0.0030(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N1 1.909(3) . ? Ti1 Cl1 2.2695(15) . ? Ti1 Cl2 2.2711(15) . ? Ti1 C10 2.326(4) . ? Ti1 C9 2.340(4) . ? Ti1 C11 2.360(4) . ? Ti1 C13 2.363(4) . ? Ti1 C12 2.376(4) . ? Si1 N1 1.809(3) . ? Si1 C15 1.857(4) . ? Si1 C14 1.863(4) . ? Si1 C16 1.865(4) . ? F1 C7 1.335(5) . ? F2 C7 1.340(5) . ? F3 C7 1.322(5) . ? F4 C8 1.319(5) . ? F5 C8 1.324(5) . ? F6 C8 1.298(5) . ? N1 C1 1.432(4) . ? C1 C2 1.393(5) . ? C1 C6 1.399(5) . ? C2 C3 1.390(5) . ? C3 C4 1.387(5) . ? C3 C7 1.501(5) . ? C4 C5 1.384(5) . ? C5 C6 1.396(5) . ? C5 C8 1.493(5) . ? C9 C10 1.403(6) . ? C9 C13 1.404(5) . ? C10 C11 1.414(5) . ? C11 C12 1.392(6) . ? C12 C13 1.403(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ti1 Cl1 102.84(10) . . ? N1 Ti1 Cl2 106.16(9) . . ? Cl1 Ti1 Cl2 104.29(6) . . ? N1 Ti1 C10 93.29(13) . . ? Cl1 Ti1 C10 99.69(11) . . ? Cl2 Ti1 C10 144.56(10) . . ? N1 Ti1 C9 86.63(13) . . ? Cl1 Ti1 C9 134.62(11) . . ? Cl2 Ti1 C9 115.56(11) . . ? C10 Ti1 C9 34.99(14) . . ? N1 Ti1 C11 127.26(13) . . ? Cl1 Ti1 C11 83.07(11) . . ? Cl2 Ti1 C11 123.27(11) . . ? C10 Ti1 C11 35.12(13) . . ? C9 Ti1 C11 57.64(13) . . ? N1 Ti1 C13 113.85(14) . . ? Cl1 Ti1 C13 137.11(11) . . ? Cl2 Ti1 C13 86.61(11) . . ? C10 Ti1 C13 58.23(14) . . ? C9 Ti1 C13 34.74(13) . . ? C11 Ti1 C13 57.44(15) . . ? N1 Ti1 C12 143.94(13) . . ? Cl1 Ti1 C12 103.04(11) . . ? Cl2 Ti1 C12 91.23(11) . . ? C10 Ti1 C12 57.83(13) . . ? C9 Ti1 C12 57.31(13) . . ? C11 Ti1 C12 34.20(14) . . ? C13 Ti1 C12 34.43(15) . . ? N1 Si1 C15 112.93(16) . . ? N1 Si1 C14 107.70(17) . . ? C15 Si1 C14 109.6(2) . . ? N1 Si1 C16 107.53(16) . . ? C15 Si1 C16 108.28(19) . . ? C14 Si1 C16 110.85(18) . . ? C1 N1 Si1 110.7(2) . . ? C1 N1 Ti1 129.0(2) . . ? Si1 N1 Ti1 120.35(15) . . ? C2 C1 C6 118.4(3) . . ? C2 C1 N1 121.4(3) . . ? C6 C1 N1 120.1(3) . . ? C3 C2 C1 120.2(3) . . ? C4 C3 C2 121.5(3) . . ? C4 C3 C7 119.5(3) . . ? C2 C3 C7 119.0(3) . . ? C5 C4 C3 118.4(3) . . ? C4 C5 C6 120.9(3) . . ? C4 C5 C8 119.7(3) . . ? C6 C5 C8 119.4(3) . . ? C5 C6 C1 120.5(3) . . ? F3 C7 F1 107.5(4) . . ? F3 C7 F2 105.9(3) . . ? F1 C7 F2 104.6(4) . . ? F3 C7 C3 113.9(3) . . ? F1 C7 C3 112.2(3) . . ? F2 C7 C3 112.1(3) . . ? F6 C8 F4 108.2(4) . . ? F6 C8 F5 106.3(4) . . ? F4 C8 F5 103.0(4) . . ? F6 C8 C5 112.3(3) . . ? F4 C8 C5 112.7(3) . . ? F5 C8 C5 113.7(3) . . ? C10 C9 C13 108.7(3) . . ? C10 C9 Ti1 71.9(2) . . ? C13 C9 Ti1 73.5(2) . . ? C9 C10 C11 107.1(3) . . ? C9 C10 Ti1 73.1(2) . . ? C11 C10 Ti1 73.8(2) . . ? C12 C11 C10 108.2(3) . . ? C12 C11 Ti1 73.5(2) . . ? C10 C11 Ti1 71.1(2) . . ? C11 C12 C13 108.6(3) . . ? C11 C12 Ti1 72.3(2) . . ? C13 C12 Ti1 72.3(2) . . ? C12 C13 C9 107.4(4) . . ? C12 C13 Ti1 73.3(2) . . ? C9 C13 Ti1 71.7(2) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.036 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.184 # Attachment '4127_web_deposit_cif_file_1_HayatoTsurugi_1297063279.cif' data_3b _database_code_depnum_ccdc_archive 'CCDC 811934' #TrackingRef '4127_web_deposit_cif_file_1_HayatoTsurugi_1297063279.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 3b _chemical_melting_point ? _chemical_formula_moiety 'C21 H27 Cl2 F6 N Si Ti' _chemical_formula_sum 'C21 H27 Cl2 F6 N Si Ti' _chemical_formula_weight 554.33 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9074(9) _cell_length_b 14.6224(16) _cell_length_c 38.661(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.014(7) _cell_angle_gamma 90.00 _cell_volume 5034.7(10) _cell_formula_units_Z 8 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 5493 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 27.42 _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 0.654 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.8537 _exptl_absorpt_correction_T_max 0.9557 _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45285 _diffrn_reflns_av_R_equivalents 0.1669 _diffrn_reflns_av_sigmaI/netI 0.1719 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.46 _reflns_number_total 11349 _reflns_number_gt 5755 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ORTEP-III _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^)+(0.1517P)^2^+17.5068P] 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 11349 _refine_ls_number_parameters 593 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2123 _refine_ls_R_factor_gt 0.1166 _refine_ls_wR_factor_ref 0.3618 _refine_ls_wR_factor_gt 0.2918 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 Ti1 Ti 0.99622(18) 0.19803(10) 0.53993(4) 0.0256(4) Uani 1 1 d . . . Ti2 Ti 0.49291(17) 0.25295(11) 0.21218(4) 0.0261(4) Uani 1 1 d . . . Cl1 Cl 1.1681(3) 0.2953(2) 0.56274(7) 0.0499(7) Uani 1 1 d . . . Cl2 Cl 1.1381(3) 0.06999(17) 0.53242(7) 0.0425(6) Uani 1 1 d . . . Cl3 Cl 0.7190(3) 0.29156(19) 0.19086(6) 0.0431(6) Uani 1 1 d . . . Cl4 Cl 0.5165(3) 0.09778(15) 0.21907(6) 0.0384(6) Uani 1 1 d . . . Si1 Si 1.1337(3) 0.29208(17) 0.47217(7) 0.0300(6) Uani 1 1 d . . . Si2 Si 0.6858(3) 0.30624(19) 0.28123(7) 0.0333(6) Uani 1 1 d . . . F1 F 0.5656(8) 0.0455(4) 0.42751(17) 0.0587(18) Uani 1 1 d . . . F2 F 0.7353(7) 0.0676(5) 0.39097(18) 0.0631(19) Uani 1 1 d . . . F3 F 0.5156(7) 0.1287(4) 0.38350(16) 0.0565(17) Uani 1 1 d . . . F4 F 0.4689(9) 0.4421(5) 0.4162(2) 0.092(3) Uani 1 1 d . . . F5 F 0.6868(9) 0.5001(5) 0.4209(3) 0.105(3) Uani 1 1 d . . . F6 F 0.5556(10) 0.4840(5) 0.46481(18) 0.079(2) Uani 1 1 d . . . F7 F 0.1437(8) 0.5128(4) 0.31774(17) 0.0628(19) Uani 1 1 d . . . F8 F 0.2539(9) 0.4729(6) 0.3644(2) 0.103(3) Uani 1 1 d . . . F9 F 0.0253(9) 0.4364(5) 0.3544(2) 0.078(2) Uani 1 1 d . . . F10 F 0.1040(7) 0.0541(4) 0.29798(15) 0.0521(16) Uani 1 1 d . . . F11 F 0.2427(6) 0.0550(4) 0.34434(18) 0.0564(18) Uani 1 1 d . . . F12 F 0.0206(6) 0.1093(4) 0.34522(15) 0.0454(15) Uani 1 1 d . . . N1 N 0.9720(8) 0.2466(4) 0.49352(17) 0.0239(15) Uani 1 1 d . . . N2 N 0.5045(8) 0.2898(5) 0.25993(18) 0.0254(16) Uani 1 1 d . . . C1 C 0.8423(10) 0.2559(6) 0.4708(2) 0.0280(19) Uani 1 1 d . . . C2 C 0.7920(10) 0.1803(6) 0.4510(2) 0.0270(19) Uani 1 1 d . . . H2 H 0.8387 0.1224 0.4539 0.032 Uiso 1 1 calc R . . C3 C 0.6753(10) 0.1905(6) 0.4274(2) 0.030(2) Uani 1 1 d . . . C4 C 0.6087(10) 0.2762(6) 0.4214(2) 0.029(2) Uani 1 1 d . . . H4 H 0.5321 0.2840 0.4043 0.035 Uiso 1 1 calc R . . C5 C 0.6594(11) 0.3495(6) 0.4416(2) 0.032(2) Uani 1 1 d . . . C6 C 0.7754(10) 0.3399(6) 0.4655(2) 0.0275(19) Uani 1 1 d . . . H6 H 0.8094 0.3915 0.4784 0.033 Uiso 1 1 calc R . . C7 C 0.6228(11) 0.1088(7) 0.4078(3) 0.039(2) Uani 1 1 d . . . C8 C 0.5929(12) 0.4440(7) 0.4354(3) 0.042(3) Uani 1 1 d . . . C9 C 0.7518(10) 0.2440(6) 0.5588(2) 0.030(2) Uani 1 1 d . . . C10 C 0.8504(10) 0.2467(6) 0.5878(2) 0.028(2) Uani 1 1 d . . . C11 C 0.9039(10) 0.1561(6) 0.5955(2) 0.0283(19) Uani 1 1 d . . . C12 C 0.8354(10) 0.0956(6) 0.5704(2) 0.0268(19) Uani 1 1 d . . . C13 C 0.7413(9) 0.1486(6) 0.5477(2) 0.0255(19) Uani 1 1 d . . . C14 C 0.6565(11) 0.3193(6) 0.5459(3) 0.036(2) Uani 1 1 d . . . H14A H 0.7162 0.3755 0.5447 0.043 Uiso 1 1 calc R . . H14B H 0.5728 0.3286 0.5617 0.043 Uiso 1 1 calc R . . H14C H 0.6170 0.3041 0.5228 0.043 Uiso 1 1 calc R . . C15 C 0.8791(12) 0.3310(7) 0.6088(3) 0.040(2) Uani 1 1 d . . . H15A H 0.7954 0.3409 0.6245 0.048 Uiso 1 1 calc R . . H15B H 0.8883 0.3837 0.5933 0.048 Uiso 1 1 calc R . . H15C H 0.9723 0.3236 0.6223 0.048 Uiso 1 1 calc R . . C16 C 1.0108(10) 0.1304(6) 0.6238(2) 0.035(2) Uani 1 1 d . . . H16A H 1.0693 0.1842 0.6308 0.042 Uiso 1 1 calc R . . H16B H 1.0787 0.0827 0.6156 0.042 Uiso 1 1 calc R . . H16C H 0.9548 0.1074 0.6436 0.042 Uiso 1 1 calc R . . C17 C 0.8464(11) -0.0071(6) 0.5700(3) 0.035(2) Uani 1 1 d . . . H17A H 0.9409 -0.0261 0.5812 0.042 Uiso 1 1 calc R . . H17B H 0.8436 -0.0289 0.5460 0.042 Uiso 1 1 calc R . . H17C H 0.7618 -0.0332 0.5825 0.042 Uiso 1 1 calc R . . C18 C 0.6336(10) 0.1087(7) 0.5218(2) 0.032(2) Uani 1 1 d . . . H18A H 0.5413 0.0907 0.5334 0.039 Uiso 1 1 calc R . . H18B H 0.6790 0.0549 0.5111 0.039 Uiso 1 1 calc R . . H18C H 0.6100 0.1543 0.5040 0.039 Uiso 1 1 calc R . . C19 C 1.1470(11) 0.4183(7) 0.4814(3) 0.044(3) Uani 1 1 d . . . H19A H 1.1331 0.4290 0.5062 0.053 Uiso 1 1 calc R . . H19B H 1.0688 0.4508 0.4682 0.053 Uiso 1 1 calc R . . H19C H 1.2460 0.4408 0.4747 0.053 Uiso 1 1 calc R . . C20 C 1.3111(10) 0.2324(7) 0.4838(3) 0.038(2) Uani 1 1 d . . . H20A H 1.3078 0.1698 0.4748 0.046 Uiso 1 1 calc R . . H20B H 1.3234 0.2307 0.5090 0.046 Uiso 1 1 calc R . . H20C H 1.3959 0.2652 0.4738 0.046 Uiso 1 1 calc R . . C21 C 1.1058(11) 0.2730(7) 0.4246(2) 0.038(2) Uani 1 1 d . . . H21A H 1.0195 0.3088 0.4163 0.045 Uiso 1 1 calc R . . H21B H 1.0872 0.2079 0.4203 0.045 Uiso 1 1 calc R . . H21C H 1.1960 0.2922 0.4125 0.045 Uiso 1 1 calc R . . C22 C 0.3843(10) 0.2871(6) 0.2835(2) 0.0286(19) Uani 1 1 d . . . C23 C 0.3308(11) 0.3646(6) 0.2991(2) 0.033(2) Uani 1 1 d . . . H23 H 0.3727 0.4225 0.2937 0.040 Uiso 1 1 calc R . . C24 C 0.2157(11) 0.3590(6) 0.3228(2) 0.030(2) Uani 1 1 d . . . C25 C 0.1508(10) 0.2745(6) 0.3315(2) 0.029(2) Uani 1 1 d . . . H25 H 0.0700 0.2716 0.3471 0.034 Uiso 1 1 calc R . . C26 C 0.2067(9) 0.1963(5) 0.3168(2) 0.0240(18) Uani 1 1 d . . . C27 C 0.3231(10) 0.2022(6) 0.2928(2) 0.030(2) Uani 1 1 d . . . H27 H 0.3611 0.1478 0.2827 0.036 Uiso 1 1 calc R . . C28 C 0.1604(12) 0.4450(7) 0.3405(3) 0.039(2) Uani 1 1 d . . . C29 C 0.1415(11) 0.1049(6) 0.3258(2) 0.034(2) Uani 1 1 d . . . C30 C 0.2534(10) 0.3235(6) 0.2033(2) 0.030(2) Uani 1 1 d . . . C31 C 0.2426(11) 0.2328(7) 0.1923(3) 0.042(3) Uani 1 1 d . . . C32 C 0.3335(12) 0.2210(7) 0.1630(3) 0.040(2) Uani 1 1 d . . . C33 C 0.4047(11) 0.3051(7) 0.1566(2) 0.039(2) Uani 1 1 d . . . C34 C 0.3584(10) 0.3687(6) 0.1820(2) 0.035(2) Uani 1 1 d . . . C35 C 0.1473(12) 0.3684(9) 0.2288(3) 0.055(3) Uani 1 1 d . . . H35A H 0.0582 0.3911 0.2164 0.066 Uiso 1 1 calc R . . H35B H 0.1987 0.4195 0.2404 0.066 Uiso 1 1 calc R . . H35C H 0.1170 0.3233 0.2461 0.066 Uiso 1 1 calc R . . C36 C 0.1370(13) 0.1620(9) 0.2061(4) 0.065(4) Uani 1 1 d . . . H36A H 0.0336 0.1782 0.1995 0.078 Uiso 1 1 calc R . . H36B H 0.1468 0.1597 0.2314 0.078 Uiso 1 1 calc R . . H36C H 0.1618 0.1021 0.1964 0.078 Uiso 1 1 calc R . . C37 C 0.3564(15) 0.1370(9) 0.1415(3) 0.070(4) Uani 1 1 d . . . H37A H 0.4609 0.1346 0.1340 0.083 Uiso 1 1 calc R . . H37B H 0.2893 0.1390 0.1211 0.083 Uiso 1 1 calc R . . H37C H 0.3341 0.0826 0.1552 0.083 Uiso 1 1 calc R . . C38 C 0.5002(15) 0.3273(10) 0.1254(3) 0.068(4) Uani 1 1 d . . . H38A H 0.4348 0.3456 0.1059 0.082 Uiso 1 1 calc R . . H38B H 0.5582 0.2732 0.1189 0.082 Uiso 1 1 calc R . . H38C H 0.5690 0.3776 0.1312 0.082 Uiso 1 1 calc R . . C39 C 0.3985(14) 0.4670(7) 0.1856(3) 0.058(3) Uani 1 1 d . . . H39A H 0.3237 0.5044 0.1732 0.070 Uiso 1 1 calc R . . H39B H 0.4977 0.4776 0.1758 0.070 Uiso 1 1 calc R . . H39C H 0.4006 0.4838 0.2101 0.070 Uiso 1 1 calc R . . C40 C 0.7765(11) 0.4125(7) 0.2678(3) 0.044(3) Uani 1 1 d . . . H40A H 0.7832 0.4138 0.2426 0.053 Uiso 1 1 calc R . . H40B H 0.8776 0.4158 0.2782 0.053 Uiso 1 1 calc R . . H40C H 0.7171 0.4649 0.2756 0.053 Uiso 1 1 calc R . . C41 C 0.6599(13) 0.3139(11) 0.3291(3) 0.069(4) Uani 1 1 d . . . H41A H 0.5964 0.2633 0.3367 0.083 Uiso 1 1 calc R . . H41B H 0.6118 0.3722 0.3347 0.083 Uiso 1 1 calc R . . H41C H 0.7579 0.3103 0.3409 0.083 Uiso 1 1 calc R . . C42 C 0.8046(11) 0.2033(7) 0.2735(3) 0.049(3) Uani 1 1 d . . . H42A H 0.8167 0.1947 0.2486 0.059 Uiso 1 1 calc R . . H42B H 0.7561 0.1493 0.2833 0.059 Uiso 1 1 calc R . . H42C H 0.9034 0.2120 0.2846 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 0.0298(9) 0.0213(8) 0.0258(8) -0.0005(6) -0.0001(7) 0.0001(7) Ti2 0.0308(9) 0.0219(8) 0.0255(8) 0.0010(6) -0.0002(7) 0.0011(7) Cl1 0.0463(15) 0.0683(19) 0.0350(13) -0.0105(12) 0.0003(11) -0.0245(14) Cl2 0.0457(15) 0.0362(13) 0.0460(14) 0.0106(11) 0.0131(12) 0.0172(11) Cl3 0.0327(13) 0.0620(17) 0.0348(13) 0.0017(12) 0.0029(10) -0.0002(12) Cl4 0.0444(14) 0.0248(12) 0.0457(14) -0.0029(10) -0.0082(11) 0.0072(10) Si1 0.0305(14) 0.0279(13) 0.0315(13) 0.0015(11) 0.0004(11) -0.0037(11) Si2 0.0292(14) 0.0411(16) 0.0297(13) 0.0002(11) -0.0013(11) -0.0049(12) F1 0.078(5) 0.032(3) 0.065(4) 0.003(3) -0.008(4) -0.025(3) F2 0.052(4) 0.065(4) 0.072(5) -0.039(4) -0.006(3) 0.003(3) F3 0.070(4) 0.046(4) 0.052(4) -0.010(3) -0.030(3) 0.002(3) F4 0.091(5) 0.047(4) 0.135(7) -0.012(4) -0.080(5) 0.024(4) F5 0.089(6) 0.043(4) 0.184(10) 0.054(5) 0.043(6) 0.009(4) F6 0.125(7) 0.048(4) 0.063(5) -0.007(3) -0.016(4) 0.049(4) F7 0.097(5) 0.028(3) 0.064(4) 0.002(3) 0.024(4) 0.019(3) F8 0.109(6) 0.085(6) 0.112(7) -0.079(5) -0.064(5) 0.054(5) F9 0.088(5) 0.044(4) 0.104(6) -0.008(4) 0.051(5) 0.009(4) F10 0.074(4) 0.036(3) 0.047(4) -0.005(3) 0.005(3) -0.019(3) F11 0.045(4) 0.042(4) 0.082(5) 0.036(3) -0.011(3) 0.000(3) F12 0.040(3) 0.041(3) 0.055(4) 0.004(3) 0.023(3) -0.002(3) N1 0.029(4) 0.019(4) 0.023(4) -0.001(3) -0.006(3) -0.002(3) N2 0.024(4) 0.018(4) 0.033(4) 0.004(3) 0.003(3) -0.001(3) C1 0.028(5) 0.025(5) 0.032(5) 0.004(4) 0.002(4) -0.006(4) C2 0.032(5) 0.020(4) 0.029(5) -0.001(3) 0.000(4) 0.007(4) C3 0.027(5) 0.033(5) 0.030(5) 0.005(4) -0.006(4) -0.009(4) C4 0.035(5) 0.018(4) 0.035(5) 0.006(4) -0.001(4) 0.003(4) C5 0.044(6) 0.026(5) 0.025(4) 0.006(4) 0.007(4) -0.003(4) C6 0.036(5) 0.022(4) 0.025(4) -0.003(4) 0.008(4) -0.003(4) C7 0.041(6) 0.033(5) 0.042(6) -0.015(5) -0.005(5) -0.001(5) C8 0.043(6) 0.023(5) 0.059(7) 0.005(5) -0.012(5) 0.004(5) C9 0.033(5) 0.031(5) 0.026(5) -0.007(4) 0.001(4) 0.004(4) C10 0.034(5) 0.025(5) 0.025(4) -0.013(4) 0.008(4) -0.004(4) C11 0.030(5) 0.031(5) 0.024(4) -0.004(4) 0.001(4) -0.003(4) C12 0.034(5) 0.024(4) 0.022(4) -0.005(3) 0.001(4) -0.005(4) C13 0.024(4) 0.026(5) 0.027(4) -0.004(4) 0.007(4) 0.005(4) C14 0.038(5) 0.027(5) 0.044(6) 0.010(4) 0.013(4) 0.015(4) C15 0.049(6) 0.034(5) 0.038(5) -0.016(4) 0.006(5) -0.006(5) C16 0.034(5) 0.028(5) 0.042(6) -0.002(4) -0.007(4) 0.000(4) C17 0.040(6) 0.027(5) 0.037(5) 0.002(4) -0.003(4) -0.005(4) C18 0.027(5) 0.039(5) 0.031(5) 0.008(4) -0.004(4) -0.009(4) C19 0.037(6) 0.036(6) 0.061(7) 0.004(5) 0.016(5) -0.014(5) C20 0.036(5) 0.031(5) 0.048(6) -0.001(4) 0.012(5) 0.004(4) C21 0.029(5) 0.056(6) 0.029(5) 0.008(4) 0.004(4) 0.006(5) C22 0.029(5) 0.033(5) 0.025(4) 0.000(4) 0.009(4) 0.005(4) C23 0.046(6) 0.021(5) 0.033(5) -0.010(4) 0.001(4) 0.003(4) C24 0.044(6) 0.016(4) 0.031(5) -0.006(3) -0.004(4) 0.005(4) C25 0.031(5) 0.034(5) 0.021(4) -0.002(4) 0.001(4) -0.003(4) C26 0.027(5) 0.016(4) 0.029(4) -0.002(3) 0.000(4) 0.001(4) C27 0.034(5) 0.028(5) 0.029(5) 0.002(4) 0.001(4) 0.002(4) C28 0.042(6) 0.030(5) 0.045(6) -0.008(5) 0.010(5) 0.006(5) C29 0.039(5) 0.032(5) 0.031(5) 0.005(4) -0.001(4) 0.004(4) C30 0.031(5) 0.038(5) 0.022(4) 0.004(4) 0.002(4) 0.013(4) C31 0.034(5) 0.045(6) 0.045(6) 0.006(5) -0.014(5) -0.011(5) C32 0.053(6) 0.034(5) 0.033(5) -0.006(4) -0.014(5) 0.010(5) C33 0.042(6) 0.056(7) 0.019(4) 0.001(4) -0.005(4) 0.007(5) C34 0.034(5) 0.030(5) 0.040(6) 0.004(4) -0.002(4) 0.003(4) C35 0.042(6) 0.093(9) 0.029(5) -0.003(6) -0.005(5) 0.031(6) C36 0.047(7) 0.061(8) 0.087(10) 0.037(7) -0.022(7) -0.012(6) C37 0.089(10) 0.053(8) 0.066(8) -0.021(6) -0.032(7) 0.025(7) C38 0.067(8) 0.108(11) 0.029(6) 0.019(7) -0.003(6) 0.000(8) C39 0.072(8) 0.041(7) 0.062(8) 0.012(6) -0.018(6) 0.001(6) C40 0.038(6) 0.036(6) 0.057(7) -0.011(5) 0.000(5) -0.007(5) C41 0.046(7) 0.125(13) 0.035(6) -0.006(7) -0.012(5) -0.010(7) C42 0.028(5) 0.038(6) 0.080(8) 0.012(6) -0.017(5) -0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N1 1.938(7) . ? Ti1 Cl1 2.257(3) . ? Ti1 Cl2 2.280(3) . ? Ti1 C10 2.390(8) . ? Ti1 C11 2.394(9) . ? Ti1 C12 2.395(9) . ? Ti1 C9 2.404(9) . ? Ti1 C13 2.407(9) . ? Ti2 N2 1.924(7) . ? Ti2 Cl3 2.261(3) . ? Ti2 Cl4 2.294(3) . ? Ti2 C31 2.364(9) . ? Ti2 C34 2.369(9) . ? Ti2 C30 2.389(9) . ? Ti2 C33 2.399(9) . ? Ti2 C32 2.400(9) . ? Si1 N1 1.800(7) . ? Si1 C20 1.853(10) . ? Si1 C21 1.871(9) . ? Si1 C19 1.883(10) . ? Si2 N2 1.815(7) . ? Si2 C40 1.831(10) . ? Si2 C42 1.867(11) . ? Si2 C41 1.873(11) . ? F1 C7 1.308(12) . ? F2 C7 1.346(11) . ? F3 C7 1.359(11) . ? F4 C8 1.320(11) . ? F5 C8 1.304(12) . ? F6 C8 1.327(13) . ? F7 C28 1.332(12) . ? F8 C28 1.301(12) . ? F9 C28 1.334(12) . ? F10 C29 1.346(11) . ? F11 C29 1.354(10) . ? F12 C29 1.324(11) . ? N1 C1 1.445(10) . ? N2 C22 1.419(11) . ? C1 C6 1.379(12) . ? C1 C2 1.413(12) . ? C2 C3 1.378(12) . ? C2 H2 0.9500 . ? C3 C4 1.403(12) . ? C3 C7 1.487(12) . ? C4 C5 1.397(12) . ? C4 H4 0.9500 . ? C5 C6 1.381(12) . ? C5 C8 1.521(13) . ? C6 H6 0.9500 . ? C9 C10 1.415(12) . ? C9 C13 1.462(12) . ? C9 C14 1.472(12) . ? C10 C11 1.438(13) . ? C10 C15 1.494(12) . ? C11 C12 1.441(11) . ? C11 C16 1.484(12) . ? C12 C13 1.430(12) . ? C12 C17 1.506(12) . ? C13 C18 1.492(12) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 C23 1.374(12) . ? C22 C27 1.406(12) . ? C23 C24 1.389(13) . ? C23 H23 0.9500 . ? C24 C25 1.407(12) . ? C24 C28 1.517(12) . ? C25 C26 1.375(12) . ? C25 H25 0.9500 . ? C26 C27 1.405(12) . ? C26 C29 1.501(12) . ? C27 H27 0.9500 . ? C30 C31 1.396(14) . ? C30 C34 1.421(13) . ? C30 C35 1.527(13) . ? C31 C32 1.415(15) . ? C31 C36 1.503(15) . ? C32 C33 1.408(14) . ? C32 C37 1.498(14) . ? C33 C34 1.418(13) . ? C33 C38 1.525(14) . ? C34 C39 1.488(14) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 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 N1 Ti1 Cl1 101.2(2) . . ? N1 Ti1 Cl2 103.6(2) . . ? Cl1 Ti1 Cl2 101.14(12) . . ? N1 Ti1 C10 123.7(3) . . ? Cl1 Ti1 C10 83.3(2) . . ? Cl2 Ti1 C10 130.8(2) . . ? N1 Ti1 C11 152.9(3) . . ? Cl1 Ti1 C11 93.0(2) . . ? Cl2 Ti1 C11 95.9(2) . . ? C10 Ti1 C11 35.0(3) . . ? N1 Ti1 C12 128.8(3) . . ? Cl1 Ti1 C12 127.5(2) . . ? Cl2 Ti1 C12 83.5(2) . . ? C10 Ti1 C12 57.8(3) . . ? C11 Ti1 C12 35.0(3) . . ? N1 Ti1 C9 95.3(3) . . ? Cl1 Ti1 C9 108.5(2) . . ? Cl2 Ti1 C9 140.8(2) . . ? C10 Ti1 C9 34.3(3) . . ? C11 Ti1 C9 58.1(3) . . ? C12 Ti1 C9 58.2(3) . . ? N1 Ti1 C13 97.8(3) . . ? Cl1 Ti1 C13 140.8(2) . . ? Cl2 Ti1 C13 107.2(2) . . ? C10 Ti1 C13 57.7(3) . . ? C11 Ti1 C13 58.1(3) . . ? C12 Ti1 C13 34.7(3) . . ? C9 Ti1 C13 35.4(3) . . ? N2 Ti2 Cl3 104.3(2) . . ? N2 Ti2 Cl4 99.3(2) . . ? Cl3 Ti2 Cl4 102.07(11) . . ? N2 Ti2 C31 112.4(3) . . ? Cl3 Ti2 C31 138.9(3) . . ? Cl4 Ti2 C31 89.9(3) . . ? N2 Ti2 C34 106.9(3) . . ? Cl3 Ti2 C34 95.1(2) . . ? Cl4 Ti2 C34 143.9(2) . . ? C31 Ti2 C34 57.5(3) . . ? N2 Ti2 C30 92.8(3) . . ? Cl3 Ti2 C30 129.7(2) . . ? Cl4 Ti2 C30 121.6(3) . . ? C31 Ti2 C30 34.1(3) . . ? C34 Ti2 C30 34.7(3) . . ? N2 Ti2 C33 141.4(3) . . ? Cl3 Ti2 C33 82.8(3) . . ? Cl4 Ti2 C33 116.5(3) . . ? C31 Ti2 C33 57.0(4) . . ? C34 Ti2 C33 34.6(3) . . ? C30 Ti2 C33 57.1(3) . . ? N2 Ti2 C32 146.7(3) . . ? Cl3 Ti2 C32 106.1(3) . . ? Cl4 Ti2 C32 87.2(2) . . ? C31 Ti2 C32 34.5(4) . . ? C34 Ti2 C32 57.4(3) . . ? C30 Ti2 C32 57.1(3) . . ? C33 Ti2 C32 34.1(3) . . ? N1 Si1 C20 113.6(4) . . ? N1 Si1 C21 107.6(4) . . ? C20 Si1 C21 105.4(5) . . ? N1 Si1 C19 108.8(4) . . ? C20 Si1 C19 111.4(5) . . ? C21 Si1 C19 109.9(5) . . ? N2 Si2 C40 112.2(4) . . ? N2 Si2 C42 108.8(4) . . ? C40 Si2 C42 112.6(5) . . ? N2 Si2 C41 109.4(4) . . ? C40 Si2 C41 107.0(6) . . ? C42 Si2 C41 106.6(6) . . ? C1 N1 Si1 108.9(5) . . ? C1 N1 Ti1 132.2(5) . . ? Si1 N1 Ti1 118.9(4) . . ? C22 N2 Si2 112.8(6) . . ? C22 N2 Ti2 125.4(6) . . ? Si2 N2 Ti2 120.3(4) . . ? C6 C1 C2 118.9(8) . . ? C6 C1 N1 120.9(8) . . ? C2 C1 N1 119.9(8) . . ? C3 C2 C1 120.1(8) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 121.2(8) . . ? C2 C3 C7 118.5(8) . . ? C4 C3 C7 120.3(8) . . ? C5 C4 C3 117.4(8) . . ? C5 C4 H4 121.3 . . ? C3 C4 H4 121.3 . . ? C6 C5 C4 121.8(8) . . ? C6 C5 C8 118.9(8) . . ? C4 C5 C8 119.1(8) . . ? C1 C6 C5 120.4(8) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? F1 C7 F2 105.4(8) . . ? F1 C7 F3 106.2(8) . . ? F2 C7 F3 106.4(8) . . ? F1 C7 C3 113.1(8) . . ? F2 C7 C3 112.1(8) . . ? F3 C7 C3 113.0(8) . . ? F5 C8 F4 108.0(10) . . ? F5 C8 F6 105.3(9) . . ? F4 C8 F6 105.8(9) . . ? F5 C8 C5 112.8(9) . . ? F4 C8 C5 112.9(8) . . ? F6 C8 C5 111.5(8) . . ? C10 C9 C13 107.2(8) . . ? C10 C9 C14 126.4(8) . . ? C13 C9 C14 125.5(8) . . ? C10 C9 Ti1 72.3(5) . . ? C13 C9 Ti1 72.4(5) . . ? C14 C9 Ti1 128.8(6) . . ? C9 C10 C11 109.6(7) . . ? C9 C10 C15 123.5(8) . . ? C11 C10 C15 126.6(8) . . ? C9 C10 Ti1 73.4(5) . . ? C11 C10 Ti1 72.7(5) . . ? C15 C10 Ti1 125.2(6) . . ? C10 C11 C12 107.0(7) . . ? C10 C11 C16 126.2(8) . . ? C12 C11 C16 126.9(8) . . ? C10 C11 Ti1 72.3(5) . . ? C12 C11 Ti1 72.5(5) . . ? C16 C11 Ti1 120.0(6) . . ? C13 C12 C11 108.5(8) . . ? C13 C12 C17 124.9(8) . . ? C11 C12 C17 126.3(8) . . ? C13 C12 Ti1 73.1(5) . . ? C11 C12 Ti1 72.4(5) . . ? C17 C12 Ti1 125.4(6) . . ? C12 C13 C9 107.6(7) . . ? C12 C13 C18 124.2(8) . . ? C9 C13 C18 127.4(8) . . ? C12 C13 Ti1 72.2(5) . . ? C9 C13 Ti1 72.2(5) . . ? C18 C13 Ti1 129.1(6) . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si1 C21 H21A 109.5 . . ? Si1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C27 118.5(8) . . ? C23 C22 N2 122.1(8) . . ? C27 C22 N2 119.3(8) . . ? C22 C23 C24 120.5(9) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C25 121.3(8) . . ? C23 C24 C28 119.8(8) . . ? C25 C24 C28 118.9(8) . . ? C26 C25 C24 118.6(8) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C25 C26 C27 119.9(8) . . ? C25 C26 C29 120.0(8) . . ? C27 C26 C29 120.1(8) . . ? C26 C27 C22 121.1(8) . . ? C26 C27 H27 119.4 . . ? C22 C27 H27 119.4 . . ? F8 C28 F7 107.4(9) . . ? F8 C28 F9 108.2(9) . . ? F7 C28 F9 104.3(8) . . ? F8 C28 C24 111.8(8) . . ? F7 C28 C24 110.8(8) . . ? F9 C28 C24 114.0(8) . . ? F12 C29 F10 106.7(8) . . ? F12 C29 F11 105.5(7) . . ? F10 C29 F11 106.2(8) . . ? F12 C29 C26 114.2(8) . . ? F10 C29 C26 113.3(8) . . ? F11 C29 C26 110.3(8) . . ? C31 C30 C34 107.9(8) . . ? C31 C30 C35 124.5(10) . . ? C34 C30 C35 126.6(9) . . ? C31 C30 Ti2 72.0(5) . . ? C34 C30 Ti2 71.9(5) . . ? C35 C30 Ti2 130.9(6) . . ? C30 C31 C32 108.9(9) . . ? C30 C31 C36 125.9(11) . . ? C32 C31 C36 124.8(11) . . ? C30 C31 Ti2 73.9(5) . . ? C32 C31 Ti2 74.1(6) . . ? C36 C31 Ti2 124.2(7) . . ? C33 C32 C31 107.4(9) . . ? C33 C32 C37 123.6(11) . . ? C31 C32 C37 129.0(11) . . ? C33 C32 Ti2 72.9(5) . . ? C31 C32 Ti2 71.3(5) . . ? C37 C32 Ti2 121.0(7) . . ? C32 C33 C34 108.3(9) . . ? C32 C33 C38 125.7(10) . . ? C34 C33 C38 125.5(10) . . ? C32 C33 Ti2 73.0(5) . . ? C34 C33 Ti2 71.6(5) . . ? C38 C33 Ti2 126.8(7) . . ? C33 C34 C30 107.4(9) . . ? C33 C34 C39 128.7(10) . . ? C30 C34 C39 123.7(9) . . ? C33 C34 Ti2 73.8(5) . . ? C30 C34 Ti2 73.4(5) . . ? C39 C34 Ti2 121.7(7) . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si2 C40 H40A 109.5 . . ? Si2 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si2 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si2 C41 H41A 109.5 . . ? Si2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si2 C42 H42A 109.5 . . ? Si2 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si2 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 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 C20 Si1 N1 C1 -147.5(6) . . . . ? C21 Si1 N1 C1 -31.2(7) . . . . ? C19 Si1 N1 C1 87.8(6) . . . . ? C20 Si1 N1 Ti1 33.2(6) . . . . ? C21 Si1 N1 Ti1 149.5(4) . . . . ? C19 Si1 N1 Ti1 -91.5(5) . . . . ? Cl1 Ti1 N1 C1 -142.5(7) . . . . ? Cl2 Ti1 N1 C1 112.9(7) . . . . ? C10 Ti1 N1 C1 -53.1(8) . . . . ? C11 Ti1 N1 C1 -22.2(11) . . . . ? C12 Ti1 N1 C1 20.3(9) . . . . ? C9 Ti1 N1 C1 -32.5(8) . . . . ? C13 Ti1 N1 C1 3.1(8) . . . . ? Cl1 Ti1 N1 Si1 36.5(4) . . . . ? Cl2 Ti1 N1 Si1 -68.0(4) . . . . ? C10 Ti1 N1 Si1 125.9(4) . . . . ? C11 Ti1 N1 Si1 156.8(5) . . . . ? C12 Ti1 N1 Si1 -160.6(3) . . . . ? C9 Ti1 N1 Si1 146.6(4) . . . . ? C13 Ti1 N1 Si1 -177.9(4) . . . . ? C40 Si2 N2 C22 -118.0(6) . . . . ? C42 Si2 N2 C22 116.7(7) . . . . ? C41 Si2 N2 C22 0.5(8) . . . . ? C40 Si2 N2 Ti2 74.9(5) . . . . ? C42 Si2 N2 Ti2 -50.4(6) . . . . ? C41 Si2 N2 Ti2 -166.6(6) . . . . ? Cl3 Ti2 N2 C22 174.0(6) . . . . ? Cl4 Ti2 N2 C22 -80.9(7) . . . . ? C31 Ti2 N2 C22 12.9(8) . . . . ? C34 Ti2 N2 C22 74.1(7) . . . . ? C30 Ti2 N2 C22 41.8(7) . . . . ? C33 Ti2 N2 C22 77.7(8) . . . . ? C32 Ti2 N2 C22 18.3(10) . . . . ? Cl3 Ti2 N2 Si2 -20.6(4) . . . . ? Cl4 Ti2 N2 Si2 84.5(4) . . . . ? C31 Ti2 N2 Si2 178.3(4) . . . . ? C34 Ti2 N2 Si2 -120.6(4) . . . . ? C30 Ti2 N2 Si2 -152.9(4) . . . . ? C33 Ti2 N2 Si2 -117.0(5) . . . . ? C32 Ti2 N2 Si2 -176.3(5) . . . . ? Si1 N1 C1 C6 -74.5(9) . . . . ? Ti1 N1 C1 C6 104.6(9) . . . . ? Si1 N1 C1 C2 98.9(8) . . . . ? Ti1 N1 C1 C2 -82.0(10) . . . . ? C6 C1 C2 C3 -1.7(13) . . . . ? N1 C1 C2 C3 -175.2(8) . . . . ? C1 C2 C3 C4 3.0(13) . . . . ? C1 C2 C3 C7 -178.3(8) . . . . ? C2 C3 C4 C5 -3.6(13) . . . . ? C7 C3 C4 C5 177.7(9) . . . . ? C3 C4 C5 C6 3.1(13) . . . . ? C3 C4 C5 C8 178.5(9) . . . . ? C2 C1 C6 C5 1.2(13) . . . . ? N1 C1 C6 C5 174.6(8) . . . . ? C4 C5 C6 C1 -1.9(13) . . . . ? C8 C5 C6 C1 -177.4(9) . . . . ? C2 C3 C7 F1 64.1(12) . . . . ? C4 C3 C7 F1 -117.1(10) . . . . ? C2 C3 C7 F2 -54.9(12) . . . . ? C4 C3 C7 F2 123.8(10) . . . . ? C2 C3 C7 F3 -175.1(8) . . . . ? C4 C3 C7 F3 3.6(13) . . . . ? C6 C5 C8 F5 67.0(13) . . . . ? C4 C5 C8 F5 -108.6(11) . . . . ? C6 C5 C8 F4 -170.2(9) . . . . ? C4 C5 C8 F4 14.2(14) . . . . ? C6 C5 C8 F6 -51.2(12) . . . . ? C4 C5 C8 F6 133.2(9) . . . . ? N1 Ti1 C9 C10 -148.7(5) . . . . ? Cl1 Ti1 C9 C10 -45.0(5) . . . . ? Cl2 Ti1 C9 C10 92.1(6) . . . . ? C11 Ti1 C9 C10 36.8(5) . . . . ? C12 Ti1 C9 C10 78.3(5) . . . . ? C13 Ti1 C9 C10 115.3(7) . . . . ? N1 Ti1 C9 C13 96.0(5) . . . . ? Cl1 Ti1 C9 C13 -160.3(4) . . . . ? Cl2 Ti1 C9 C13 -23.2(7) . . . . ? C10 Ti1 C9 C13 -115.3(7) . . . . ? C11 Ti1 C9 C13 -78.5(5) . . . . ? C12 Ti1 C9 C13 -37.0(5) . . . . ? N1 Ti1 C9 C14 -25.8(9) . . . . ? Cl1 Ti1 C9 C14 77.9(8) . . . . ? Cl2 Ti1 C9 C14 -145.0(7) . . . . ? C10 Ti1 C9 C14 122.9(11) . . . . ? C11 Ti1 C9 C14 159.7(9) . . . . ? C12 Ti1 C9 C14 -158.8(9) . . . . ? C13 Ti1 C9 C14 -121.8(10) . . . . ? C13 C9 C10 C11 0.3(10) . . . . ? C14 C9 C10 C11 170.3(9) . . . . ? Ti1 C9 C10 C11 -64.1(6) . . . . ? C13 C9 C10 C15 -174.0(8) . . . . ? C14 C9 C10 C15 -4.0(15) . . . . ? Ti1 C9 C10 C15 121.6(9) . . . . ? C13 C9 C10 Ti1 64.5(6) . . . . ? C14 C9 C10 Ti1 -125.5(9) . . . . ? N1 Ti1 C10 C9 38.5(6) . . . . ? Cl1 Ti1 C10 C9 137.6(5) . . . . ? Cl2 Ti1 C10 C9 -123.5(5) . . . . ? C11 Ti1 C10 C9 -117.4(7) . . . . ? C12 Ti1 C10 C9 -79.5(5) . . . . ? C13 Ti1 C10 C9 -38.2(5) . . . . ? N1 Ti1 C10 C11 155.9(5) . . . . ? Cl1 Ti1 C10 C11 -105.0(5) . . . . ? Cl2 Ti1 C10 C11 -6.0(6) . . . . ? C12 Ti1 C10 C11 37.9(5) . . . . ? C9 Ti1 C10 C11 117.4(7) . . . . ? C13 Ti1 C10 C11 79.2(5) . . . . ? N1 Ti1 C10 C15 -81.1(8) . . . . ? Cl1 Ti1 C10 C15 18.0(8) . . . . ? Cl2 Ti1 C10 C15 116.9(8) . . . . ? C11 Ti1 C10 C15 123.0(10) . . . . ? C12 Ti1 C10 C15 160.9(9) . . . . ? C9 Ti1 C10 C15 -119.6(10) . . . . ? C13 Ti1 C10 C15 -157.9(9) . . . . ? C9 C10 C11 C12 -0.2(10) . . . . ? C15 C10 C11 C12 173.9(8) . . . . ? Ti1 C10 C11 C12 -64.8(6) . . . . ? C9 C10 C11 C16 179.2(9) . . . . ? C15 C10 C11 C16 -6.7(15) . . . . ? Ti1 C10 C11 C16 114.6(9) . . . . ? C9 C10 C11 Ti1 64.6(6) . . . . ? C15 C10 C11 Ti1 -121.3(9) . . . . ? N1 Ti1 C11 C10 -48.1(9) . . . . ? Cl1 Ti1 C11 C10 73.9(5) . . . . ? Cl2 Ti1 C11 C10 175.4(5) . . . . ? C12 Ti1 C11 C10 -114.9(7) . . . . ? C9 Ti1 C11 C10 -36.1(5) . . . . ? C13 Ti1 C11 C10 -78.0(5) . . . . ? N1 Ti1 C11 C12 66.8(9) . . . . ? Cl1 Ti1 C11 C12 -171.2(5) . . . . ? Cl2 Ti1 C11 C12 -69.7(5) . . . . ? C10 Ti1 C11 C12 114.9(7) . . . . ? C9 Ti1 C11 C12 78.8(5) . . . . ? C13 Ti1 C11 C12 36.9(5) . . . . ? N1 Ti1 C11 C16 -170.2(6) . . . . ? Cl1 Ti1 C11 C16 -48.2(7) . . . . ? Cl2 Ti1 C11 C16 53.3(7) . . . . ? C10 Ti1 C11 C16 -122.1(9) . . . . ? C12 Ti1 C11 C16 123.0(9) . . . . ? C9 Ti1 C11 C16 -158.2(8) . . . . ? C13 Ti1 C11 C16 159.9(8) . . . . ? C10 C11 C12 C13 -0.1(10) . . . . ? C16 C11 C12 C13 -179.5(8) . . . . ? Ti1 C11 C12 C13 -64.7(6) . . . . ? C10 C11 C12 C17 -173.9(8) . . . . ? C16 C11 C12 C17 6.7(15) . . . . ? Ti1 C11 C12 C17 121.5(9) . . . . ? C10 C11 C12 Ti1 64.6(6) . . . . ? C16 C11 C12 Ti1 -114.8(9) . . . . ? N1 Ti1 C12 C13 -31.2(6) . . . . ? Cl1 Ti1 C12 C13 127.5(4) . . . . ? Cl2 Ti1 C12 C13 -133.5(5) . . . . ? C10 Ti1 C12 C13 78.5(5) . . . . ? C11 Ti1 C12 C13 116.4(7) . . . . ? C9 Ti1 C12 C13 37.8(5) . . . . ? N1 Ti1 C12 C11 -147.6(5) . . . . ? Cl1 Ti1 C12 C11 11.1(6) . . . . ? Cl2 Ti1 C12 C11 110.1(5) . . . . ? C10 Ti1 C12 C11 -37.9(5) . . . . ? C9 Ti1 C12 C11 -78.6(5) . . . . ? C13 Ti1 C12 C11 -116.4(7) . . . . ? N1 Ti1 C12 C17 90.0(8) . . . . ? Cl1 Ti1 C12 C17 -111.4(7) . . . . ? Cl2 Ti1 C12 C17 -12.3(7) . . . . ? C10 Ti1 C12 C17 -160.3(8) . . . . ? C11 Ti1 C12 C17 -122.4(10) . . . . ? C9 Ti1 C12 C17 158.9(8) . . . . ? C13 Ti1 C12 C17 121.2(9) . . . . ? C11 C12 C13 C9 0.3(10) . . . . ? C17 C12 C13 C9 174.2(8) . . . . ? Ti1 C12 C13 C9 -64.0(6) . . . . ? C11 C12 C13 C18 -170.1(8) . . . . ? C17 C12 C13 C18 3.8(14) . . . . ? Ti1 C12 C13 C18 125.6(8) . . . . ? C11 C12 C13 Ti1 64.3(6) . . . . ? C17 C12 C13 Ti1 -121.8(9) . . . . ? C10 C9 C13 C12 -0.4(10) . . . . ? C14 C9 C13 C12 -170.5(8) . . . . ? Ti1 C9 C13 C12 64.0(6) . . . . ? C10 C9 C13 C18 169.6(8) . . . . ? C14 C9 C13 C18 -0.5(14) . . . . ? Ti1 C9 C13 C18 -126.0(9) . . . . ? C10 C9 C13 Ti1 -64.4(6) . . . . ? C14 C9 C13 Ti1 125.5(9) . . . . ? N1 Ti1 C13 C12 156.0(5) . . . . ? Cl1 Ti1 C13 C12 -85.4(5) . . . . ? Cl2 Ti1 C13 C12 49.0(5) . . . . ? C10 Ti1 C13 C12 -78.8(5) . . . . ? C11 Ti1 C13 C12 -37.3(5) . . . . ? C9 Ti1 C13 C12 -115.9(7) . . . . ? N1 Ti1 C13 C9 -88.1(5) . . . . ? Cl1 Ti1 C13 C9 30.5(6) . . . . ? Cl2 Ti1 C13 C9 164.9(4) . . . . ? C10 Ti1 C13 C9 37.1(5) . . . . ? C11 Ti1 C13 C9 78.6(5) . . . . ? C12 Ti1 C13 C9 115.9(7) . . . . ? N1 Ti1 C13 C18 36.0(8) . . . . ? Cl1 Ti1 C13 C18 154.6(6) . . . . ? Cl2 Ti1 C13 C18 -71.0(8) . . . . ? C10 Ti1 C13 C18 161.2(9) . . . . ? C11 Ti1 C13 C18 -157.3(9) . . . . ? C12 Ti1 C13 C18 -120.0(10) . . . . ? C9 Ti1 C13 C18 124.1(10) . . . . ? Si2 N2 C22 C23 75.0(9) . . . . ? Ti2 N2 C22 C23 -118.7(8) . . . . ? Si2 N2 C22 C27 -101.3(8) . . . . ? Ti2 N2 C22 C27 65.0(10) . . . . ? C27 C22 C23 C24 -1.9(13) . . . . ? N2 C22 C23 C24 -178.1(8) . . . . ? C22 C23 C24 C25 -0.1(14) . . . . ? C22 C23 C24 C28 178.6(9) . . . . ? C23 C24 C25 C26 2.0(13) . . . . ? C28 C24 C25 C26 -176.7(8) . . . . ? C24 C25 C26 C27 -2.0(12) . . . . ? C24 C25 C26 C29 179.1(8) . . . . ? C25 C26 C27 C22 0.1(13) . . . . ? C29 C26 C27 C22 179.0(8) . . . . ? C23 C22 C27 C26 1.9(13) . . . . ? N2 C22 C27 C26 178.3(8) . . . . ? C23 C24 C28 F8 -75.4(12) . . . . ? C25 C24 C28 F8 103.4(11) . . . . ? C23 C24 C28 F7 44.3(12) . . . . ? C25 C24 C28 F7 -136.9(9) . . . . ? C23 C24 C28 F9 161.6(9) . . . . ? C25 C24 C28 F9 -19.7(13) . . . . ? C25 C26 C29 F12 7.0(12) . . . . ? C27 C26 C29 F12 -171.9(8) . . . . ? C25 C26 C29 F10 129.5(9) . . . . ? C27 C26 C29 F10 -49.4(11) . . . . ? C25 C26 C29 F11 -111.6(9) . . . . ? C27 C26 C29 F11 69.5(11) . . . . ? N2 Ti2 C30 C31 -127.4(6) . . . . ? Cl3 Ti2 C30 C31 121.3(6) . . . . ? Cl4 Ti2 C30 C31 -24.7(6) . . . . ? C34 Ti2 C30 C31 116.5(8) . . . . ? C33 Ti2 C30 C31 78.4(6) . . . . ? C32 Ti2 C30 C31 37.5(6) . . . . ? N2 Ti2 C30 C34 116.1(6) . . . . ? Cl3 Ti2 C30 C34 4.9(7) . . . . ? Cl4 Ti2 C30 C34 -141.1(5) . . . . ? C31 Ti2 C30 C34 -116.5(8) . . . . ? C33 Ti2 C30 C34 -38.1(6) . . . . ? C32 Ti2 C30 C34 -79.0(6) . . . . ? N2 Ti2 C30 C35 -7.1(10) . . . . ? Cl3 Ti2 C30 C35 -118.3(9) . . . . ? Cl4 Ti2 C30 C35 95.7(10) . . . . ? C31 Ti2 C30 C35 120.4(12) . . . . ? C34 Ti2 C30 C35 -123.2(12) . . . . ? C33 Ti2 C30 C35 -161.2(11) . . . . ? C32 Ti2 C30 C35 157.9(11) . . . . ? C34 C30 C31 C32 -3.1(10) . . . . ? C35 C30 C31 C32 165.9(8) . . . . ? Ti2 C30 C31 C32 -66.4(7) . . . . ? C34 C30 C31 C36 -175.7(9) . . . . ? C35 C30 C31 C36 -6.8(15) . . . . ? Ti2 C30 C31 C36 120.9(10) . . . . ? C34 C30 C31 Ti2 63.3(6) . . . . ? C35 C30 C31 Ti2 -127.7(8) . . . . ? N2 Ti2 C31 C30 59.1(6) . . . . ? Cl3 Ti2 C31 C30 -92.4(6) . . . . ? Cl4 Ti2 C31 C30 159.2(5) . . . . ? C34 Ti2 C31 C30 -37.2(5) . . . . ? C33 Ti2 C31 C30 -78.6(6) . . . . ? C32 Ti2 C31 C30 -115.6(8) . . . . ? N2 Ti2 C31 C32 174.8(5) . . . . ? Cl3 Ti2 C31 C32 23.3(8) . . . . ? Cl4 Ti2 C31 C32 -85.2(6) . . . . ? C34 Ti2 C31 C32 78.4(6) . . . . ? C30 Ti2 C31 C32 115.6(8) . . . . ? C33 Ti2 C31 C32 37.0(6) . . . . ? N2 Ti2 C31 C36 -63.6(11) . . . . ? Cl3 Ti2 C31 C36 144.9(9) . . . . ? Cl4 Ti2 C31 C36 36.4(10) . . . . ? C34 Ti2 C31 C36 -160.0(12) . . . . ? C30 Ti2 C31 C36 -122.7(13) . . . . ? C33 Ti2 C31 C36 158.6(12) . . . . ? C32 Ti2 C31 C36 121.6(13) . . . . ? C30 C31 C32 C33 1.8(11) . . . . ? C36 C31 C32 C33 174.6(9) . . . . ? Ti2 C31 C32 C33 -64.5(7) . . . . ? C30 C31 C32 C37 -178.6(10) . . . . ? C36 C31 C32 C37 -5.8(16) . . . . ? Ti2 C31 C32 C37 115.2(10) . . . . ? C30 C31 C32 Ti2 66.3(6) . . . . ? C36 C31 C32 Ti2 -121.0(10) . . . . ? N2 Ti2 C32 C33 106.9(8) . . . . ? Cl3 Ti2 C32 C33 -48.6(6) . . . . ? Cl4 Ti2 C32 C33 -150.4(6) . . . . ? C31 Ti2 C32 C33 115.7(8) . . . . ? C34 Ti2 C32 C33 37.0(6) . . . . ? C30 Ti2 C32 C33 78.6(6) . . . . ? N2 Ti2 C32 C31 -8.8(9) . . . . ? Cl3 Ti2 C32 C31 -164.3(5) . . . . ? Cl4 Ti2 C32 C31 93.9(6) . . . . ? C34 Ti2 C32 C31 -78.7(6) . . . . ? C30 Ti2 C32 C31 -37.1(6) . . . . ? C33 Ti2 C32 C31 -115.7(8) . . . . ? N2 Ti2 C32 C37 -133.8(9) . . . . ? Cl3 Ti2 C32 C37 70.7(10) . . . . ? Cl4 Ti2 C32 C37 -31.0(10) . . . . ? C31 Ti2 C32 C37 -124.9(12) . . . . ? C34 Ti2 C32 C37 156.4(11) . . . . ? C30 Ti2 C32 C37 -162.0(11) . . . . ? C33 Ti2 C32 C37 119.4(12) . . . . ? C31 C32 C33 C34 0.2(11) . . . . ? C37 C32 C33 C34 -179.5(9) . . . . ? Ti2 C32 C33 C34 -63.3(7) . . . . ? C31 C32 C33 C38 -173.1(9) . . . . ? C37 C32 C33 C38 7.2(16) . . . . ? Ti2 C32 C33 C38 123.5(10) . . . . ? C31 C32 C33 Ti2 63.4(7) . . . . ? C37 C32 C33 Ti2 -116.2(10) . . . . ? N2 Ti2 C33 C32 -122.7(7) . . . . ? Cl3 Ti2 C33 C32 133.4(6) . . . . ? Cl4 Ti2 C33 C32 33.5(7) . . . . ? C31 Ti2 C33 C32 -37.5(6) . . . . ? C34 Ti2 C33 C32 -116.7(9) . . . . ? C30 Ti2 C33 C32 -78.5(6) . . . . ? N2 Ti2 C33 C34 -6.1(9) . . . . ? Cl3 Ti2 C33 C34 -109.9(6) . . . . ? Cl4 Ti2 C33 C34 150.2(5) . . . . ? C31 Ti2 C33 C34 79.2(6) . . . . ? C30 Ti2 C33 C34 38.2(5) . . . . ? C32 Ti2 C33 C34 116.7(9) . . . . ? N2 Ti2 C33 C38 115.0(10) . . . . ? Cl3 Ti2 C33 C38 11.1(10) . . . . ? Cl4 Ti2 C33 C38 -88.8(10) . . . . ? C31 Ti2 C33 C38 -159.8(12) . . . . ? C34 Ti2 C33 C38 121.1(13) . . . . ? C30 Ti2 C33 C38 159.3(12) . . . . ? C32 Ti2 C33 C38 -122.3(13) . . . . ? C32 C33 C34 C30 -2.0(11) . . . . ? C38 C33 C34 C30 171.2(9) . . . . ? Ti2 C33 C34 C30 -66.2(6) . . . . ? C32 C33 C34 C39 -177.8(10) . . . . ? C38 C33 C34 C39 -4.5(16) . . . . ? Ti2 C33 C34 C39 118.0(10) . . . . ? C32 C33 C34 Ti2 64.2(7) . . . . ? C38 C33 C34 Ti2 -122.5(10) . . . . ? C31 C30 C34 C33 3.1(10) . . . . ? C35 C30 C34 C33 -165.5(9) . . . . ? Ti2 C30 C34 C33 66.5(6) . . . . ? C31 C30 C34 C39 179.2(9) . . . . ? C35 C30 C34 C39 10.5(15) . . . . ? Ti2 C30 C34 C39 -117.4(9) . . . . ? C31 C30 C34 Ti2 -63.4(6) . . . . ? C35 C30 C34 Ti2 127.9(9) . . . . ? N2 Ti2 C34 C33 176.0(6) . . . . ? Cl3 Ti2 C34 C33 69.4(6) . . . . ? Cl4 Ti2 C34 C33 -49.1(8) . . . . ? C31 Ti2 C34 C33 -77.7(6) . . . . ? C30 Ti2 C34 C33 -114.3(8) . . . . ? C32 Ti2 C34 C33 -36.5(6) . . . . ? N2 Ti2 C34 C30 -69.6(6) . . . . ? Cl3 Ti2 C34 C30 -176.3(5) . . . . ? Cl4 Ti2 C34 C30 65.2(7) . . . . ? C31 Ti2 C34 C30 36.6(5) . . . . ? C33 Ti2 C34 C30 114.3(8) . . . . ? C32 Ti2 C34 C30 77.8(6) . . . . ? N2 Ti2 C34 C39 50.1(9) . . . . ? Cl3 Ti2 C34 C39 -56.5(9) . . . . ? Cl4 Ti2 C34 C39 -175.0(7) . . . . ? C31 Ti2 C34 C39 156.3(10) . . . . ? C30 Ti2 C34 C39 119.8(11) . . . . ? C33 Ti2 C34 C39 -125.9(11) . . . . ? C32 Ti2 C34 C39 -162.4(10) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.736 _refine_diff_density_min -1.173 _refine_diff_density_rms 0.238 # Attachment '4128_web_deposit_cif_file_2_HayatoTsurugi_1297063279.cif' data_4a _database_code_depnum_ccdc_archive 'CCDC 811935' #TrackingRef '4128_web_deposit_cif_file_2_HayatoTsurugi_1297063279.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 4a _chemical_melting_point ? _chemical_formula_moiety 'C26 H16 Cl2 F12 N2 Ti2, C6H6' _chemical_formula_sum 'C32 H22 Cl2 F12 N2 Ti2' _chemical_formula_weight 829.22 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.882(6) _cell_length_b 8.044(3) _cell_length_c 26.068(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.757(16) _cell_angle_gamma 90.00 _cell_volume 3291.8(19) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 1499 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.32 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 0.743 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.8078 _exptl_absorpt_correction_T_max 0.9294 _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12742 _diffrn_reflns_av_R_equivalents 0.1325 _diffrn_reflns_av_sigmaI/netI 0.1592 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.26 _reflns_number_total 3583 _reflns_number_gt 1537 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SIR92 (Altomare, et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' _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^)+(0.1990P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3583 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2064 _refine_ls_R_factor_gt 0.1118 _refine_ls_wR_factor_ref 0.3652 _refine_ls_wR_factor_gt 0.2845 _refine_ls_goodness_of_fit_ref 0.995 _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 Ti1 Ti 0.56759(9) -0.0523(2) -0.02637(6) 0.0366(5) Uani 1 1 d . . . Cl1 Cl 0.60901(15) -0.3219(3) -0.00339(9) 0.0493(7) Uani 1 1 d . . . F1 F 0.8672(4) -0.0578(8) 0.1240(2) 0.0712(19) Uani 1 1 d . . . F2 F 0.8017(4) -0.1282(9) 0.1863(3) 0.082(2) Uani 1 1 d . . . F3 F 0.8812(3) 0.0873(7) 0.1940(2) 0.0587(16) Uani 1 1 d . . . F4 F 0.6397(4) 0.6469(7) 0.1266(2) 0.0624(16) Uani 1 1 d . . . F5 F 0.7027(4) 0.5680(7) 0.2009(2) 0.0648(17) Uani 1 1 d . . . F6 F 0.5690(4) 0.5256(7) 0.1794(2) 0.0627(17) Uani 1 1 d . . . N1 N 0.5562(4) 0.0575(9) 0.0376(3) 0.0378(17) Uani 1 1 d . . . C1 C 0.6163(5) 0.1302(11) 0.0779(3) 0.0323(19) Uani 1 1 d . . . C2 C 0.6887(5) 0.0412(10) 0.0982(3) 0.0352(19) Uani 1 1 d . . . H1 H 0.6985 -0.0652 0.0845 0.042 Uiso 1 1 calc R . . C3 C 0.7479(5) 0.1082(11) 0.1392(3) 0.038(2) Uani 1 1 d . . . C4 C 0.7354(5) 0.2653(11) 0.1590(3) 0.039(2) Uani 1 1 d . . . H2 H 0.7758 0.3104 0.1860 0.047 Uiso 1 1 calc R . . C5 C 0.6623(5) 0.3568(11) 0.1386(3) 0.0360(19) Uani 1 1 d . . . C6 C 0.6022(5) 0.2894(10) 0.0987(3) 0.037(2) Uani 1 1 d . . . H3 H 0.5522 0.3503 0.0857 0.044 Uiso 1 1 calc R . . C7 C 0.8252(6) 0.0054(11) 0.1611(3) 0.039(2) Uani 1 1 d . . . C8 C 0.6443(6) 0.5225(11) 0.1614(3) 0.037(2) Uani 1 1 d . . . C9 C 0.6909(6) 0.0842(11) -0.0427(4) 0.044(2) Uani 1 1 d . . . H4 H 0.7379 0.0960 -0.0157 0.053 Uiso 1 1 calc R . . C10 C 0.6234(6) 0.1950(12) -0.0540(3) 0.048(2) Uani 1 1 d . . . H5 H 0.6164 0.2956 -0.0360 0.058 Uiso 1 1 calc R . . C11 C 0.5660(6) 0.1313(12) -0.0976(3) 0.047(2) Uani 1 1 d . . . H6 H 0.5143 0.1809 -0.1136 0.056 Uiso 1 1 calc R . . C12 C 0.6021(6) -0.0213(12) -0.1121(4) 0.048(2) Uani 1 1 d . . . H7 H 0.5786 -0.0918 -0.1398 0.057 Uiso 1 1 calc R . . C13 C 0.6777(6) -0.0488(12) -0.0783(4) 0.049(2) Uani 1 1 d . . . H8 H 0.7143 -0.1418 -0.0792 0.058 Uiso 1 1 calc R . . C14 C 0.5000 -0.1397(18) 0.2500 0.049(3) Uani 1 2 d S . . H9 H 0.5000 -0.2578 0.2500 0.058 Uiso 1 2 calc SR . . C15 C 0.5686(6) -0.0559(13) 0.2375(4) 0.052(3) Uani 1 1 d . . . H10 H 0.6160 -0.1159 0.2287 0.062 Uiso 1 1 calc R . . C16 C 0.5697(6) 0.1164(12) 0.2375(3) 0.044(2) Uani 1 1 d . . . H11 H 0.6175 0.1754 0.2290 0.053 Uiso 1 1 calc R . . C17 C 0.5000 0.2007(15) 0.2500 0.049(3) Uani 1 2 d S . . H12 H 0.5000 0.3188 0.2500 0.059 Uiso 1 2 calc SR . . 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 0.0327(9) 0.0436(11) 0.0333(9) -0.0017(7) 0.0046(7) -0.0007(7) Cl1 0.0565(15) 0.0405(13) 0.0514(14) 0.0034(11) 0.0101(11) 0.0074(11) F1 0.054(4) 0.090(5) 0.066(4) -0.023(3) -0.002(3) 0.032(3) F2 0.054(4) 0.077(4) 0.109(5) 0.043(4) -0.005(4) -0.004(3) F3 0.034(3) 0.064(4) 0.070(4) -0.011(3) -0.019(3) 0.009(3) F4 0.087(4) 0.047(3) 0.057(3) 0.004(3) 0.023(3) 0.018(3) F5 0.066(4) 0.056(4) 0.064(4) -0.018(3) -0.018(3) 0.009(3) F6 0.059(4) 0.053(3) 0.085(4) -0.020(3) 0.041(3) -0.011(3) N1 0.035(4) 0.049(5) 0.028(4) 0.007(3) -0.001(3) 0.002(3) C1 0.027(4) 0.040(5) 0.030(4) -0.003(4) 0.004(3) -0.002(4) C2 0.035(5) 0.036(5) 0.033(5) 0.000(4) -0.005(4) -0.010(4) C3 0.036(5) 0.041(5) 0.038(5) 0.004(4) 0.004(4) -0.002(4) C4 0.035(5) 0.042(5) 0.037(5) 0.001(4) -0.004(4) 0.002(4) C5 0.037(5) 0.037(5) 0.035(5) 0.000(4) 0.008(4) -0.001(4) C6 0.033(4) 0.040(5) 0.039(5) 0.007(4) 0.012(4) 0.008(4) C7 0.035(5) 0.041(5) 0.037(5) 0.005(4) -0.013(4) 0.001(4) C8 0.041(5) 0.040(5) 0.029(5) -0.009(4) 0.003(4) -0.008(4) C9 0.035(5) 0.051(6) 0.048(6) 0.002(4) 0.011(4) -0.001(4) C10 0.060(6) 0.050(6) 0.039(5) -0.006(4) 0.020(4) -0.005(5) C11 0.042(5) 0.056(6) 0.042(5) 0.013(5) 0.008(4) 0.002(5) C12 0.044(6) 0.058(6) 0.041(5) 0.001(5) 0.006(5) -0.012(5) C13 0.048(6) 0.057(6) 0.045(6) 0.002(5) 0.020(5) 0.003(5) C14 0.042(8) 0.049(8) 0.052(8) 0.000 -0.003(6) 0.000 C15 0.044(6) 0.072(7) 0.040(5) -0.002(5) 0.006(4) 0.018(5) C16 0.044(5) 0.049(6) 0.039(5) 0.001(4) 0.005(4) -0.005(4) C17 0.073(10) 0.025(7) 0.046(8) 0.000 0.001(7) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N1 1.920(7) . ? Ti1 N1 1.944(7) 5_655 ? Ti1 Cl1 2.318(3) . ? Ti1 C10 2.337(9) . ? Ti1 C9 2.341(9) . ? Ti1 C13 2.369(9) . ? Ti1 C11 2.370(9) . ? Ti1 C12 2.392(9) . ? Ti1 Ti1 2.847(3) 5_655 ? F1 C7 1.353(11) . ? F2 C7 1.343(10) . ? F3 C7 1.315(10) . ? F4 C8 1.345(10) . ? F5 C8 1.328(10) . ? F6 C8 1.351(10) . ? N1 C1 1.433(10) . ? N1 Ti1 1.944(7) 5_655 ? C1 C2 1.388(11) . ? C1 C6 1.422(11) . ? C2 C3 1.419(11) . ? C2 H1 0.9500 . ? C3 C4 1.391(12) . ? C3 C7 1.517(12) . ? C4 C5 1.409(12) . ? C4 H2 0.9500 . ? C5 C6 1.409(12) . ? C5 C8 1.504(12) . ? C6 H3 0.9500 . ? C9 C10 1.391(13) . ? C9 C13 1.412(13) . ? C9 H4 0.9500 . ? C10 C11 1.439(13) . ? C10 H5 0.9500 . ? C11 C12 1.430(13) . ? C11 H6 0.9500 . ? C12 C13 1.394(14) . ? C12 H7 0.9500 . ? C13 H8 0.9500 . ? C14 C15 1.363(12) . ? C14 C15 1.363(12) 2_655 ? C14 H9 0.9500 . ? C15 C16 1.387(13) . ? C15 H10 0.9500 . ? C16 C17 1.379(11) . ? C16 H11 0.9500 . ? C17 C16 1.379(11) 2_655 ? C17 H12 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ti1 N1 85.0(3) . 5_655 ? N1 Ti1 Cl1 105.5(2) . . ? N1 Ti1 Cl1 105.1(2) 5_655 . ? N1 Ti1 C10 88.1(3) . . ? N1 Ti1 C10 113.2(3) 5_655 . ? Cl1 Ti1 C10 140.4(3) . . ? N1 Ti1 C9 97.7(3) . . ? N1 Ti1 C9 146.9(3) 5_655 . ? Cl1 Ti1 C9 105.9(2) . . ? C10 Ti1 C9 34.6(3) . . ? N1 Ti1 C13 131.8(3) . . ? N1 Ti1 C13 137.0(3) 5_655 . ? Cl1 Ti1 C13 87.4(3) . . ? C10 Ti1 C13 57.7(3) . . ? C9 Ti1 C13 34.9(3) . . ? N1 Ti1 C11 113.7(3) . . ? N1 Ti1 C11 90.3(3) 5_655 . ? Cl1 Ti1 C11 139.0(2) . . ? C10 Ti1 C11 35.6(3) . . ? C9 Ti1 C11 58.3(3) . . ? C13 Ti1 C11 57.7(3) . . ? N1 Ti1 C12 145.9(3) . . ? N1 Ti1 C12 103.4(3) 5_655 . ? Cl1 Ti1 C12 104.0(3) . . ? C10 Ti1 C12 58.1(3) . . ? C9 Ti1 C12 57.6(3) . . ? C13 Ti1 C12 34.0(3) . . ? C11 Ti1 C12 34.9(3) . . ? N1 Ti1 Ti1 42.8(2) . 5_655 ? N1 Ti1 Ti1 42.2(2) 5_655 5_655 ? Cl1 Ti1 Ti1 110.92(10) . 5_655 ? C10 Ti1 Ti1 104.3(2) . 5_655 ? C9 Ti1 Ti1 131.5(2) . 5_655 ? C13 Ti1 Ti1 161.6(3) . 5_655 ? C11 Ti1 Ti1 106.0(2) . 5_655 ? C12 Ti1 Ti1 135.8(3) . 5_655 ? C1 N1 Ti1 133.2(5) . . ? C1 N1 Ti1 131.7(5) . 5_655 ? Ti1 N1 Ti1 95.0(3) . 5_655 ? C2 C1 C6 119.3(7) . . ? C2 C1 N1 119.3(7) . . ? C6 C1 N1 121.4(7) . . ? C1 C2 C3 120.5(8) . . ? C1 C2 H1 119.8 . . ? C3 C2 H1 119.8 . . ? C4 C3 C2 120.6(8) . . ? C4 C3 C7 120.6(8) . . ? C2 C3 C7 118.9(8) . . ? C3 C4 C5 119.4(8) . . ? C3 C4 H2 120.3 . . ? C5 C4 H2 120.3 . . ? C4 C5 C6 120.3(8) . . ? C4 C5 C8 120.7(8) . . ? C6 C5 C8 118.9(7) . . ? C5 C6 C1 120.0(7) . . ? C5 C6 H3 120.0 . . ? C1 C6 H3 120.0 . . ? F3 C7 F2 107.0(7) . . ? F3 C7 F1 107.2(7) . . ? F2 C7 F1 104.7(8) . . ? F3 C7 C3 113.6(7) . . ? F2 C7 C3 110.6(7) . . ? F1 C7 C3 113.2(7) . . ? F5 C8 F4 106.2(7) . . ? F5 C8 F6 106.0(7) . . ? F4 C8 F6 105.1(7) . . ? F5 C8 C5 113.4(7) . . ? F4 C8 C5 112.8(7) . . ? F6 C8 C5 112.6(7) . . ? C10 C9 C13 108.3(9) . . ? C10 C9 Ti1 72.5(5) . . ? C13 C9 Ti1 73.7(5) . . ? C10 C9 H4 125.9 . . ? C13 C9 H4 125.9 . . ? Ti1 C9 H4 119.8 . . ? C9 C10 C11 108.3(8) . . ? C9 C10 Ti1 72.9(5) . . ? C11 C10 Ti1 73.5(5) . . ? C9 C10 H5 125.8 . . ? C11 C10 H5 125.8 . . ? Ti1 C10 H5 119.7 . . ? C12 C11 C10 106.4(8) . . ? C12 C11 Ti1 73.4(5) . . ? C10 C11 Ti1 70.9(5) . . ? C12 C11 H6 126.8 . . ? C10 C11 H6 126.8 . . ? Ti1 C11 H6 120.7 . . ? C13 C12 C11 108.1(9) . . ? C13 C12 Ti1 72.1(5) . . ? C11 C12 Ti1 71.7(5) . . ? C13 C12 H7 125.9 . . ? C11 C12 H7 125.9 . . ? Ti1 C12 H7 122.0 . . ? C12 C13 C9 108.8(9) . . ? C12 C13 Ti1 73.9(5) . . ? C9 C13 Ti1 71.5(5) . . ? C12 C13 H8 125.6 . . ? C9 C13 H8 125.6 . . ? Ti1 C13 H8 120.8 . . ? C15 C14 C15 120.7(14) . 2_655 ? C15 C14 H9 119.6 . . ? C15 C14 H9 119.6 2_655 . ? C14 C15 C16 120.3(10) . . ? C14 C15 H10 119.9 . . ? C16 C15 H10 119.9 . . ? C17 C16 C15 118.8(9) . . ? C17 C16 H11 120.6 . . ? C15 C16 H11 120.6 . . ? C16 C17 C16 121.1(12) . 2_655 ? C16 C17 H12 119.4 . . ? C16 C17 H12 119.4 2_655 . ? 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 N1 Ti1 N1 C1 -175.6(9) 5_655 . . . ? Cl1 Ti1 N1 C1 80.1(8) . . . . ? C10 Ti1 N1 C1 -62.1(8) . . . . ? C9 Ti1 N1 C1 -28.8(8) . . . . ? C13 Ti1 N1 C1 -20.4(9) . . . . ? C11 Ti1 N1 C1 -87.5(8) . . . . ? C12 Ti1 N1 C1 -68.9(10) . . . . ? Ti1 Ti1 N1 C1 -175.6(9) 5_655 . . . ? N1 Ti1 N1 Ti1 0.0 5_655 . . 5_655 ? Cl1 Ti1 N1 Ti1 -104.3(2) . . . 5_655 ? C10 Ti1 N1 Ti1 113.5(3) . . . 5_655 ? C9 Ti1 N1 Ti1 146.8(3) . . . 5_655 ? C13 Ti1 N1 Ti1 155.2(4) . . . 5_655 ? C11 Ti1 N1 Ti1 88.1(3) . . . 5_655 ? C12 Ti1 N1 Ti1 106.7(6) . . . 5_655 ? Ti1 N1 C1 C2 -48.3(11) . . . . ? Ti1 N1 C1 C2 137.5(7) 5_655 . . . ? Ti1 N1 C1 C6 133.8(7) . . . . ? Ti1 N1 C1 C6 -40.3(11) 5_655 . . . ? C6 C1 C2 C3 -0.1(12) . . . . ? N1 C1 C2 C3 -178.0(7) . . . . ? C1 C2 C3 C4 -1.3(12) . . . . ? C1 C2 C3 C7 178.7(8) . . . . ? C2 C3 C4 C5 1.2(12) . . . . ? C7 C3 C4 C5 -178.8(8) . . . . ? C3 C4 C5 C6 0.3(12) . . . . ? C3 C4 C5 C8 176.3(8) . . . . ? C4 C5 C6 C1 -1.7(12) . . . . ? C8 C5 C6 C1 -177.8(7) . . . . ? C2 C1 C6 C5 1.6(11) . . . . ? N1 C1 C6 C5 179.5(7) . . . . ? C4 C3 C7 F3 -8.5(12) . . . . ? C2 C3 C7 F3 171.6(7) . . . . ? C4 C3 C7 F2 111.9(10) . . . . ? C2 C3 C7 F2 -68.1(11) . . . . ? C4 C3 C7 F1 -131.0(8) . . . . ? C2 C3 C7 F1 49.0(11) . . . . ? C4 C5 C8 F5 -0.3(11) . . . . ? C6 C5 C8 F5 175.8(7) . . . . ? C4 C5 C8 F4 120.5(8) . . . . ? C6 C5 C8 F4 -63.4(10) . . . . ? C4 C5 C8 F6 -120.7(9) . . . . ? C6 C5 C8 F6 55.4(10) . . . . ? N1 Ti1 C9 C10 -75.1(6) . . . . ? N1 Ti1 C9 C10 17.6(9) 5_655 . . . ? Cl1 Ti1 C9 C10 176.3(5) . . . . ? C13 Ti1 C9 C10 115.8(8) . . . . ? C11 Ti1 C9 C10 38.0(5) . . . . ? C12 Ti1 C9 C10 79.5(6) . . . . ? Ti1 Ti1 C9 C10 -45.4(6) 5_655 . . . ? N1 Ti1 C9 C13 169.1(6) . . . . ? N1 Ti1 C9 C13 -98.2(7) 5_655 . . . ? Cl1 Ti1 C9 C13 60.5(6) . . . . ? C10 Ti1 C9 C13 -115.8(8) . . . . ? C11 Ti1 C9 C13 -77.7(6) . . . . ? C12 Ti1 C9 C13 -36.3(6) . . . . ? Ti1 Ti1 C9 C13 -161.1(5) 5_655 . . . ? C13 C9 C10 C11 0.1(10) . . . . ? Ti1 C9 C10 C11 -65.4(6) . . . . ? C13 C9 C10 Ti1 65.5(6) . . . . ? N1 Ti1 C10 C9 106.6(6) . . . . ? N1 Ti1 C10 C9 -169.7(5) 5_655 . . . ? Cl1 Ti1 C10 C9 -5.6(7) . . . . ? C13 Ti1 C10 C9 -37.5(5) . . . . ? C11 Ti1 C10 C9 -115.8(8) . . . . ? C12 Ti1 C10 C9 -77.9(6) . . . . ? Ti1 Ti1 C10 C9 146.6(5) 5_655 . . . ? N1 Ti1 C10 C11 -137.6(5) . . . . ? N1 Ti1 C10 C11 -53.9(6) 5_655 . . . ? Cl1 Ti1 C10 C11 110.2(5) . . . . ? C9 Ti1 C10 C11 115.8(8) . . . . ? C13 Ti1 C10 C11 78.3(6) . . . . ? C12 Ti1 C10 C11 37.8(5) . . . . ? Ti1 Ti1 C10 C11 -97.6(5) 5_655 . . . ? C9 C10 C11 C12 -0.3(10) . . . . ? Ti1 C10 C11 C12 -65.4(6) . . . . ? C9 C10 C11 Ti1 65.0(6) . . . . ? N1 Ti1 C11 C12 161.9(5) . . . . ? N1 Ti1 C11 C12 -113.4(6) 5_655 . . . ? Cl1 Ti1 C11 C12 0.3(7) . . . . ? C10 Ti1 C11 C12 114.5(8) . . . . ? C9 Ti1 C11 C12 77.6(6) . . . . ? C13 Ti1 C11 C12 36.2(5) . . . . ? Ti1 Ti1 C11 C12 -153.1(5) 5_655 . . . ? N1 Ti1 C11 C10 47.4(6) . . . . ? N1 Ti1 C11 C10 132.1(5) 5_655 . . . ? Cl1 Ti1 C11 C10 -114.2(5) . . . . ? C9 Ti1 C11 C10 -37.0(5) . . . . ? C13 Ti1 C11 C10 -78.3(6) . . . . ? C12 Ti1 C11 C10 -114.5(8) . . . . ? Ti1 Ti1 C11 C10 92.3(5) 5_655 . . . ? C10 C11 C12 C13 0.4(10) . . . . ? Ti1 C11 C12 C13 -63.3(6) . . . . ? C10 C11 C12 Ti1 63.7(6) . . . . ? N1 Ti1 C12 C13 86.4(8) . . . . ? N1 Ti1 C12 C13 -172.5(6) 5_655 . . . ? Cl1 Ti1 C12 C13 -62.9(6) . . . . ? C10 Ti1 C12 C13 78.3(6) . . . . ? C9 Ti1 C12 C13 37.2(6) . . . . ? C11 Ti1 C12 C13 116.9(8) . . . . ? Ti1 Ti1 C12 C13 155.4(5) 5_655 . . . ? N1 Ti1 C12 C11 -30.5(9) . . . . ? N1 Ti1 C12 C11 70.6(6) 5_655 . . . ? Cl1 Ti1 C12 C11 -179.8(5) . . . . ? C10 Ti1 C12 C11 -38.6(5) . . . . ? C9 Ti1 C12 C11 -79.7(6) . . . . ? C13 Ti1 C12 C11 -116.9(8) . . . . ? Ti1 Ti1 C12 C11 38.5(7) 5_655 . . . ? C11 C12 C13 C9 -0.4(10) . . . . ? Ti1 C12 C13 C9 -63.4(6) . . . . ? C11 C12 C13 Ti1 63.0(6) . . . . ? C10 C9 C13 C12 0.2(10) . . . . ? Ti1 C9 C13 C12 64.9(6) . . . . ? C10 C9 C13 Ti1 -64.8(6) . . . . ? N1 Ti1 C13 C12 -131.4(6) . . . . ? N1 Ti1 C13 C12 10.8(8) 5_655 . . . ? Cl1 Ti1 C13 C12 120.2(6) . . . . ? C10 Ti1 C13 C12 -79.6(6) . . . . ? C9 Ti1 C13 C12 -116.8(9) . . . . ? C11 Ti1 C13 C12 -37.2(6) . . . . ? Ti1 Ti1 C13 C12 -66.8(11) 5_655 . . . ? N1 Ti1 C13 C9 -14.6(8) . . . . ? N1 Ti1 C13 C9 127.6(6) 5_655 . . . ? Cl1 Ti1 C13 C9 -123.0(6) . . . . ? C10 Ti1 C13 C9 37.2(5) . . . . ? C11 Ti1 C13 C9 79.6(6) . . . . ? C12 Ti1 C13 C9 116.8(9) . . . . ? Ti1 Ti1 C13 C9 50.0(11) 5_655 . . . ? C15 C14 C15 C16 0.2(6) 2_655 . . . ? C14 C15 C16 C17 -0.4(12) . . . . ? C15 C16 C17 C16 0.2(6) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.26 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.075 _refine_diff_density_min -1.347 _refine_diff_density_rms 0.243 # Attachment '4129_web_deposit_cif_file_3_HayatoTsurugi_1297063279.cif' data_4b _database_code_depnum_ccdc_archive 'CCDC 811936' #TrackingRef '4129_web_deposit_cif_file_3_HayatoTsurugi_1297063279.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 4b _chemical_melting_point ? _chemical_formula_moiety 'C36 H36 Cl2 F12 N2 Ti2' _chemical_formula_sum 'C36 H36 Cl2 F12 N2 Ti2' _chemical_formula_weight 891.37 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.8477(16) _cell_length_b 22.113(3) _cell_length_c 10.0609(14) _cell_angle_alpha 90.00 _cell_angle_beta 109.928(5) _cell_angle_gamma 90.00 _cell_volume 1850.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 4207 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.7316 _exptl_absorpt_correction_T_max 0.9363 _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16827 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4181 _reflns_number_gt 3514 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ORTEP-III _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^)+(0.0811P)^2^+2.2854P] 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 4181 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1494 _refine_ls_wR_factor_gt 0.1409 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 Ti1 Ti 0.41649(5) 0.011223(19) 0.59551(5) 0.01476(15) Uani 1 1 d . . . Cl1 Cl 0.16451(7) 0.04801(3) 0.47380(7) 0.02281(18) Uani 1 1 d . . . F1 F 0.3547(3) 0.26747(11) 0.6343(3) 0.0578(6) Uani 1 1 d . . . F2 F 0.2761(3) 0.26286(11) 0.4117(3) 0.0617(7) Uani 1 1 d . . . F3 F 0.4608(3) 0.32582(9) 0.5220(4) 0.0793(10) Uani 1 1 d . . . F4 F 1.0675(3) 0.19529(18) 0.7345(4) 0.1042(14) Uani 1 1 d . . . F5 F 1.0008(3) 0.26900(9) 0.5983(4) 0.0732(9) Uani 1 1 d . . . F6 F 1.0457(4) 0.18201(15) 0.5304(5) 0.1096(16) Uani 1 1 d . . . N1 N 0.5545(3) 0.05595(9) 0.5142(2) 0.0169(4) Uani 1 1 d . . . C1 C 0.5989(3) 0.11682(11) 0.5292(3) 0.0171(5) Uani 1 1 d . . . C2 C 0.4849(3) 0.16236(12) 0.5179(3) 0.0206(5) Uani 1 1 d . . . H1 H 0.3798 0.1515 0.5024 0.026 Uiso 1 1 d . . . C3 C 0.5322(3) 0.22279(12) 0.5342(3) 0.0236(6) Uani 1 1 d . . . C4 C 0.6907(4) 0.23950(12) 0.5607(3) 0.0265(6) Uani 1 1 d . . . H2 H 0.7323 0.2785 0.5847 0.032 Uiso 1 1 d . . . C5 C 0.8033(3) 0.19442(12) 0.5712(3) 0.0230(6) Uani 1 1 d . . . C6 C 0.7595(3) 0.13388(11) 0.5559(3) 0.0189(5) Uani 1 1 d . . . H3 H 0.8435 0.1041 0.5666 0.024 Uiso 1 1 d . . . C7 C 0.4065(4) 0.27018(14) 0.5247(4) 0.0366(8) Uani 1 1 d . . . C8 C 0.9762(4) 0.21125(14) 0.6010(4) 0.0354(8) Uani 1 1 d . . . C9 C 0.4745(3) 0.05782(12) 0.8203(3) 0.0195(5) Uani 1 1 d . . . C10 C 0.3387(3) 0.01991(12) 0.8013(3) 0.0192(5) Uani 1 1 d . . . C11 C 0.3865(3) -0.04092(11) 0.7925(3) 0.0187(5) Uani 1 1 d . . . C12 C 0.5522(3) -0.04080(12) 0.8063(3) 0.0190(5) Uani 1 1 d . . . C13 C 0.6063(3) 0.02064(12) 0.8230(3) 0.0183(5) Uani 1 1 d . . . C14 C 0.4753(4) 0.12494(12) 0.8397(3) 0.0257(6) Uani 1 1 d . . . H4 H 0.4760 0.1346 0.9267 0.032 Uiso 1 1 d . . . H5 H 0.3907 0.1452 0.7821 0.032 Uiso 1 1 d . . . H6 H 0.5611 0.1445 0.8204 0.032 Uiso 1 1 d . . . C15 C 0.1762(3) 0.03958(13) 0.7995(3) 0.0235(6) Uani 1 1 d . . . H7 H 0.1747 0.0366 0.9002 0.029 Uiso 1 1 d . . . H8 H 0.0985 0.0192 0.7404 0.029 Uiso 1 1 d . . . H9 H 0.1670 0.0780 0.7746 0.029 Uiso 1 1 d . . . C16 C 0.2790(4) -0.09486(13) 0.7788(3) 0.0253(6) Uani 1 1 d . . . H10 H 0.2540 -0.0997 0.8659 0.030 Uiso 1 1 calc R . . H11 H 0.3338 -0.1312 0.7628 0.030 Uiso 1 1 calc R . . H12 H 0.1792 -0.0889 0.6989 0.030 Uiso 1 1 calc R . . C17 C 0.6569(3) -0.09500(13) 0.8130(3) 0.0236(6) Uani 1 1 d . . . H13 H 0.7182 -0.1044 0.9120 0.028 Uiso 1 1 calc R . . H14 H 0.7313 -0.0863 0.7623 0.028 Uiso 1 1 calc R . . H15 H 0.5895 -0.1297 0.7691 0.028 Uiso 1 1 calc R . . C18 C 0.7757(3) 0.04052(13) 0.8473(3) 0.0245(6) Uani 1 1 d . . . H16 H 0.8497 0.0379 0.9465 0.030 Uiso 1 1 d . . . H17 H 0.7827 0.0799 0.8232 0.030 Uiso 1 1 d . . . H18 H 0.8287 0.0198 0.7972 0.030 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0155(3) 0.0125(2) 0.0160(2) 0.00016(15) 0.00498(18) -0.00042(15) Cl1 0.0169(3) 0.0277(3) 0.0223(3) 0.0021(2) 0.0047(2) 0.0032(2) F1 0.0594(15) 0.0522(14) 0.0758(17) -0.0024(12) 0.0412(14) 0.0214(12) F2 0.0453(13) 0.0552(14) 0.0699(16) -0.0010(12) 0.0006(12) 0.0300(11) F3 0.0519(15) 0.0149(9) 0.187(3) 0.0080(14) 0.0611(19) 0.0058(9) F4 0.0339(14) 0.120(3) 0.129(3) 0.052(2) -0.0109(16) -0.0193(16) F5 0.0338(12) 0.0194(10) 0.168(3) 0.0030(14) 0.0358(15) -0.0074(9) F6 0.0599(17) 0.087(2) 0.218(4) -0.094(3) 0.095(2) -0.0445(16) N1 0.0192(11) 0.0128(10) 0.0185(10) 0.0011(8) 0.0062(8) -0.0016(8) C1 0.0205(12) 0.0138(11) 0.0170(11) 0.0010(9) 0.0066(9) -0.0013(9) C2 0.0174(12) 0.0185(12) 0.0266(13) 0.0019(10) 0.0085(10) 0.0012(10) C3 0.0231(14) 0.0154(12) 0.0333(14) 0.0004(10) 0.0108(11) 0.0021(10) C4 0.0299(15) 0.0119(12) 0.0389(16) -0.0027(11) 0.0131(13) -0.0021(10) C5 0.0220(14) 0.0159(12) 0.0329(14) -0.0016(10) 0.0116(11) -0.0028(10) C6 0.0189(12) 0.0143(12) 0.0240(12) 0.0002(9) 0.0079(10) 0.0002(9) C7 0.0282(16) 0.0181(14) 0.065(2) 0.0003(14) 0.0176(16) 0.0027(12) C8 0.0224(15) 0.0193(13) 0.065(2) -0.0060(14) 0.0152(15) -0.0026(11) C9 0.0232(13) 0.0187(12) 0.0149(11) -0.0016(9) 0.0043(10) -0.0029(10) C10 0.0207(13) 0.0215(13) 0.0161(11) 0.0011(9) 0.0069(10) 0.0005(10) C11 0.0215(13) 0.0179(12) 0.0167(12) 0.0011(9) 0.0063(10) -0.0020(10) C12 0.0216(13) 0.0189(12) 0.0153(11) 0.0029(9) 0.0045(10) 0.0002(10) C13 0.0190(13) 0.0209(12) 0.0129(11) -0.0004(9) 0.0028(9) -0.0027(10) C14 0.0339(15) 0.0185(13) 0.0233(13) -0.0037(10) 0.0080(11) -0.0014(11) C15 0.0221(13) 0.0273(14) 0.0226(13) -0.0014(11) 0.0093(11) -0.0003(11) C16 0.0276(14) 0.0235(13) 0.0251(13) 0.0011(11) 0.0095(11) -0.0064(11) C17 0.0243(13) 0.0237(13) 0.0208(13) 0.0052(10) 0.0053(11) 0.0067(11) C18 0.0185(13) 0.0304(15) 0.0223(13) 0.0000(11) 0.0041(10) -0.0040(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N1 1.920(2) 3_656 ? Ti1 N1 1.954(2) . ? Ti1 Cl1 2.2957(8) . ? Ti1 C13 2.341(2) . ? Ti1 C12 2.351(2) . ? Ti1 C9 2.377(3) . ? Ti1 C11 2.384(3) . ? Ti1 C10 2.402(3) . ? Ti1 Ti1 2.8390(10) 3_656 ? F1 C7 1.332(4) . ? F2 C7 1.325(4) . ? F3 C7 1.325(4) . ? F4 C8 1.357(5) . ? F5 C8 1.297(4) . ? F6 C8 1.264(4) . ? N1 C1 1.396(3) . ? N1 Ti1 1.920(2) 3_656 ? C1 C2 1.402(4) . ? C1 C6 1.405(4) . ? C2 C3 1.393(4) . ? C3 C4 1.386(4) . ? C3 C7 1.507(4) . ? C4 C5 1.388(4) . ? C5 C6 1.388(4) . ? C5 C8 1.502(4) . ? C9 C13 1.419(4) . ? C9 C10 1.423(4) . ? C9 C14 1.497(4) . ? C10 C11 1.422(4) . ? C10 C15 1.496(4) . ? C11 C12 1.424(4) . ? C11 C16 1.502(4) . ? C12 C13 1.431(4) . ? C12 C17 1.502(4) . ? C13 C18 1.500(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 N1 Ti1 N1 85.74(9) 3_656 . ? N1 Ti1 Cl1 105.27(7) 3_656 . ? N1 Ti1 Cl1 103.25(7) . . ? N1 Ti1 C13 116.05(9) 3_656 . ? N1 Ti1 C13 91.26(9) . . ? Cl1 Ti1 C13 137.09(7) . . ? N1 Ti1 C12 90.74(9) 3_656 . ? N1 Ti1 C12 115.18(9) . . ? Cl1 Ti1 C12 139.38(7) . . ? C13 Ti1 C12 35.52(9) . . ? N1 Ti1 C9 148.76(9) 3_656 . ? N1 Ti1 C9 102.46(9) . . ? Cl1 Ti1 C9 102.09(7) . . ? C13 Ti1 C9 35.00(9) . . ? C12 Ti1 C9 58.36(9) . . ? N1 Ti1 C11 100.28(9) 3_656 . ? N1 Ti1 C11 148.76(9) . . ? Cl1 Ti1 C11 104.58(7) . . ? C13 Ti1 C11 58.42(9) . . ? C12 Ti1 C11 35.00(9) . . ? C9 Ti1 C11 57.85(9) . . ? N1 Ti1 C10 133.76(9) 3_656 . ? N1 Ti1 C10 136.37(9) . . ? Cl1 Ti1 C10 85.41(7) . . ? C13 Ti1 C10 58.05(9) . . ? C12 Ti1 C10 57.98(9) . . ? C9 Ti1 C10 34.65(9) . . ? C11 Ti1 C10 34.56(9) . . ? N1 Ti1 Ti1 43.34(7) 3_656 3_656 ? N1 Ti1 Ti1 42.40(6) . 3_656 ? Cl1 Ti1 Ti1 109.62(3) . 3_656 ? C13 Ti1 Ti1 108.18(7) . 3_656 ? C12 Ti1 Ti1 107.55(7) . 3_656 ? C9 Ti1 Ti1 136.60(7) . 3_656 ? C11 Ti1 Ti1 135.16(7) . 3_656 ? C10 Ti1 Ti1 164.96(7) . 3_656 ? C1 N1 Ti1 136.07(18) . 3_656 ? C1 N1 Ti1 129.50(18) . . ? Ti1 N1 Ti1 94.26(9) 3_656 . ? N1 C1 C2 121.0(2) . . ? N1 C1 C6 120.6(2) . . ? C2 C1 C6 118.4(2) . . ? C3 C2 C1 120.0(2) . . ? C4 C3 C2 121.5(2) . . ? C4 C3 C7 120.2(2) . . ? C2 C3 C7 118.3(3) . . ? C3 C4 C5 118.5(2) . . ? C6 C5 C4 121.2(3) . . ? C6 C5 C8 119.2(2) . . ? C4 C5 C8 119.5(2) . . ? C5 C6 C1 120.4(2) . . ? F3 C7 F2 108.1(3) . . ? F3 C7 F1 106.8(3) . . ? F2 C7 F1 105.1(3) . . ? F3 C7 C3 112.5(3) . . ? F2 C7 C3 112.1(3) . . ? F1 C7 C3 111.8(3) . . ? F6 C8 F5 112.0(3) . . ? F6 C8 F4 100.6(4) . . ? F5 C8 F4 103.3(3) . . ? F6 C8 C5 114.7(3) . . ? F5 C8 C5 114.0(3) . . ? F4 C8 C5 110.8(3) . . ? C13 C9 C10 108.2(2) . . ? C13 C9 C14 127.2(3) . . ? C10 C9 C14 124.6(3) . . ? C13 C9 Ti1 71.13(14) . . ? C10 C9 Ti1 73.62(14) . . ? C14 C9 Ti1 122.93(18) . . ? C11 C10 C9 108.1(2) . . ? C11 C10 C15 125.4(2) . . ? C9 C10 C15 126.4(2) . . ? C11 C10 Ti1 72.06(15) . . ? C9 C10 Ti1 71.73(15) . . ? C15 C10 Ti1 124.71(18) . . ? C10 C11 C12 108.1(2) . . ? C10 C11 C16 124.4(2) . . ? C12 C11 C16 127.5(2) . . ? C10 C11 Ti1 73.38(15) . . ? C12 C11 Ti1 71.21(14) . . ? C16 C11 Ti1 123.65(18) . . ? C11 C12 C13 107.8(2) . . ? C11 C12 C17 127.0(2) . . ? C13 C12 C17 125.1(2) . . ? C11 C12 Ti1 73.79(14) . . ? C13 C12 Ti1 71.89(14) . . ? C17 C12 Ti1 123.26(18) . . ? C9 C13 C12 107.9(2) . . ? C9 C13 C18 127.0(2) . . ? C12 C13 C18 125.0(2) . . ? C9 C13 Ti1 73.86(14) . . ? C12 C13 Ti1 72.60(14) . . ? C18 C13 Ti1 121.93(18) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.253 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.100 data_shelxl _database_code_depnum_ccdc_archive 'CCDC 811937' #TrackingRef '5a_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 5a _chemical_melting_point ? _chemical_formula_moiety 'C26 H16 Cl2 F12 N2 Ti2, C10 H10 Co, 2(C1 H2 Cl2)' _chemical_formula_sum 'C38 H30 Cl6 Co F12 N2 Ti2' _chemical_formula_weight 1110.07 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.139(12) _cell_length_b 11.696(7) _cell_length_c 21.035(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.064(7) _cell_angle_gamma 90.00 _cell_volume 4456(5) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 7677 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2212 _exptl_absorpt_coefficient_mu 1.159 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5480 _exptl_absorpt_correction_T_max 0.7604 _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41425 _diffrn_reflns_av_R_equivalents 0.0867 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.43 _reflns_number_total 10099 _reflns_number_gt 6253 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'Il Milione (Burla, et al., 2007)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics ORTEP-III _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^)+(0.1489P)^2^+9.0337P] 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 10099 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1462 _refine_ls_R_factor_gt 0.0964 _refine_ls_wR_factor_ref 0.2932 _refine_ls_wR_factor_gt 0.2514 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 Co1 Co 0.25546(5) 0.25187(7) 0.25709(4) 0.0335(3) Uani 1 1 d . . . Ti1 Ti 0.93616(6) 0.56348(9) 0.50326(5) 0.0254(3) Uani 1 1 d . . . Ti2 Ti 0.56191(6) 0.56189(9) 0.48580(5) 0.0256(3) Uani 1 1 d . . . Cl1 Cl 0.89952(10) 0.63931(14) 0.40263(8) 0.0429(4) Uani 1 1 d . . . Cl2 Cl 0.61966(10) 0.64139(14) 0.57764(8) 0.0401(4) Uani 1 1 d . . . Cl3 Cl 0.97801(15) 0.1237(3) 0.30020(16) 0.0933(9) Uani 1 1 d . . . Cl4 Cl 0.96328(19) 0.3370(3) 0.22740(18) 0.1107(12) Uani 1 1 d . . . Cl5 Cl 0.5200(2) 0.2275(5) 0.28925(19) 0.156(2) Uani 1 1 d . . . Cl6 Cl 0.5269(2) 0.4132(3) 0.2018(2) 0.1327(16) Uani 1 1 d . . . F1 F 0.7617(5) 0.1498(5) 0.3092(3) 0.131(3) Uani 1 1 d . . . F2 F 0.7535(3) 0.3284(4) 0.3228(3) 0.0862(19) Uani 1 1 d . . . F3 F 0.6900(3) 0.2187(8) 0.3725(3) 0.133(3) Uani 1 1 d . . . F4 F 0.9028(3) -0.0870(4) 0.4790(3) 0.0679(14) Uani 1 1 d . . . F5 F 0.9496(3) -0.0040(4) 0.5603(2) 0.0647(13) Uani 1 1 d . . . F6 F 0.8324(3) -0.0298(4) 0.5494(3) 0.083(2) Uani 1 1 d . . . F7 F 0.8151(2) 0.2184(5) 0.6148(2) 0.0719(15) Uani 1 1 d . . . F8 F 0.7486(3) 0.3238(4) 0.6705(2) 0.0580(13) Uani 1 1 d . . . F9 F 0.7435(3) 0.1417(4) 0.6797(2) 0.0710(15) Uani 1 1 d . . . F10 F 0.6668(3) -0.0348(5) 0.4454(4) 0.107(3) Uani 1 1 d . . . F11 F 0.5919(4) -0.0842(4) 0.5107(3) 0.091(2) Uani 1 1 d . . . F12 F 0.5511(4) -0.0005(5) 0.4310(3) 0.113(3) Uani 1 1 d . . . N1 N 0.9591(3) 0.4052(4) 0.4859(2) 0.0269(10) Uani 1 1 d . . . N2 N 0.5423(3) 0.4057(4) 0.5102(2) 0.0267(10) Uani 1 1 d . . . C1 C 0.9161(3) 0.3112(5) 0.4694(3) 0.0255(12) Uani 1 1 d . . . C2 C 0.8600(3) 0.3182(5) 0.4201(3) 0.0303(13) Uani 1 1 d . . . H2 H 0.8512 0.3885 0.3984 0.036 Uiso 1 1 calc R . . C3 C 0.8174(3) 0.2213(5) 0.4032(3) 0.0331(14) Uani 1 1 d . . . C4 C 0.8279(3) 0.1186(5) 0.4357(3) 0.0340(14) Uani 1 1 d . . . H4 H 0.7985 0.0536 0.4248 0.041 Uiso 1 1 calc R . . C5 C 0.8819(3) 0.1131(5) 0.4840(3) 0.0305(13) Uani 1 1 d . . . C6 C 0.9266(3) 0.2065(5) 0.5012(3) 0.0298(13) Uani 1 1 d . . . H6 H 0.9640 0.1991 0.5343 0.036 Uiso 1 1 calc R . . C7 C 0.7596(5) 0.2297(6) 0.3514(4) 0.0501(19) Uani 1 1 d . . . C8 C 0.8911(4) -0.0003(5) 0.5187(4) 0.0408(16) Uani 1 1 d . . . C9 C 0.8773(4) 0.4963(6) 0.5939(3) 0.0440(17) Uani 1 1 d . . . H9 H 0.8828 0.4183 0.6058 0.053 Uiso 1 1 calc R . . C10 C 0.9243(4) 0.5875(6) 0.6144(3) 0.0422(16) Uani 1 1 d . . . H10 H 0.9663 0.5815 0.6431 0.051 Uiso 1 1 calc R . . C11 C 0.8981(4) 0.6873(6) 0.5850(3) 0.0413(16) Uani 1 1 d . . . H11 H 0.9197 0.7610 0.5898 0.050 Uiso 1 1 calc R . . C12 C 0.8347(4) 0.6608(7) 0.5475(4) 0.0462(18) Uani 1 1 d . . . H12 H 0.8056 0.7133 0.5226 0.055 Uiso 1 1 calc R . . C13 C 0.8214(4) 0.5416(8) 0.5532(4) 0.053(2) Uani 1 1 d . . . H13 H 0.7817 0.5002 0.5329 0.063 Uiso 1 1 calc R . . C14 C 0.5861(3) 0.3111(5) 0.5237(3) 0.0284(13) Uani 1 1 d . . . C15 C 0.6439(3) 0.3161(5) 0.5713(3) 0.0287(13) Uani 1 1 d . . . H15 H 0.6532 0.3860 0.5933 0.034 Uiso 1 1 calc R . . C16 C 0.6879(3) 0.2215(5) 0.5867(3) 0.0315(13) Uani 1 1 d . . . C17 C 0.6755(3) 0.1172(5) 0.5541(3) 0.0305(13) Uani 1 1 d . . . H17 H 0.7047 0.0518 0.5646 0.037 Uiso 1 1 calc R . . C18 C 0.6197(3) 0.1123(5) 0.5060(3) 0.0343(14) Uani 1 1 d . . . C19 C 0.5746(4) 0.2058(5) 0.4907(3) 0.0335(14) Uani 1 1 d . . . H19 H 0.5362 0.1992 0.4584 0.040 Uiso 1 1 calc R . . C20 C 0.7474(4) 0.2265(5) 0.6372(3) 0.0357(15) Uani 1 1 d . . . C21 C 0.6068(4) 0.0020(6) 0.4723(4) 0.0459(18) Uani 1 1 d . . . C22 C 0.5496(4) 0.5771(6) 0.3737(3) 0.0421(16) Uani 1 1 d . . . H22 H 0.5024 0.5666 0.3528 0.050 Uiso 1 1 calc R . . C23 C 0.5797(4) 0.6830(6) 0.3970(3) 0.0434(17) Uani 1 1 d . . . H23 H 0.5563 0.7556 0.3939 0.052 Uiso 1 1 calc R . . C24 C 0.6496(4) 0.6606(7) 0.4250(3) 0.0449(17) Uani 1 1 d . . . H24 H 0.6821 0.7152 0.4450 0.054 Uiso 1 1 calc R . . C25 C 0.6638(4) 0.5416(7) 0.4184(3) 0.0481(19) Uani 1 1 d . . . H25 H 0.7075 0.5024 0.4327 0.058 Uiso 1 1 calc R . . C26 C 0.6013(4) 0.4931(6) 0.3870(3) 0.0469(18) Uani 1 1 d . . . H26 H 0.5955 0.4145 0.3765 0.056 Uiso 1 1 calc R . . C27 C 0.3011(5) 0.3693(6) 0.1983(4) 0.0498(19) Uani 1 1 d . . . H27 H 0.3407 0.3578 0.1711 0.060 Uiso 1 1 calc R . . C28 C 0.2247(6) 0.3517(6) 0.1827(4) 0.063(3) Uani 1 1 d . . . H28 H 0.2041 0.3244 0.1431 0.076 Uiso 1 1 calc R . . C29 C 0.1841(5) 0.3821(7) 0.2365(6) 0.068(3) Uani 1 1 d . . . H29 H 0.1321 0.3801 0.2392 0.082 Uiso 1 1 calc R . . C30 C 0.2359(6) 0.4155(6) 0.2844(4) 0.063(2) Uani 1 1 d . . . H30 H 0.2251 0.4400 0.3260 0.075 Uiso 1 1 calc R . . C31 C 0.3065(5) 0.4066(6) 0.2608(4) 0.0470(18) Uani 1 1 d . . . H31 H 0.3514 0.4237 0.2842 0.056 Uiso 1 1 calc R . . C32 C 0.2331(6) 0.0867(6) 0.2345(4) 0.064(3) Uani 1 1 d . . . H32 H 0.2099 0.0609 0.1956 0.076 Uiso 1 1 calc R . . C33 C 0.1967(5) 0.1188(6) 0.2906(5) 0.059(2) Uani 1 1 d . . . H33 H 0.1450 0.1184 0.2957 0.071 Uiso 1 1 calc R . . C34 C 0.2514(5) 0.1507(6) 0.3363(3) 0.0468(18) Uani 1 1 d . . . H34 H 0.2430 0.1751 0.3784 0.056 Uiso 1 1 calc R . . C35 C 0.3203(4) 0.1413(6) 0.3107(3) 0.0422(16) Uani 1 1 d . . . H35 H 0.3663 0.1593 0.3320 0.051 Uiso 1 1 calc R . . C36 C 0.3101(5) 0.1004(5) 0.2477(3) 0.0458(18) Uani 1 1 d . . . H36 H 0.3479 0.0848 0.2194 0.055 Uiso 1 1 calc R . . C37 C 0.9552(6) 0.1897(9) 0.2246(5) 0.088(4) Uani 1 1 d . . . H37A H 0.9883 0.1593 0.1927 0.106 Uiso 1 1 calc R . . H37B H 0.9039 0.1692 0.2107 0.106 Uiso 1 1 calc R . . C38 C 0.5719(5) 0.2983(9) 0.2376(5) 0.077(3) Uani 1 1 d . . . H38A H 0.5866 0.2445 0.2042 0.093 Uiso 1 1 calc R . . H38B H 0.6175 0.3258 0.2607 0.093 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 Co1 0.0445(5) 0.0205(4) 0.0360(5) -0.0001(3) 0.0066(4) 0.0024(3) Ti1 0.0288(5) 0.0198(5) 0.0275(5) -0.0014(4) 0.0011(4) 0.0011(4) Ti2 0.0321(6) 0.0189(5) 0.0256(5) 0.0012(4) 0.0007(4) 0.0003(4) Cl1 0.0578(11) 0.0334(9) 0.0359(9) 0.0046(7) -0.0115(7) 0.0022(8) Cl2 0.0484(9) 0.0333(9) 0.0374(8) -0.0064(7) -0.0086(7) -0.0022(7) Cl3 0.0717(17) 0.098(2) 0.107(2) -0.0084(17) -0.0180(15) 0.0067(15) Cl4 0.115(2) 0.087(2) 0.125(3) -0.0089(19) -0.047(2) -0.0055(18) Cl5 0.118(3) 0.245(5) 0.102(3) 0.059(3) -0.032(2) -0.100(3) Cl6 0.125(3) 0.096(2) 0.167(4) 0.023(2) -0.085(3) -0.035(2) F1 0.206(8) 0.073(4) 0.102(5) -0.051(4) -0.097(5) 0.057(5) F2 0.110(4) 0.051(3) 0.090(4) 0.019(3) -0.061(3) -0.024(3) F3 0.061(4) 0.237(9) 0.095(5) 0.059(6) -0.032(4) -0.036(5) F4 0.095(4) 0.025(2) 0.085(4) 0.005(2) 0.011(3) 0.019(2) F5 0.081(3) 0.037(3) 0.073(3) 0.018(2) -0.022(3) -0.002(2) F6 0.055(3) 0.057(3) 0.143(5) 0.063(3) 0.056(3) 0.025(2) F7 0.033(2) 0.117(4) 0.065(3) -0.018(3) -0.004(2) 0.012(3) F8 0.073(3) 0.039(2) 0.059(3) -0.011(2) -0.033(2) 0.015(2) F9 0.104(4) 0.046(3) 0.059(3) 0.024(2) -0.030(3) -0.012(3) F10 0.084(4) 0.080(4) 0.164(6) -0.086(4) 0.067(4) -0.040(3) F11 0.140(5) 0.031(3) 0.106(5) -0.014(3) 0.029(4) -0.032(3) F12 0.145(6) 0.057(4) 0.127(5) -0.050(3) -0.077(5) 0.031(4) N1 0.031(3) 0.023(2) 0.027(2) 0.0001(19) 0.003(2) -0.0029(19) N2 0.039(3) 0.019(2) 0.022(2) 0.0021(18) 0.002(2) 0.002(2) C1 0.030(3) 0.019(3) 0.028(3) -0.001(2) 0.008(2) -0.002(2) C2 0.037(3) 0.024(3) 0.030(3) -0.003(2) 0.004(3) -0.001(2) C3 0.037(3) 0.026(3) 0.036(3) -0.002(3) 0.002(3) -0.001(3) C4 0.037(3) 0.022(3) 0.043(4) -0.003(3) 0.002(3) -0.006(3) C5 0.032(3) 0.017(3) 0.044(4) 0.001(2) 0.005(3) 0.001(2) C6 0.031(3) 0.024(3) 0.035(3) 0.000(2) 0.000(3) 0.002(2) C7 0.059(5) 0.041(4) 0.048(4) 0.000(3) -0.012(4) -0.021(4) C8 0.042(4) 0.020(3) 0.060(5) 0.007(3) 0.004(3) 0.005(3) C9 0.060(5) 0.039(4) 0.035(4) 0.001(3) 0.022(3) -0.001(3) C10 0.045(4) 0.052(4) 0.030(3) -0.004(3) 0.009(3) 0.006(3) C11 0.046(4) 0.034(4) 0.046(4) -0.011(3) 0.012(3) -0.001(3) C12 0.036(4) 0.053(5) 0.050(4) -0.005(3) 0.012(3) 0.024(3) C13 0.030(4) 0.076(6) 0.052(5) -0.012(4) 0.008(3) -0.005(4) C14 0.038(3) 0.016(3) 0.032(3) 0.002(2) 0.006(3) 0.001(2) C15 0.038(3) 0.018(3) 0.030(3) 0.001(2) 0.003(3) 0.005(2) C16 0.037(3) 0.027(3) 0.031(3) 0.004(2) 0.004(3) 0.005(3) C17 0.034(3) 0.015(3) 0.042(4) 0.006(2) 0.004(3) 0.009(2) C18 0.034(3) 0.028(3) 0.040(4) -0.001(3) 0.001(3) -0.003(3) C19 0.038(3) 0.028(3) 0.035(3) -0.001(3) 0.009(3) 0.000(3) C20 0.045(4) 0.025(3) 0.036(3) 0.004(3) -0.008(3) 0.007(3) C21 0.043(4) 0.029(4) 0.066(5) -0.006(3) 0.004(4) -0.001(3) C22 0.042(4) 0.053(4) 0.032(3) 0.010(3) 0.001(3) -0.005(3) C23 0.061(5) 0.033(4) 0.038(4) 0.015(3) 0.018(3) 0.010(3) C24 0.045(4) 0.051(5) 0.040(4) -0.001(3) 0.010(3) -0.012(3) C25 0.048(4) 0.061(5) 0.037(4) 0.008(3) 0.019(3) 0.021(4) C26 0.074(5) 0.031(4) 0.037(4) 0.000(3) 0.021(4) -0.005(4) C27 0.077(6) 0.036(4) 0.038(4) 0.003(3) 0.020(4) 0.004(4) C28 0.100(7) 0.027(4) 0.059(5) 0.013(4) -0.030(5) -0.013(4) C29 0.060(5) 0.033(4) 0.114(8) 0.030(5) 0.018(6) 0.012(4) C30 0.103(7) 0.025(4) 0.063(5) 0.004(4) 0.033(5) 0.010(4) C31 0.069(5) 0.026(3) 0.046(4) 0.002(3) 0.000(4) -0.004(3) C32 0.104(7) 0.017(3) 0.065(6) -0.001(3) -0.034(5) -0.004(4) C33 0.051(5) 0.027(4) 0.100(7) 0.019(4) 0.010(5) 0.000(3) C34 0.074(5) 0.032(4) 0.036(4) 0.005(3) 0.019(4) 0.008(4) C35 0.057(4) 0.032(4) 0.038(4) 0.004(3) -0.003(3) 0.016(3) C36 0.076(5) 0.021(3) 0.040(4) 0.007(3) 0.010(4) 0.017(3) C37 0.092(8) 0.074(7) 0.094(8) -0.028(6) -0.043(6) 0.005(6) C38 0.056(5) 0.101(8) 0.074(6) -0.017(6) 0.001(5) 0.014(5) _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 Co1 C28 2.008(8) . ? Co1 C32 2.026(7) . ? Co1 C29 2.030(8) . ? Co1 C31 2.033(7) . ? Co1 C33 2.034(8) . ? Co1 C30 2.035(8) . ? Co1 C36 2.045(7) . ? Co1 C35 2.046(6) . ? Co1 C34 2.048(7) . ? Co1 C27 2.053(7) . ? Ti1 N1 1.937(5) 3_766 ? Ti1 N1 1.937(5) . ? Ti1 Cl1 2.358(2) . ? Ti1 C9 2.369(7) . ? Ti1 C10 2.375(7) . ? Ti1 C11 2.379(7) . ? Ti1 C12 2.394(6) . ? Ti1 C13 2.394(7) . ? Ti1 Ti1 2.761(2) 3_766 ? Ti2 N2 1.934(5) 3_666 ? Ti2 N2 1.936(5) . ? Ti2 Cl2 2.340(2) . ? Ti2 C22 2.363(7) . ? Ti2 C26 2.373(7) . ? Ti2 C23 2.380(6) . ? Ti2 C24 2.391(7) . ? Ti2 C25 2.400(7) . ? Ti2 Ti2 2.764(2) 3_666 ? Cl3 C37 1.795(11) . ? Cl4 C37 1.730(11) . ? Cl5 C38 1.692(11) . ? Cl6 C38 1.724(11) . ? F1 C7 1.291(9) . ? F2 C7 1.304(9) . ? F3 C7 1.367(10) . ? F4 C8 1.338(8) . ? F5 C8 1.339(8) . ? F6 C8 1.320(8) . ? F7 C20 1.342(8) . ? F8 C20 1.336(7) . ? F9 C20 1.340(7) . ? F10 C21 1.326(8) . ? F11 C21 1.328(9) . ? F12 C21 1.297(9) . ? N1 C1 1.381(7) . ? N1 Ti1 1.936(5) 3_766 ? N2 C14 1.382(7) . ? N2 Ti2 1.934(5) 3_666 ? C1 C6 1.404(8) . ? C1 C2 1.415(8) . ? C2 C3 1.407(8) . ? C2 H2 0.9500 . ? C3 C4 1.391(9) . ? C3 C7 1.476(10) . ? C4 C5 1.374(9) . ? C4 H4 0.9500 . ? C5 C6 1.396(8) . ? C5 C8 1.518(8) . ? C6 H6 0.9500 . ? C9 C13 1.396(11) . ? C9 C10 1.418(10) . ? C9 H9 0.9500 . ? C10 C11 1.392(10) . ? C10 H10 0.9500 . ? C11 C12 1.393(10) . ? C11 H11 0.9500 . ? C12 C13 1.421(11) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.413(8) . ? C14 C19 1.423(8) . ? C15 C16 1.392(8) . ? C15 H15 0.9500 . ? C16 C17 1.413(8) . ? C16 C20 1.474(9) . ? C17 C18 1.394(9) . ? C17 H17 0.9500 . ? C18 C19 1.393(9) . ? C18 C21 1.483(9) . ? C19 H19 0.9500 . ? C22 C26 1.377(10) . ? C22 C23 1.429(10) . ? C22 H22 0.9500 . ? C23 C24 1.394(10) . ? C23 H23 0.9500 . ? C24 C25 1.424(11) . ? C24 H24 0.9500 . ? C25 C26 1.401(11) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C31 1.384(10) . ? C27 C28 1.423(12) . ? C27 H27 0.9500 . ? C28 C29 1.427(13) . ? C28 H28 0.9500 . ? C29 C30 1.396(14) . ? C29 H29 0.9500 . ? C30 C31 1.402(12) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C36 1.419(12) . ? C32 C33 1.432(13) . ? C32 H32 0.9500 . ? C33 C34 1.397(12) . ? C33 H33 0.9500 . ? C34 C35 1.390(10) . ? C34 H34 0.9500 . ? C35 C36 1.412(10) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? 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 C28 Co1 C32 109.2(3) . . ? C28 Co1 C29 41.4(4) . . ? C32 Co1 C29 123.3(4) . . ? C28 Co1 C31 67.6(3) . . ? C32 Co1 C31 160.7(4) . . ? C29 Co1 C31 67.9(4) . . ? C28 Co1 C33 125.9(4) . . ? C32 Co1 C33 41.3(4) . . ? C29 Co1 C33 108.0(3) . . ? C31 Co1 C33 156.1(4) . . ? C28 Co1 C30 68.2(4) . . ? C32 Co1 C30 158.1(4) . . ? C29 Co1 C30 40.2(4) . . ? C31 Co1 C30 40.3(3) . . ? C33 Co1 C30 121.3(4) . . ? C28 Co1 C36 123.0(4) . . ? C32 Co1 C36 40.8(3) . . ? C29 Co1 C36 159.4(4) . . ? C31 Co1 C36 123.6(3) . . ? C33 Co1 C36 68.6(3) . . ? C30 Co1 C36 159.2(4) . . ? C28 Co1 C35 157.7(4) . . ? C32 Co1 C35 68.2(3) . . ? C29 Co1 C35 158.9(4) . . ? C31 Co1 C35 107.1(3) . . ? C33 Co1 C35 67.8(3) . . ? C30 Co1 C35 122.8(4) . . ? C36 Co1 C35 40.4(3) . . ? C28 Co1 C34 161.7(4) . . ? C32 Co1 C34 67.9(3) . . ? C29 Co1 C34 123.9(4) . . ? C31 Co1 C34 121.3(3) . . ? C33 Co1 C34 40.0(3) . . ? C30 Co1 C34 107.4(3) . . ? C36 Co1 C34 67.4(3) . . ? C35 Co1 C34 39.7(3) . . ? C28 Co1 C27 41.0(3) . . ? C32 Co1 C27 125.4(4) . . ? C29 Co1 C27 69.0(3) . . ? C31 Co1 C27 39.6(3) . . ? C33 Co1 C27 163.1(4) . . ? C30 Co1 C27 67.9(3) . . ? C36 Co1 C27 108.0(3) . . ? C35 Co1 C27 121.1(3) . . ? C34 Co1 C27 155.5(3) . . ? N1 Ti1 N1 89.1(2) 3_766 . ? N1 Ti1 Cl1 105.22(16) 3_766 . ? N1 Ti1 Cl1 104.07(16) . . ? N1 Ti1 C9 116.7(2) 3_766 . ? N1 Ti1 C9 86.9(2) . . ? Cl1 Ti1 C9 136.9(2) . . ? N1 Ti1 C10 90.1(2) 3_766 . ? N1 Ti1 C10 109.3(2) . . ? Cl1 Ti1 C10 143.41(19) . . ? C9 Ti1 C10 34.8(2) . . ? N1 Ti1 C11 96.9(2) 3_766 . ? N1 Ti1 C11 142.4(2) . . ? Cl1 Ti1 C11 109.96(19) . . ? C9 Ti1 C11 57.3(2) . . ? C10 Ti1 C11 34.1(2) . . ? N1 Ti1 C12 129.3(2) 3_766 . ? N1 Ti1 C12 134.9(2) . . ? Cl1 Ti1 C12 89.1(2) . . ? C9 Ti1 C12 57.0(3) . . ? C10 Ti1 C12 56.5(2) . . ? C11 Ti1 C12 33.9(2) . . ? N1 Ti1 C13 147.0(2) 3_766 . ? N1 Ti1 C13 100.4(3) . . ? Cl1 Ti1 C13 102.9(2) . . ? C9 Ti1 C13 34.1(3) . . ? C10 Ti1 C13 56.9(3) . . ? C11 Ti1 C13 57.0(3) . . ? C12 Ti1 C13 34.5(3) . . ? N1 Ti1 Ti1 44.55(15) 3_766 3_766 ? N1 Ti1 Ti1 44.54(14) . 3_766 ? Cl1 Ti1 Ti1 110.78(8) . 3_766 ? C9 Ti1 Ti1 106.07(19) . 3_766 ? C10 Ti1 Ti1 103.48(18) . 3_766 ? C11 Ti1 Ti1 129.80(19) . 3_766 ? C12 Ti1 Ti1 159.9(2) . 3_766 ? C13 Ti1 Ti1 135.7(2) . 3_766 ? N2 Ti2 N2 88.8(2) 3_666 . ? N2 Ti2 Cl2 106.33(15) 3_666 . ? N2 Ti2 Cl2 103.71(15) . . ? N2 Ti2 C22 89.3(2) 3_666 . ? N2 Ti2 C22 109.0(2) . . ? Cl2 Ti2 C22 143.89(19) . . ? N2 Ti2 C26 116.5(2) 3_666 . ? N2 Ti2 C26 88.8(2) . . ? Cl2 Ti2 C26 135.6(2) . . ? C22 Ti2 C26 33.8(2) . . ? N2 Ti2 C23 95.3(2) 3_666 . ? N2 Ti2 C23 143.5(2) . . ? Cl2 Ti2 C23 109.7(2) . . ? C22 Ti2 C23 35.1(2) . . ? C26 Ti2 C23 57.0(2) . . ? N2 Ti2 C24 127.5(2) 3_666 . ? N2 Ti2 C24 137.3(2) . . ? Cl2 Ti2 C24 88.17(19) . . ? C22 Ti2 C24 57.3(2) . . ? C26 Ti2 C24 57.0(3) . . ? C23 Ti2 C24 34.0(2) . . ? N2 Ti2 C25 146.2(2) 3_666 . ? N2 Ti2 C25 102.8(2) . . ? Cl2 Ti2 C25 101.6(2) . . ? C22 Ti2 C25 56.9(3) . . ? C26 Ti2 C25 34.1(3) . . ? C23 Ti2 C25 56.9(2) . . ? C24 Ti2 C25 34.6(3) . . ? N2 Ti2 Ti2 44.44(15) 3_666 3_666 ? N2 Ti2 Ti2 44.40(15) . 3_666 ? Cl2 Ti2 Ti2 111.27(8) . 3_666 ? C22 Ti2 Ti2 102.74(18) . 3_666 ? C26 Ti2 Ti2 107.32(19) . 3_666 ? C23 Ti2 Ti2 128.9(2) . 3_666 ? C24 Ti2 Ti2 160.07(19) . 3_666 ? C25 Ti2 Ti2 137.4(2) . 3_666 ? C1 N1 Ti1 135.9(4) . 3_766 ? C1 N1 Ti1 133.1(4) . . ? Ti1 N1 Ti1 90.9(2) 3_766 . ? C14 N2 Ti2 134.4(4) . 3_666 ? C14 N2 Ti2 134.3(4) . . ? Ti2 N2 Ti2 91.2(2) 3_666 . ? N1 C1 C6 121.0(5) . . ? N1 C1 C2 120.8(5) . . ? C6 C1 C2 118.2(5) . . ? C3 C2 C1 120.2(6) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 120.8(6) . . ? C4 C3 C7 119.6(6) . . ? C2 C3 C7 119.5(6) . . ? C5 C4 C3 118.5(6) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C4 C5 C6 122.4(5) . . ? C4 C5 C8 116.9(5) . . ? C6 C5 C8 120.8(6) . . ? C5 C6 C1 119.9(5) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? F1 C7 F2 109.2(7) . . ? F1 C7 F3 102.6(8) . . ? F2 C7 F3 100.2(7) . . ? F1 C7 C3 114.5(7) . . ? F2 C7 C3 116.0(6) . . ? F3 C7 C3 112.6(7) . . ? F6 C8 F4 105.4(6) . . ? F6 C8 F5 107.7(6) . . ? F4 C8 F5 103.6(5) . . ? F6 C8 C5 113.1(5) . . ? F4 C8 C5 112.3(6) . . ? F5 C8 C5 113.9(5) . . ? C13 C9 C10 107.8(7) . . ? C13 C9 Ti1 73.9(4) . . ? C10 C9 Ti1 72.9(4) . . ? C13 C9 H9 126.1 . . ? C10 C9 H9 126.1 . . ? Ti1 C9 H9 119.0 . . ? C11 C10 C9 108.2(6) . . ? C11 C10 Ti1 73.1(4) . . ? C9 C10 Ti1 72.4(4) . . ? C11 C10 H10 125.9 . . ? C9 C10 H10 125.9 . . ? Ti1 C10 H10 120.4 . . ? C12 C11 C10 108.4(6) . . ? C12 C11 Ti1 73.6(4) . . ? C10 C11 Ti1 72.8(4) . . ? C12 C11 H11 125.8 . . ? C10 C11 H11 125.8 . . ? Ti1 C11 H11 119.6 . . ? C11 C12 C13 108.0(7) . . ? C11 C12 Ti1 72.4(4) . . ? C13 C12 Ti1 72.7(4) . . ? C11 C12 H12 126.0 . . ? C13 C12 H12 126.0 . . ? Ti1 C12 H12 120.6 . . ? C9 C13 C12 107.6(7) . . ? C9 C13 Ti1 72.0(4) . . ? C12 C13 Ti1 72.7(4) . . ? C9 C13 H13 126.2 . . ? C12 C13 H13 126.2 . . ? Ti1 C13 H13 120.9 . . ? N2 C14 C15 120.6(5) . . ? N2 C14 C19 121.7(6) . . ? C15 C14 C19 117.7(5) . . ? C16 C15 C14 121.8(5) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C17 120.0(6) . . ? C15 C16 C20 121.7(6) . . ? C17 C16 C20 118.3(5) . . ? C18 C17 C16 118.6(5) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? C19 C18 C17 122.0(6) . . ? C19 C18 C21 119.8(6) . . ? C17 C18 C21 118.2(6) . . ? C18 C19 C14 119.9(6) . . ? C18 C19 H19 120.0 . . ? C14 C19 H19 120.0 . . ? F8 C20 F9 106.3(6) . . ? F8 C20 F7 104.8(6) . . ? F9 C20 F7 105.4(6) . . ? F8 C20 C16 113.6(5) . . ? F9 C20 C16 112.8(6) . . ? F7 C20 C16 113.2(6) . . ? F12 C21 F10 109.5(7) . . ? F12 C21 F11 102.3(7) . . ? F10 C21 F11 102.2(6) . . ? F12 C21 C18 115.9(6) . . ? F10 C21 C18 112.0(6) . . ? F11 C21 C18 113.7(7) . . ? C26 C22 C23 107.8(6) . . ? C26 C22 Ti2 73.5(4) . . ? C23 C22 Ti2 73.1(4) . . ? C26 C22 H22 126.1 . . ? C23 C22 H22 126.1 . . ? Ti2 C22 H22 119.1 . . ? C24 C23 C22 107.7(6) . . ? C24 C23 Ti2 73.4(4) . . ? C22 C23 Ti2 71.8(4) . . ? C24 C23 H23 126.1 . . ? C22 C23 H23 126.1 . . ? Ti2 C23 H23 120.4 . . ? C23 C24 C25 107.9(7) . . ? C23 C24 Ti2 72.6(4) . . ? C25 C24 Ti2 73.1(4) . . ? C23 C24 H24 126.0 . . ? C25 C24 H24 126.0 . . ? Ti2 C24 H24 120.1 . . ? C26 C25 C24 107.2(6) . . ? C26 C25 Ti2 71.9(4) . . ? C24 C25 Ti2 72.4(4) . . ? C26 C25 H25 126.4 . . ? C24 C25 H25 126.4 . . ? Ti2 C25 H25 121.1 . . ? C22 C26 C25 109.4(7) . . ? C22 C26 Ti2 72.7(4) . . ? C25 C26 Ti2 74.0(4) . . ? C22 C26 H26 125.3 . . ? C25 C26 H26 125.3 . . ? Ti2 C26 H26 119.8 . . ? C31 C27 C28 106.4(7) . . ? C31 C27 Co1 69.4(4) . . ? C28 C27 Co1 67.8(4) . . ? C31 C27 H27 126.8 . . ? C28 C27 H27 126.8 . . ? Co1 C27 H27 127.5 . . ? C27 C28 C29 108.5(8) . . ? C27 C28 Co1 71.2(4) . . ? C29 C28 Co1 70.1(5) . . ? C27 C28 H28 125.7 . . ? C29 C28 H28 125.7 . . ? Co1 C28 H28 124.6 . . ? C30 C29 C28 106.7(8) . . ? C30 C29 Co1 70.1(5) . . ? C28 C29 Co1 68.5(5) . . ? C30 C29 H29 126.6 . . ? C28 C29 H29 126.6 . . ? Co1 C29 H29 126.3 . . ? C29 C30 C31 108.3(8) . . ? C29 C30 Co1 69.7(5) . . ? C31 C30 Co1 69.7(4) . . ? C29 C30 H30 125.8 . . ? C31 C30 H30 125.8 . . ? Co1 C30 H30 126.3 . . ? C27 C31 C30 109.9(8) . . ? C27 C31 Co1 71.0(4) . . ? C30 C31 Co1 69.9(4) . . ? C27 C31 H31 125.0 . . ? C30 C31 H31 125.0 . . ? Co1 C31 H31 125.6 . . ? C36 C32 C33 107.6(7) . . ? C36 C32 Co1 70.3(4) . . ? C33 C32 Co1 69.6(4) . . ? C36 C32 H32 126.2 . . ? C33 C32 H32 126.2 . . ? Co1 C32 H32 125.4 . . ? C34 C33 C32 107.2(7) . . ? C34 C33 Co1 70.5(4) . . ? C32 C33 Co1 69.0(4) . . ? C34 C33 H33 126.4 . . ? C32 C33 H33 126.4 . . ? Co1 C33 H33 125.6 . . ? C35 C34 C33 109.4(7) . . ? C35 C34 Co1 70.1(4) . . ? C33 C34 Co1 69.4(4) . . ? C35 C34 H34 125.3 . . ? C33 C34 H34 125.3 . . ? Co1 C34 H34 126.8 . . ? C34 C35 C36 108.4(7) . . ? C34 C35 Co1 70.2(4) . . ? C36 C35 Co1 69.8(4) . . ? C34 C35 H35 125.8 . . ? C36 C35 H35 125.8 . . ? Co1 C35 H35 125.8 . . ? C35 C36 C32 107.5(7) . . ? C35 C36 Co1 69.9(4) . . ? C32 C36 Co1 68.9(4) . . ? C35 C36 H36 126.3 . . ? C32 C36 H36 126.3 . . ? Co1 C36 H36 126.6 . . ? Cl4 C37 Cl3 112.5(5) . . ? Cl4 C37 H37A 109.1 . . ? Cl3 C37 H37A 109.1 . . ? Cl4 C37 H37B 109.1 . . ? Cl3 C37 H37B 109.1 . . ? H37A C37 H37B 107.8 . . ? Cl5 C38 Cl6 113.3(6) . . ? Cl5 C38 H38A 108.9 . . ? Cl6 C38 H38A 108.9 . . ? Cl5 C38 H38B 108.9 . . ? Cl6 C38 H38B 108.9 . . ? H38A C38 H38B 107.7 . . ? 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 N1 Ti1 N1 C1 -177.4(6) 3_766 . . . ? Cl1 Ti1 N1 C1 -71.9(5) . . . . ? C9 Ti1 N1 C1 65.8(5) . . . . ? C10 Ti1 N1 C1 92.9(6) . . . . ? C11 Ti1 N1 C1 82.5(6) . . . . ? C12 Ti1 N1 C1 31.3(7) . . . . ? C13 Ti1 N1 C1 34.4(6) . . . . ? Ti1 Ti1 N1 C1 -177.4(6) 3_766 . . . ? N1 Ti1 N1 Ti1 0.0 3_766 . . 3_766 ? Cl1 Ti1 N1 Ti1 105.46(16) . . . 3_766 ? C9 Ti1 N1 Ti1 -116.8(2) . . . 3_766 ? C10 Ti1 N1 Ti1 -89.8(2) . . . 3_766 ? C11 Ti1 N1 Ti1 -100.2(4) . . . 3_766 ? C12 Ti1 N1 Ti1 -151.4(3) . . . 3_766 ? C13 Ti1 N1 Ti1 -148.2(2) . . . 3_766 ? N2 Ti2 N2 C14 -176.0(6) 3_666 . . . ? Cl2 Ti2 N2 C14 -69.5(5) . . . . ? C22 Ti2 N2 C14 95.1(6) . . . . ? C26 Ti2 N2 C14 67.5(6) . . . . ? C23 Ti2 N2 C14 86.7(6) . . . . ? C24 Ti2 N2 C14 33.0(7) . . . . ? C25 Ti2 N2 C14 36.1(6) . . . . ? Ti2 Ti2 N2 C14 -176.0(6) 3_666 . . . ? N2 Ti2 N2 Ti2 0.0 3_666 . . 3_666 ? Cl2 Ti2 N2 Ti2 106.53(15) . . . 3_666 ? C22 Ti2 N2 Ti2 -88.9(2) . . . 3_666 ? C26 Ti2 N2 Ti2 -116.5(2) . . . 3_666 ? C23 Ti2 N2 Ti2 -97.3(4) . . . 3_666 ? C24 Ti2 N2 Ti2 -151.0(3) . . . 3_666 ? C25 Ti2 N2 Ti2 -147.9(2) . . . 3_666 ? Ti1 N1 C1 C6 51.9(8) 3_766 . . . ? Ti1 N1 C1 C6 -131.8(5) . . . . ? Ti1 N1 C1 C2 -128.2(5) 3_766 . . . ? Ti1 N1 C1 C2 48.0(8) . . . . ? N1 C1 C2 C3 179.0(5) . . . . ? C6 C1 C2 C3 -1.2(9) . . . . ? C1 C2 C3 C4 2.0(9) . . . . ? C1 C2 C3 C7 -179.5(6) . . . . ? C2 C3 C4 C5 -1.2(9) . . . . ? C7 C3 C4 C5 -179.7(7) . . . . ? C3 C4 C5 C6 -0.4(10) . . . . ? C3 C4 C5 C8 179.4(6) . . . . ? C4 C5 C6 C1 1.2(9) . . . . ? C8 C5 C6 C1 -178.6(6) . . . . ? N1 C1 C6 C5 179.4(5) . . . . ? C2 C1 C6 C5 -0.4(8) . . . . ? C4 C3 C7 F1 -50.8(10) . . . . ? C2 C3 C7 F1 130.7(8) . . . . ? C4 C3 C7 F2 -179.4(7) . . . . ? C2 C3 C7 F2 2.1(11) . . . . ? C4 C3 C7 F3 66.0(9) . . . . ? C2 C3 C7 F3 -112.6(8) . . . . ? C4 C5 C8 F6 -63.7(9) . . . . ? C6 C5 C8 F6 116.2(7) . . . . ? C4 C5 C8 F4 55.5(8) . . . . ? C6 C5 C8 F4 -124.6(7) . . . . ? C4 C5 C8 F5 172.9(6) . . . . ? C6 C5 C8 F5 -7.2(9) . . . . ? N1 Ti1 C9 C13 158.7(4) 3_766 . . . ? N1 Ti1 C9 C13 -113.9(5) . . . . ? Cl1 Ti1 C9 C13 -6.5(6) . . . . ? C10 Ti1 C9 C13 114.9(7) . . . . ? C11 Ti1 C9 C13 78.1(5) . . . . ? C12 Ti1 C9 C13 37.5(5) . . . . ? Ti1 Ti1 C9 C13 -154.5(4) 3_766 . . . ? N1 Ti1 C9 C10 43.8(5) 3_766 . . . ? N1 Ti1 C9 C10 131.2(4) . . . . ? Cl1 Ti1 C9 C10 -121.4(4) . . . . ? C11 Ti1 C9 C10 -36.8(4) . . . . ? C12 Ti1 C9 C10 -77.4(5) . . . . ? C13 Ti1 C9 C10 -114.9(7) . . . . ? Ti1 Ti1 C9 C10 90.6(4) 3_766 . . . ? C13 C9 C10 C11 -1.4(8) . . . . ? Ti1 C9 C10 C11 64.9(5) . . . . ? C13 C9 C10 Ti1 -66.2(5) . . . . ? N1 Ti1 C10 C11 102.3(4) 3_766 . . . ? N1 Ti1 C10 C11 -168.7(4) . . . . ? Cl1 Ti1 C10 C11 -14.0(6) . . . . ? C9 Ti1 C10 C11 -116.0(6) . . . . ? C12 Ti1 C10 C11 -37.0(4) . . . . ? C13 Ti1 C10 C11 -78.6(5) . . . . ? Ti1 Ti1 C10 C11 145.2(4) 3_766 . . . ? N1 Ti1 C10 C9 -141.8(4) 3_766 . . . ? N1 Ti1 C10 C9 -52.7(5) . . . . ? Cl1 Ti1 C10 C9 102.0(5) . . . . ? C11 Ti1 C10 C9 116.0(6) . . . . ? C12 Ti1 C10 C9 78.9(5) . . . . ? C13 Ti1 C10 C9 37.4(4) . . . . ? Ti1 Ti1 C10 C9 -98.9(4) 3_766 . . . ? C9 C10 C11 C12 1.2(8) . . . . ? Ti1 C10 C11 C12 65.5(5) . . . . ? C9 C10 C11 Ti1 -64.4(5) . . . . ? N1 Ti1 C11 C12 164.3(5) 3_766 . . . ? N1 Ti1 C11 C12 -98.1(5) . . . . ? Cl1 Ti1 C11 C12 55.4(5) . . . . ? C9 Ti1 C11 C12 -78.3(5) . . . . ? C10 Ti1 C11 C12 -115.8(6) . . . . ? C13 Ti1 C11 C12 -37.4(4) . . . . ? Ti1 Ti1 C11 C12 -162.1(4) 3_766 . . . ? N1 Ti1 C11 C10 -79.8(4) 3_766 . . . ? N1 Ti1 C11 C10 17.7(6) . . . . ? Cl1 Ti1 C11 C10 171.2(4) . . . . ? C9 Ti1 C11 C10 37.5(4) . . . . ? C12 Ti1 C11 C10 115.8(6) . . . . ? C13 Ti1 C11 C10 78.4(5) . . . . ? Ti1 Ti1 C11 C10 -46.3(5) 3_766 . . . ? C10 C11 C12 C13 -0.5(8) . . . . ? Ti1 C11 C12 C13 64.5(5) . . . . ? C10 C11 C12 Ti1 -65.0(5) . . . . ? N1 Ti1 C12 C11 -20.3(6) 3_766 . . . ? N1 Ti1 C12 C11 121.5(5) . . . . ? Cl1 Ti1 C12 C11 -129.3(4) . . . . ? C9 Ti1 C12 C11 79.0(5) . . . . ? C10 Ti1 C12 C11 37.2(4) . . . . ? C13 Ti1 C12 C11 116.0(7) . . . . ? Ti1 Ti1 C12 C11 43.4(9) 3_766 . . . ? N1 Ti1 C12 C13 -136.3(4) 3_766 . . . ? N1 Ti1 C12 C13 5.5(6) . . . . ? Cl1 Ti1 C12 C13 114.7(4) . . . . ? C9 Ti1 C12 C13 -37.0(4) . . . . ? C10 Ti1 C12 C13 -78.8(5) . . . . ? C11 Ti1 C12 C13 -116.0(7) . . . . ? Ti1 Ti1 C12 C13 -72.5(8) 3_766 . . . ? C10 C9 C13 C12 1.1(8) . . . . ? Ti1 C9 C13 C12 -64.5(5) . . . . ? C10 C9 C13 Ti1 65.5(5) . . . . ? C11 C12 C13 C9 -0.4(8) . . . . ? Ti1 C12 C13 C9 64.0(5) . . . . ? C11 C12 C13 Ti1 -64.3(5) . . . . ? N1 Ti1 C13 C9 -36.5(8) 3_766 . . . ? N1 Ti1 C13 C9 68.2(5) . . . . ? Cl1 Ti1 C13 C9 175.4(4) . . . . ? C10 Ti1 C13 C9 -38.1(4) . . . . ? C11 Ti1 C13 C9 -79.0(5) . . . . ? C12 Ti1 C13 C9 -115.8(7) . . . . ? Ti1 Ti1 C13 C9 36.3(6) 3_766 . . . ? N1 Ti1 C13 C12 79.3(7) 3_766 . . . ? N1 Ti1 C13 C12 -176.0(4) . . . . ? Cl1 Ti1 C13 C12 -68.8(4) . . . . ? C9 Ti1 C13 C12 115.8(7) . . . . ? C10 Ti1 C13 C12 77.6(5) . . . . ? C11 Ti1 C13 C12 36.8(4) . . . . ? Ti1 Ti1 C13 C12 152.1(4) 3_766 . . . ? Ti2 N2 C14 C15 -118.7(6) 3_666 . . . ? Ti2 N2 C14 C15 55.7(8) . . . . ? Ti2 N2 C14 C19 61.1(8) 3_666 . . . ? Ti2 N2 C14 C19 -124.6(6) . . . . ? N2 C14 C15 C16 178.6(5) . . . . ? C19 C14 C15 C16 -1.1(9) . . . . ? C14 C15 C16 C17 0.6(9) . . . . ? C14 C15 C16 C20 -179.0(6) . . . . ? C15 C16 C17 C18 0.9(9) . . . . ? C20 C16 C17 C18 -179.5(6) . . . . ? C16 C17 C18 C19 -1.9(10) . . . . ? C16 C17 C18 C21 -179.5(6) . . . . ? C17 C18 C19 C14 1.4(10) . . . . ? C21 C18 C19 C14 179.0(6) . . . . ? N2 C14 C19 C18 -179.7(6) . . . . ? C15 C14 C19 C18 0.1(9) . . . . ? C15 C16 C20 F8 7.6(9) . . . . ? C17 C16 C20 F8 -172.0(6) . . . . ? C15 C16 C20 F9 128.7(6) . . . . ? C17 C16 C20 F9 -50.9(8) . . . . ? C15 C16 C20 F7 -111.7(7) . . . . ? C17 C16 C20 F7 68.6(8) . . . . ? C19 C18 C21 F12 -2.1(11) . . . . ? C17 C18 C21 F12 175.6(7) . . . . ? C19 C18 C21 F10 124.5(8) . . . . ? C17 C18 C21 F10 -57.8(9) . . . . ? C19 C18 C21 F11 -120.3(7) . . . . ? C17 C18 C21 F11 57.4(9) . . . . ? N2 Ti2 C22 C26 -144.9(4) 3_666 . . . ? N2 Ti2 C22 C26 -56.4(5) . . . . ? Cl2 Ti2 C22 C26 97.6(5) . . . . ? C23 Ti2 C22 C26 115.0(6) . . . . ? C24 Ti2 C22 C26 78.2(5) . . . . ? C25 Ti2 C22 C26 36.7(4) . . . . ? Ti2 Ti2 C22 C26 -102.2(4) 3_666 . . . ? N2 Ti2 C22 C23 100.1(4) 3_666 . . . ? N2 Ti2 C22 C23 -171.3(4) . . . . ? Cl2 Ti2 C22 C23 -17.4(6) . . . . ? C26 Ti2 C22 C23 -115.0(6) . . . . ? C24 Ti2 C22 C23 -36.8(4) . . . . ? C25 Ti2 C22 C23 -78.2(5) . . . . ? Ti2 Ti2 C22 C23 142.8(4) 3_666 . . . ? C26 C22 C23 C24 -0.7(8) . . . . ? Ti2 C22 C23 C24 65.2(5) . . . . ? C26 C22 C23 Ti2 -65.9(5) . . . . ? N2 Ti2 C23 C24 163.1(4) 3_666 . . . ? N2 Ti2 C23 C24 -101.7(5) . . . . ? Cl2 Ti2 C23 C24 53.6(4) . . . . ? C22 Ti2 C23 C24 -115.6(6) . . . . ? C26 Ti2 C23 C24 -78.6(5) . . . . ? C25 Ti2 C23 C24 -37.6(4) . . . . ? Ti2 Ti2 C23 C24 -164.8(4) 3_666 . . . ? N2 Ti2 C23 C22 -81.3(4) 3_666 . . . ? N2 Ti2 C23 C22 13.9(6) . . . . ? Cl2 Ti2 C23 C22 169.2(4) . . . . ? C26 Ti2 C23 C22 37.0(4) . . . . ? C24 Ti2 C23 C22 115.6(6) . . . . ? C25 Ti2 C23 C22 78.0(5) . . . . ? Ti2 Ti2 C23 C22 -49.2(5) 3_666 . . . ? C22 C23 C24 C25 0.9(8) . . . . ? Ti2 C23 C24 C25 65.0(5) . . . . ? C22 C23 C24 Ti2 -64.1(5) . . . . ? N2 Ti2 C24 C23 -21.4(5) 3_666 . . . ? N2 Ti2 C24 C23 121.0(5) . . . . ? Cl2 Ti2 C24 C23 -130.7(4) . . . . ? C22 Ti2 C24 C23 38.0(4) . . . . ? C26 Ti2 C24 C23 78.5(5) . . . . ? C25 Ti2 C24 C23 115.6(6) . . . . ? Ti2 Ti2 C24 C23 36.9(8) 3_666 . . . ? N2 Ti2 C24 C25 -137.0(4) 3_666 . . . ? N2 Ti2 C24 C25 5.3(6) . . . . ? Cl2 Ti2 C24 C25 113.7(4) . . . . ? C22 Ti2 C24 C25 -77.6(5) . . . . ? C26 Ti2 C24 C25 -37.1(4) . . . . ? C23 Ti2 C24 C25 -115.6(6) . . . . ? Ti2 Ti2 C24 C25 -78.7(7) 3_666 . . . ? C23 C24 C25 C26 -0.8(8) . . . . ? Ti2 C24 C25 C26 63.9(5) . . . . ? C23 C24 C25 Ti2 -64.7(5) . . . . ? N2 Ti2 C25 C26 -39.3(7) 3_666 . . . ? N2 Ti2 C25 C26 68.2(5) . . . . ? Cl2 Ti2 C25 C26 175.4(4) . . . . ? C22 Ti2 C25 C26 -36.4(4) . . . . ? C23 Ti2 C25 C26 -78.5(5) . . . . ? C24 Ti2 C25 C26 -115.5(6) . . . . ? Ti2 Ti2 C25 C26 34.9(5) 3_666 . . . ? N2 Ti2 C25 C24 76.2(6) 3_666 . . . ? N2 Ti2 C25 C24 -176.3(4) . . . . ? Cl2 Ti2 C25 C24 -69.1(4) . . . . ? C22 Ti2 C25 C24 79.1(5) . . . . ? C26 Ti2 C25 C24 115.5(6) . . . . ? C23 Ti2 C25 C24 37.0(4) . . . . ? Ti2 Ti2 C25 C24 150.4(4) 3_666 . . . ? C23 C22 C26 C25 0.2(8) . . . . ? Ti2 C22 C26 C25 -65.4(5) . . . . ? C23 C22 C26 Ti2 65.6(5) . . . . ? C24 C25 C26 C22 0.3(8) . . . . ? Ti2 C25 C26 C22 64.5(5) . . . . ? C24 C25 C26 Ti2 -64.2(5) . . . . ? N2 Ti2 C26 C22 40.0(5) 3_666 . . . ? N2 Ti2 C26 C22 128.1(4) . . . . ? Cl2 Ti2 C26 C22 -123.4(4) . . . . ? C23 Ti2 C26 C22 -38.4(4) . . . . ? C24 Ti2 C26 C22 -79.2(5) . . . . ? C25 Ti2 C26 C22 -116.8(6) . . . . ? Ti2 Ti2 C26 C22 87.1(4) 3_666 . . . ? N2 Ti2 C26 C25 156.8(4) 3_666 . . . ? N2 Ti2 C26 C25 -115.1(5) . . . . ? Cl2 Ti2 C26 C25 -6.5(6) . . . . ? C22 Ti2 C26 C25 116.8(6) . . . . ? C23 Ti2 C26 C25 78.4(5) . . . . ? C24 Ti2 C26 C25 37.6(4) . . . . ? Ti2 Ti2 C26 C25 -156.1(4) 3_666 . . . ? C28 Co1 C27 C31 118.6(7) . . . . ? C32 Co1 C27 C31 -163.1(5) . . . . ? C29 Co1 C27 C31 80.3(6) . . . . ? C33 Co1 C27 C31 163.1(9) . . . . ? C30 Co1 C27 C31 36.9(5) . . . . ? C36 Co1 C27 C31 -121.3(5) . . . . ? C35 Co1 C27 C31 -79.0(5) . . . . ? C34 Co1 C27 C31 -46.5(9) . . . . ? C32 Co1 C27 C28 78.3(6) . . . . ? C29 Co1 C27 C28 -38.4(5) . . . . ? C31 Co1 C27 C28 -118.6(7) . . . . ? C33 Co1 C27 C28 44.5(12) . . . . ? C30 Co1 C27 C28 -81.7(6) . . . . ? C36 Co1 C27 C28 120.0(5) . . . . ? C35 Co1 C27 C28 162.3(5) . . . . ? C34 Co1 C27 C28 -165.1(7) . . . . ? C31 C27 C28 C29 1.5(8) . . . . ? Co1 C27 C28 C29 60.5(5) . . . . ? C31 C27 C28 Co1 -58.9(5) . . . . ? C32 Co1 C28 C27 -122.3(5) . . . . ? C29 Co1 C28 C27 118.7(7) . . . . ? C31 Co1 C28 C27 37.2(4) . . . . ? C33 Co1 C28 C27 -165.5(4) . . . . ? C30 Co1 C28 C27 80.9(5) . . . . ? C36 Co1 C28 C27 -79.2(5) . . . . ? C35 Co1 C28 C27 -43.3(10) . . . . ? C34 Co1 C28 C27 160.1(8) . . . . ? C32 Co1 C28 C29 118.9(6) . . . . ? C31 Co1 C28 C29 -81.5(6) . . . . ? C33 Co1 C28 C29 75.8(7) . . . . ? C30 Co1 C28 C29 -37.8(5) . . . . ? C36 Co1 C28 C29 162.0(5) . . . . ? C35 Co1 C28 C29 -162.0(8) . . . . ? C34 Co1 C28 C29 41.4(12) . . . . ? C27 Co1 C28 C29 -118.7(7) . . . . ? C27 C28 C29 C30 -1.2(9) . . . . ? Co1 C28 C29 C30 60.0(5) . . . . ? C27 C28 C29 Co1 -61.1(5) . . . . ? C28 Co1 C29 C30 -118.1(7) . . . . ? C32 Co1 C29 C30 160.5(5) . . . . ? C31 Co1 C29 C30 -37.4(5) . . . . ? C33 Co1 C29 C30 117.5(6) . . . . ? C36 Co1 C29 C30 -165.5(8) . . . . ? C35 Co1 C29 C30 42.8(11) . . . . ? C34 Co1 C29 C30 76.3(6) . . . . ? C27 Co1 C29 C30 -80.1(5) . . . . ? C32 Co1 C29 C28 -81.3(6) . . . . ? C31 Co1 C29 C28 80.7(5) . . . . ? C33 Co1 C29 C28 -124.3(6) . . . . ? C30 Co1 C29 C28 118.1(7) . . . . ? C36 Co1 C29 C28 -47.3(11) . . . . ? C35 Co1 C29 C28 161.0(8) . . . . ? C34 Co1 C29 C28 -165.6(5) . . . . ? C27 Co1 C29 C28 38.0(5) . . . . ? C28 C29 C30 C31 0.3(9) . . . . ? Co1 C29 C30 C31 59.2(5) . . . . ? C28 C29 C30 Co1 -58.9(5) . . . . ? C28 Co1 C30 C29 38.9(5) . . . . ? C32 Co1 C30 C29 -48.3(11) . . . . ? C31 Co1 C30 C29 119.6(7) . . . . ? C33 Co1 C30 C29 -80.8(6) . . . . ? C36 Co1 C30 C29 165.6(8) . . . . ? C35 Co1 C30 C29 -163.1(5) . . . . ? C34 Co1 C30 C29 -122.3(6) . . . . ? C27 Co1 C30 C29 83.3(6) . . . . ? C28 Co1 C30 C31 -80.7(5) . . . . ? C32 Co1 C30 C31 -167.9(8) . . . . ? C29 Co1 C30 C31 -119.6(7) . . . . ? C33 Co1 C30 C31 159.6(5) . . . . ? C36 Co1 C30 C31 46.0(11) . . . . ? C35 Co1 C30 C31 77.4(6) . . . . ? C34 Co1 C30 C31 118.1(5) . . . . ? C27 Co1 C30 C31 -36.3(5) . . . . ? C28 C27 C31 C30 -1.3(8) . . . . ? Co1 C27 C31 C30 -59.3(5) . . . . ? C28 C27 C31 Co1 57.9(5) . . . . ? C29 C30 C31 C27 0.6(9) . . . . ? Co1 C30 C31 C27 59.9(5) . . . . ? C29 C30 C31 Co1 -59.2(5) . . . . ? C28 Co1 C31 C27 -38.5(5) . . . . ? C32 Co1 C31 C27 45.7(11) . . . . ? C29 Co1 C31 C27 -83.4(6) . . . . ? C33 Co1 C31 C27 -168.0(7) . . . . ? C30 Co1 C31 C27 -120.7(7) . . . . ? C36 Co1 C31 C27 77.2(6) . . . . ? C35 Co1 C31 C27 118.4(5) . . . . ? C34 Co1 C31 C27 159.4(5) . . . . ? C28 Co1 C31 C30 82.1(6) . . . . ? C32 Co1 C31 C30 166.3(9) . . . . ? C29 Co1 C31 C30 37.3(6) . . . . ? C33 Co1 C31 C30 -47.3(10) . . . . ? C36 Co1 C31 C30 -162.1(5) . . . . ? C35 Co1 C31 C30 -120.9(5) . . . . ? C34 Co1 C31 C30 -79.9(6) . . . . ? C27 Co1 C31 C30 120.7(7) . . . . ? C28 Co1 C32 C36 118.7(5) . . . . ? C29 Co1 C32 C36 162.5(5) . . . . ? C31 Co1 C32 C36 41.8(11) . . . . ? C33 Co1 C32 C36 -118.3(7) . . . . ? C30 Co1 C32 C36 -162.3(8) . . . . ? C35 Co1 C32 C36 -37.6(4) . . . . ? C34 Co1 C32 C36 -80.6(5) . . . . ? C27 Co1 C32 C36 75.9(6) . . . . ? C28 Co1 C32 C33 -123.0(6) . . . . ? C29 Co1 C32 C33 -79.2(6) . . . . ? C31 Co1 C32 C33 160.1(9) . . . . ? C30 Co1 C32 C33 -44.0(11) . . . . ? C36 Co1 C32 C33 118.3(7) . . . . ? C35 Co1 C32 C33 80.7(5) . . . . ? C34 Co1 C32 C33 37.8(5) . . . . ? C27 Co1 C32 C33 -165.8(5) . . . . ? C36 C32 C33 C34 -0.2(8) . . . . ? Co1 C32 C33 C34 -60.6(5) . . . . ? C36 C32 C33 Co1 60.4(5) . . . . ? C28 Co1 C33 C34 -164.0(5) . . . . ? C32 Co1 C33 C34 118.1(7) . . . . ? C29 Co1 C33 C34 -121.6(6) . . . . ? C31 Co1 C33 C34 -45.8(10) . . . . ? C30 Co1 C33 C34 -79.6(6) . . . . ? C36 Co1 C33 C34 79.9(5) . . . . ? C35 Co1 C33 C34 36.3(4) . . . . ? C27 Co1 C33 C34 161.5(9) . . . . ? C28 Co1 C33 C32 77.9(6) . . . . ? C29 Co1 C33 C32 120.3(6) . . . . ? C31 Co1 C33 C32 -163.9(7) . . . . ? C30 Co1 C33 C32 162.3(5) . . . . ? C36 Co1 C33 C32 -38.1(5) . . . . ? C35 Co1 C33 C32 -81.8(5) . . . . ? C34 Co1 C33 C32 -118.1(7) . . . . ? C27 Co1 C33 C32 43.4(12) . . . . ? C32 C33 C34 C35 0.8(8) . . . . ? Co1 C33 C34 C35 -58.8(5) . . . . ? C32 C33 C34 Co1 59.6(5) . . . . ? C28 Co1 C34 C35 166.4(9) . . . . ? C32 Co1 C34 C35 82.0(5) . . . . ? C29 Co1 C34 C35 -161.9(5) . . . . ? C31 Co1 C34 C35 -78.9(5) . . . . ? C33 Co1 C34 C35 120.9(7) . . . . ? C30 Co1 C34 C35 -120.8(5) . . . . ? C36 Co1 C34 C35 37.7(4) . . . . ? C27 Co1 C34 C35 -46.2(9) . . . . ? C28 Co1 C34 C33 45.5(11) . . . . ? C32 Co1 C34 C33 -38.9(5) . . . . ? C29 Co1 C34 C33 77.2(6) . . . . ? C31 Co1 C34 C33 160.2(5) . . . . ? C30 Co1 C34 C33 118.3(5) . . . . ? C36 Co1 C34 C33 -83.2(5) . . . . ? C35 Co1 C34 C33 -120.9(7) . . . . ? C27 Co1 C34 C33 -167.1(6) . . . . ? C33 C34 C35 C36 -1.2(8) . . . . ? Co1 C34 C35 C36 -59.6(5) . . . . ? C33 C34 C35 Co1 58.4(5) . . . . ? C28 Co1 C35 C34 -168.8(7) . . . . ? C32 Co1 C35 C34 -81.3(5) . . . . ? C29 Co1 C35 C34 45.8(11) . . . . ? C31 Co1 C35 C34 118.6(5) . . . . ? C33 Co1 C35 C34 -36.6(5) . . . . ? C30 Co1 C35 C34 77.3(6) . . . . ? C36 Co1 C35 C34 -119.3(7) . . . . ? C27 Co1 C35 C34 159.5(4) . . . . ? C28 Co1 C35 C36 -49.5(10) . . . . ? C32 Co1 C35 C36 38.0(5) . . . . ? C29 Co1 C35 C36 165.1(8) . . . . ? C31 Co1 C35 C36 -122.1(5) . . . . ? C33 Co1 C35 C36 82.7(5) . . . . ? C30 Co1 C35 C36 -163.5(5) . . . . ? C34 Co1 C35 C36 119.3(7) . . . . ? C27 Co1 C35 C36 -81.2(5) . . . . ? C34 C35 C36 C32 1.0(8) . . . . ? Co1 C35 C36 C32 -58.8(5) . . . . ? C34 C35 C36 Co1 59.8(5) . . . . ? C33 C32 C36 C35 -0.5(8) . . . . ? Co1 C32 C36 C35 59.4(5) . . . . ? C33 C32 C36 Co1 -60.0(5) . . . . ? C28 Co1 C36 C35 159.9(5) . . . . ? C32 Co1 C36 C35 -119.0(7) . . . . ? C29 Co1 C36 C35 -164.7(8) . . . . ? C31 Co1 C36 C35 76.4(5) . . . . ? C33 Co1 C36 C35 -80.4(5) . . . . ? C30 Co1 C36 C35 42.4(11) . . . . ? C34 Co1 C36 C35 -37.1(5) . . . . ? C27 Co1 C36 C35 117.2(5) . . . . ? C28 Co1 C36 C32 -81.2(6) . . . . ? C29 Co1 C36 C32 -45.7(11) . . . . ? C31 Co1 C36 C32 -164.6(5) . . . . ? C33 Co1 C36 C32 38.6(5) . . . . ? C30 Co1 C36 C32 161.4(8) . . . . ? C35 Co1 C36 C32 119.0(7) . . . . ? C34 Co1 C36 C32 81.9(5) . . . . ? C27 Co1 C36 C32 -123.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.593 _refine_diff_density_min -0.785 _refine_diff_density_rms 0.151