# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Kotohiro Nomura' _publ_contact_author_email NOMURAK@MS.NAIST.JP _publ_section_title ; Effect of Aryloxo Substituents in Ethylene Polymerisation by Tris(pyrazolyl)borate Titanium(IV) Complexes Containing Aryloxo Ligands of Type, TpTiCl2(OAr) ; loop_ _publ_author_name 'Kotohiro Nomura' 'Michiya Fujiki' 'Shinya Hasumi' 'Koji Itagaki' # Attachment 'CIF_for_revision.txt' data_TpTiCl2(OC6F5) _database_code_depnum_ccdc_archive 'CCDC 731624' _audit_creation_date 2009-08-21 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C16 H10 B Cl4 F5 N6 O Ti ' _chemical_formula_moiety 'C15 H10 B Cl2 F5 N6 O Ti, C Cl2 ' _chemical_formula_weight 597.81 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _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_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 11.5340(4) _cell_length_b 12.9265(4) _cell_length_c 15.6367(7) _cell_angle_alpha 90.0000 _cell_angle_beta 98.7577(12) _cell_angle_gamma 90.0000 _cell_volume 2304.15(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used 15787 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.3 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184.00 _exptl_absorpt_coefficient_mu 0.898 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.718 _exptl_absorpt_correction_T_max 0.898 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 18147 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_theta_max 25.30 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.30 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_ambient_temperature 193.1 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4185 _reflns_number_gt 3847 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.1842 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 4185 _refine_ls_number_parameters 326 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1048P)^2^+6.5259P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.04 _refine_diff_density_min -1.70 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; B B 0.001 0.001 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ti Ti 0.278 0.446 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ti(1) Ti 0.26783(6) 0.20009(5) 0.68940(4) 0.0246(2) Uani 1.00 1 d . . . Cl(1) Cl 0.22698(9) 0.04087(8) 0.73886(7) 0.0349(2) Uani 1.00 1 d . . . Cl(2) Cl 0.18584(9) 0.18311(9) 0.54876(7) 0.0385(2) Uani 1.00 1 d . . . Cl(3) Cl -0.0333(4) 0.4724(3) 0.6099(2) 0.0911(11) Uani 0.50 1 d P . . Cl(4) Cl -0.2024(5) 0.3265(3) 0.5849(2) 0.208(2) Uani 1.00 1 d . . . Cl(5) Cl -0.0308(8) 0.4466(6) 0.5000(5) 0.173(2) Uani 0.50 1 d P . . F(1) F 0.1764(2) 0.4513(2) 0.81124(19) 0.0444(6) Uani 1.00 1 d . . . F(2) F 0.0224(2) 0.5160(2) 0.91350(19) 0.0510(7) Uani 1.00 1 d . . . F(3) F -0.1641(2) 0.3921(2) 0.93774(18) 0.0528(7) Uani 1.00 1 d . . . F(4) F -0.1931(2) 0.2073(2) 0.85613(19) 0.0474(6) Uani 1.00 1 d . . . F(5) F -0.0419(2) 0.1439(2) 0.7512(2) 0.0480(6) Uani 1.00 1 d . . . O(1) O 0.1478(2) 0.2650(2) 0.7282(2) 0.0352(6) Uani 1.00 1 d . . . N(1) N 0.5386(2) 0.1811(2) 0.6850(2) 0.0248(6) Uani 1.00 1 d . . . N(2) N 0.4310(2) 0.1361(2) 0.6601(2) 0.0248(6) Uani 1.00 1 d . . . N(3) N 0.4917(2) 0.2640(2) 0.8186(2) 0.0262(6) Uani 1.00 1 d . . . N(4) N 0.3790(2) 0.2294(2) 0.8118(2) 0.0285(7) Uani 1.00 1 d . . . N(5) N 0.4655(2) 0.3627(2) 0.6805(2) 0.0263(6) Uani 1.00 1 d . . . N(6) N 0.3486(2) 0.3409(2) 0.6577(2) 0.0286(7) Uani 1.00 1 d . . . C(1) C 0.6219(3) 0.1205(3) 0.6606(2) 0.0324(8) Uani 1.00 1 d . . . C(2) C 0.5692(3) 0.0349(3) 0.6182(2) 0.0361(9) Uani 1.00 1 d . . . C(3) C 0.4509(3) 0.0482(3) 0.6193(2) 0.0316(8) Uani 1.00 1 d . . . C(4) C 0.5364(3) 0.2737(3) 0.9029(2) 0.0305(8) Uani 1.00 1 d . . . C(5) C 0.4529(4) 0.2450(3) 0.9522(2) 0.0364(9) Uani 1.00 1 d . . . C(6) C 0.3557(4) 0.2181(3) 0.8930(2) 0.0347(9) Uani 1.00 1 d . . . C(7) C 0.4886(4) 0.4564(3) 0.6503(2) 0.0360(9) Uani 1.00 1 d . . . C(8) C 0.3847(4) 0.4969(3) 0.6058(3) 0.0467(11) Uani 1.00 1 d . . . C(9) C 0.3011(4) 0.4230(3) 0.6122(3) 0.0405(10) Uani 1.00 1 d . . . C(10) C 0.0728(3) 0.2957(3) 0.7802(2) 0.0296(8) Uani 1.00 1 d . . . C(11) C 0.0855(3) 0.3904(3) 0.8225(2) 0.0315(8) Uani 1.00 1 d . . . C(12) C 0.0071(3) 0.4235(3) 0.8756(2) 0.0349(9) Uani 1.00 1 d . . . C(13) C -0.0855(3) 0.3617(3) 0.8872(2) 0.0365(9) Uani 1.00 1 d . . . C(14) C -0.1010(3) 0.2673(3) 0.8457(2) 0.0348(9) Uani 1.00 1 d . . . C(15) C -0.0234(3) 0.2344(3) 0.7928(2) 0.0318(8) Uani 1.00 1 d . . . C(16) C -0.0723(16) 0.3573(14) 0.5548(10) 0.116(7) Uani 0.50 1 d P . . C(17) C -0.1002(8) 0.4339(8) 0.5818(6) 0.047(2) Uani 0.50 1 d P . . B(1) B 0.5453(3) 0.2841(3) 0.7355(2) 0.0252(8) Uani 1.00 1 d . . . H(1) H 0.7038 0.1341 0.6707 0.039 Uiso 1.00 1 c R . . H(2) H 0.6064 -0.0209 0.5936 0.043 Uiso 1.00 1 c R . . H(3) H 0.3916 0.0015 0.5946 0.038 Uiso 1.00 1 c R . . H(4) H 0.6134 0.2968 0.9248 0.037 Uiso 1.00 1 c R . . H(5) H 0.4602 0.2439 1.0135 0.044 Uiso 1.00 1 c R . . H(6) H 0.2830 0.1950 0.9076 0.042 Uiso 1.00 1 c R . . H(7) H 0.5631 0.4895 0.6580 0.043 Uiso 1.00 1 c R . . H(8) H 0.3740 0.5617 0.5771 0.056 Uiso 1.00 1 c R . . H(9) H 0.2207 0.4290 0.5879 0.049 Uiso 1.00 1 c R . . H(10) H 0.6278 0.3098 0.7491 0.030 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti(1) 0.0207(3) 0.0239(3) 0.0295(4) -0.0011(2) 0.0049(2) 0.0008(2) Cl(1) 0.0317(5) 0.0300(5) 0.0427(5) -0.0066(3) 0.0052(4) 0.0059(3) Cl(2) 0.0340(5) 0.0464(6) 0.0329(5) -0.0100(4) -0.0020(4) 0.0029(4) Cl(3) 0.111(3) 0.092(2) 0.077(2) -0.006(2) 0.038(2) -0.004(2) Cl(4) 0.337(7) 0.153(3) 0.135(2) -0.005(4) 0.042(3) 0.010(2) Cl(5) 0.203(8) 0.152(6) 0.168(6) -0.022(5) 0.039(5) -0.006(5) F(1) 0.0341(13) 0.0347(13) 0.0643(17) -0.0077(10) 0.0074(12) -0.0023(11) F(2) 0.0613(17) 0.0409(14) 0.0507(16) 0.0033(13) 0.0086(13) -0.0139(12) F(3) 0.0488(15) 0.0674(19) 0.0467(15) 0.0105(14) 0.0217(12) -0.0022(13) F(4) 0.0301(12) 0.0545(16) 0.0594(17) -0.0043(11) 0.0125(11) 0.0125(13) F(5) 0.0395(14) 0.0350(13) 0.0706(18) -0.0065(11) 0.0122(12) -0.0107(12) O(1) 0.0267(13) 0.0342(15) 0.0465(16) 0.0019(11) 0.0115(12) -0.0016(12) N(1) 0.0220(15) 0.0257(15) 0.0266(15) -0.0001(12) 0.0035(12) -0.0005(12) N(2) 0.0256(15) 0.0223(15) 0.0266(15) -0.0019(12) 0.0041(12) -0.0011(12) N(3) 0.0268(15) 0.0229(15) 0.0285(16) 0.0002(12) 0.0030(12) -0.0027(12) N(4) 0.0287(16) 0.0293(17) 0.0288(16) -0.0016(13) 0.0086(13) -0.0027(13) N(5) 0.0254(15) 0.0228(15) 0.0303(16) -0.0027(12) 0.0029(12) -0.0001(12) N(6) 0.0235(15) 0.0240(16) 0.0376(17) 0.0012(12) 0.0022(13) 0.0014(13) C(1) 0.0254(19) 0.035(2) 0.037(2) 0.0066(16) 0.0065(15) -0.0006(16) C(2) 0.038(2) 0.030(2) 0.042(2) 0.0075(17) 0.0109(18) -0.0066(17) C(3) 0.036(2) 0.0251(19) 0.033(2) -0.0017(16) 0.0032(16) -0.0043(15) C(4) 0.037(2) 0.0237(18) 0.0289(19) 0.0028(16) -0.0012(16) -0.0050(15) C(5) 0.050(2) 0.036(2) 0.0248(19) 0.0040(19) 0.0081(17) -0.0029(16) C(6) 0.041(2) 0.035(2) 0.031(2) -0.0003(18) 0.0138(17) -0.0006(16) C(7) 0.040(2) 0.026(2) 0.041(2) -0.0075(17) 0.0033(18) 0.0045(16) C(8) 0.049(2) 0.026(2) 0.061(3) -0.0045(19) -0.005(2) 0.013(2) C(9) 0.034(2) 0.029(2) 0.055(2) 0.0051(17) -0.0038(19) 0.0097(19) C(10) 0.0216(18) 0.032(2) 0.035(2) 0.0056(15) 0.0034(15) 0.0045(15) C(11) 0.0242(18) 0.030(2) 0.039(2) 0.0009(15) 0.0010(16) 0.0037(16) C(12) 0.037(2) 0.033(2) 0.033(2) 0.0063(17) -0.0009(17) -0.0009(16) C(13) 0.032(2) 0.047(2) 0.031(2) 0.0114(18) 0.0074(16) 0.0036(18) C(14) 0.0245(19) 0.040(2) 0.039(2) 0.0025(17) 0.0044(16) 0.0118(18) C(15) 0.0237(18) 0.029(2) 0.041(2) 0.0008(15) 0.0012(16) 0.0007(16) C(16) 0.149(17) 0.133(16) 0.074(9) -0.090(14) 0.046(10) -0.034(10) C(17) 0.045(5) 0.052(5) 0.041(5) -0.040(5) -0.006(4) -0.020(4) B(1) 0.0228(19) 0.0228(19) 0.030(2) -0.0018(16) 0.0038(16) -0.0008(16) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ti(1) Cl(1) 2.2731(12) yes . . Ti(1) Cl(2) 2.2683(11) yes . . Ti(1) O(1) 1.801(3) yes . . Ti(1) N(2) 2.168(3) yes . . Ti(1) N(4) 2.168(3) yes . . Ti(1) N(6) 2.138(3) yes . . Cl(3) Cl(5) 1.755(10) yes . . Cl(3) Cl(5) 2.231(10) yes . 3_566 Cl(3) C(16) 1.743(18) yes . . Cl(3) C(17) 0.966(10) yes . . Cl(4) C(16) 1.69(2) yes . . Cl(4) C(17) 1.826(12) yes . . Cl(5) Cl(5) 1.554(12) yes . 3_566 Cl(5) C(16) 1.56(2) yes . . Cl(5) C(17) 1.618(14) yes . . F(1) C(11) 1.343(4) yes . . F(2) C(12) 1.333(5) yes . . F(3) C(13) 1.348(5) yes . . F(4) C(14) 1.345(5) yes . . F(5) C(15) 1.338(5) yes . . O(1) C(10) 1.335(5) yes . . N(1) N(2) 1.373(4) yes . . N(1) C(1) 1.340(5) yes . . N(1) B(1) 1.544(5) yes . . N(2) C(3) 1.339(5) yes . . N(3) N(4) 1.364(4) yes . . N(3) C(4) 1.345(4) yes . . N(3) B(1) 1.544(5) yes . . N(4) C(6) 1.345(5) yes . . N(5) N(6) 1.370(4) yes . . N(5) C(7) 1.341(5) yes . . N(5) B(1) 1.542(5) yes . . N(6) C(9) 1.347(5) yes . . C(1) C(2) 1.382(5) yes . . C(2) C(3) 1.378(6) yes . . C(4) C(5) 1.374(6) yes . . C(5) C(6) 1.385(5) yes . . C(7) C(8) 1.394(6) yes . . C(8) C(9) 1.371(6) yes . . C(10) C(11) 1.389(5) yes . . C(10) C(15) 1.402(5) yes . . C(11) C(12) 1.385(6) yes . . C(12) C(13) 1.369(6) yes . . C(13) C(14) 1.381(6) yes . . C(14) C(15) 1.376(6) yes . . C(16) C(17) 1.14(2) yes . . C(1) H(1) 0.950 no . . C(2) H(2) 0.950 no . . C(3) H(3) 0.950 no . . C(4) H(4) 0.950 no . . C(5) H(5) 0.950 no . . C(6) H(6) 0.950 no . . C(7) H(7) 0.950 no . . C(8) H(8) 0.950 no . . C(9) H(9) 0.950 no . . B(1) H(10) 1.000 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Ti(1) Cl(2) 99.49(4) yes . . . Cl(1) Ti(1) O(1) 95.59(10) yes . . . Cl(1) Ti(1) N(2) 87.61(9) yes . . . Cl(1) Ti(1) N(4) 89.03(9) yes . . . Cl(1) Ti(1) N(6) 166.00(9) yes . . . Cl(2) Ti(1) O(1) 98.24(9) yes . . . Cl(2) Ti(1) N(2) 90.29(8) yes . . . Cl(2) Ti(1) N(4) 167.35(10) yes . . . Cl(2) Ti(1) N(6) 89.41(9) yes . . . O(1) Ti(1) N(2) 170.25(12) yes . . . O(1) Ti(1) N(4) 90.16(13) yes . . . O(1) Ti(1) N(6) 93.78(13) yes . . . N(2) Ti(1) N(4) 80.67(12) yes . . . N(2) Ti(1) N(6) 81.52(12) yes . . . N(4) Ti(1) N(6) 80.56(12) yes . . . Cl(5) Cl(3) Cl(5) 43.9(3) yes . . 3_566 Cl(5) Cl(3) C(16) 52.8(6) yes . . . Cl(5) Cl(3) C(17) 65.7(7) yes . . . Cl(5) Cl(3) C(16) 96.4(6) yes 3_566 . . Cl(5) Cl(3) C(17) 103.2(7) yes 3_566 . . C(16) Cl(3) C(17) 37.6(8) yes . . . C(16) Cl(4) C(17) 37.7(7) yes . . . Cl(3) Cl(5) Cl(3) 136.1(4) yes . . 3_566 Cl(3) Cl(5) Cl(5) 84.6(5) yes . . 3_566 Cl(3) Cl(5) C(16) 63.2(7) yes . . . Cl(3) Cl(5) C(17) 33.0(4) yes . . . Cl(3) Cl(5) Cl(5) 51.5(4) yes 3_566 . 3_566 Cl(3) Cl(5) C(16) 159.7(8) yes 3_566 . . Cl(3) Cl(5) C(17) 156.7(6) yes 3_566 . . Cl(5) Cl(5) C(16) 146.9(9) yes 3_566 . . Cl(5) Cl(5) C(17) 111.8(7) yes 3_566 . . C(16) Cl(5) C(17) 42.1(8) yes . . . Ti(1) O(1) C(10) 161.2(2) yes . . . N(2) N(1) C(1) 109.1(3) yes . . . N(2) N(1) B(1) 118.9(3) yes . . . C(1) N(1) B(1) 131.9(3) yes . . . Ti(1) N(2) N(1) 123.7(2) yes . . . Ti(1) N(2) C(3) 129.9(2) yes . . . N(1) N(2) C(3) 106.4(3) yes . . . N(4) N(3) C(4) 109.0(3) yes . . . N(4) N(3) B(1) 119.2(2) yes . . . C(4) N(3) B(1) 131.7(3) yes . . . Ti(1) N(4) N(3) 123.7(2) yes . . . Ti(1) N(4) C(6) 129.7(2) yes . . . N(3) N(4) C(6) 106.6(3) yes . . . N(6) N(5) C(7) 109.5(3) yes . . . N(6) N(5) B(1) 119.3(3) yes . . . C(7) N(5) B(1) 131.1(3) yes . . . Ti(1) N(6) N(5) 124.1(2) yes . . . Ti(1) N(6) C(9) 129.5(2) yes . . . N(5) N(6) C(9) 106.3(3) yes . . . N(1) C(1) C(2) 108.8(3) yes . . . C(1) C(2) C(3) 104.9(3) yes . . . N(2) C(3) C(2) 110.7(3) yes . . . N(3) C(4) C(5) 109.1(3) yes . . . C(4) C(5) C(6) 105.0(3) yes . . . N(4) C(6) C(5) 110.3(3) yes . . . N(5) C(7) C(8) 108.2(3) yes . . . C(7) C(8) C(9) 105.3(4) yes . . . N(6) C(9) C(8) 110.7(3) yes . . . O(1) C(10) C(11) 121.4(3) yes . . . O(1) C(10) C(15) 121.2(3) yes . . . C(11) C(10) C(15) 117.4(3) yes . . . F(1) C(11) C(10) 118.8(3) yes . . . F(1) C(11) C(12) 119.4(3) yes . . . C(10) C(11) C(12) 121.8(3) yes . . . F(2) C(12) C(11) 119.3(3) yes . . . F(2) C(12) C(13) 121.2(4) yes . . . C(11) C(12) C(13) 119.5(3) yes . . . F(3) C(13) C(12) 121.0(4) yes . . . F(3) C(13) C(14) 118.9(3) yes . . . C(12) C(13) C(14) 120.1(4) yes . . . F(4) C(14) C(13) 120.1(3) yes . . . F(4) C(14) C(15) 119.5(3) yes . . . C(13) C(14) C(15) 120.4(3) yes . . . F(5) C(15) C(10) 119.8(3) yes . . . F(5) C(15) C(14) 119.5(3) yes . . . C(10) C(15) C(14) 120.7(3) yes . . . Cl(3) C(16) Cl(4) 103.7(10) yes . . . Cl(3) C(16) Cl(5) 64.0(7) yes . . . Cl(3) C(16) C(17) 31.1(7) yes . . . Cl(4) C(16) Cl(5) 133.6(12) yes . . . Cl(4) C(16) C(17) 77.8(11) yes . . . Cl(5) C(16) C(17) 71.8(11) yes . . . Cl(3) C(17) Cl(4) 148.6(9) yes . . . Cl(3) C(17) Cl(5) 81.3(7) yes . . . Cl(3) C(17) C(16) 111.3(13) yes . . . Cl(4) C(17) Cl(5) 119.8(6) yes . . . Cl(4) C(17) C(16) 64.6(10) yes . . . Cl(5) C(17) C(16) 66.1(11) yes . . . N(1) B(1) N(3) 106.9(3) yes . . . N(1) B(1) N(5) 107.7(2) yes . . . N(3) B(1) N(5) 107.4(3) yes . . . N(1) C(1) H(1) 125.6 no . . . C(2) C(1) H(1) 125.6 no . . . C(1) C(2) H(2) 127.5 no . . . C(3) C(2) H(2) 127.5 no . . . N(2) C(3) H(3) 124.6 no . . . C(2) C(3) H(3) 124.6 no . . . N(3) C(4) H(4) 125.5 no . . . C(5) C(4) H(4) 125.4 no . . . C(4) C(5) H(5) 127.5 no . . . C(6) C(5) H(5) 127.5 no . . . N(4) C(6) H(6) 124.9 no . . . C(5) C(6) H(6) 124.9 no . . . N(5) C(7) H(7) 125.9 no . . . C(8) C(7) H(7) 125.9 no . . . C(7) C(8) H(8) 127.4 no . . . C(9) C(8) H(8) 127.4 no . . . N(6) C(9) H(9) 124.7 no . . . C(8) C(9) H(9) 124.7 no . . . N(1) B(1) H(10) 111.5 no . . . N(3) B(1) H(10) 111.5 no . . . N(5) B(1) H(10) 111.5 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cl(1) Ti(1) O(1) C(10) 47.4(8) ? . . . . Cl(1) Ti(1) N(2) N(1) -130.1(2) ? . . . . Cl(1) Ti(1) N(2) C(3) 47.3(3) ? . . . . Cl(1) Ti(1) N(4) N(3) 129.1(2) ? . . . . Cl(1) Ti(1) N(4) C(6) -50.5(3) ? . . . . Cl(1) Ti(1) N(6) N(5) 0.3(6) ? . . . . Cl(1) Ti(1) N(6) C(9) 178.9(3) ? . . . . Cl(2) Ti(1) O(1) C(10) 147.8(8) ? . . . . Cl(2) Ti(1) N(2) N(1) 130.4(2) ? . . . . Cl(2) Ti(1) N(2) C(3) -52.2(3) ? . . . . Cl(2) Ti(1) N(4) N(3) -3.5(6) ? . . . . Cl(2) Ti(1) N(4) C(6) 176.9(3) ? . . . . Cl(2) Ti(1) N(6) N(5) -129.5(2) ? . . . . Cl(2) Ti(1) N(6) C(9) 49.1(3) ? . . . . O(1) Ti(1) N(2) N(1) -20.7(9) ? . . . . O(1) Ti(1) N(2) C(3) 156.7(7) ? . . . . N(2) Ti(1) O(1) C(10) -61.4(12) ? . . . . O(1) Ti(1) N(4) N(3) -135.3(2) ? . . . . O(1) Ti(1) N(4) C(6) 45.1(3) ? . . . . N(4) Ti(1) O(1) C(10) -41.7(8) ? . . . . O(1) Ti(1) N(6) N(5) 132.3(3) ? . . . . O(1) Ti(1) N(6) C(9) -49.2(4) ? . . . . N(6) Ti(1) O(1) C(10) -122.2(8) ? . . . . N(2) Ti(1) N(4) N(3) 41.4(2) ? . . . . N(2) Ti(1) N(4) C(6) -138.2(3) ? . . . . N(4) Ti(1) N(2) N(1) -40.7(2) ? . . . . N(4) Ti(1) N(2) C(3) 136.7(3) ? . . . . N(2) Ti(1) N(6) N(5) -39.1(2) ? . . . . N(2) Ti(1) N(6) C(9) 139.4(4) ? . . . . N(6) Ti(1) N(2) N(1) 41.1(2) ? . . . . N(6) Ti(1) N(2) C(3) -141.6(3) ? . . . . N(4) Ti(1) N(6) N(5) 42.7(2) ? . . . . N(4) Ti(1) N(6) C(9) -138.7(4) ? . . . . N(6) Ti(1) N(4) N(3) -41.5(2) ? . . . . N(6) Ti(1) N(4) C(6) 138.9(3) ? . . . . Cl(5) Cl(3) Cl(5) C(16) 160(2) ? . . 3_566 3_566 Cl(5) Cl(3) Cl(5) C(17) -49.8(15) ? . . 3_566 3_566 Cl(5) Cl(3) Cl(5) C(16) 172.3(9) ? 3_566 . . . Cl(5) Cl(3) Cl(5) C(17) -146.2(9) ? 3_566 . . . Cl(5) Cl(3) C(16) Cl(4) -132.1(11) ? . . . . Cl(5) Cl(3) C(16) C(17) -97.9(13) ? . . . . C(16) Cl(3) Cl(5) Cl(3) -172.3(11) ? . . . 3_566 C(16) Cl(3) Cl(5) C(17) 41.5(10) ? . . . . C(16) Cl(3) Cl(5) Cl(5) -172.3(9) ? . . . 3_566 Cl(5) Cl(3) C(17) Cl(4) 136(2) ? . . . . Cl(5) Cl(3) C(17) C(16) 60.0(12) ? . . . . C(17) Cl(3) Cl(5) Cl(3) 146.2(10) ? . . . 3_566 C(17) Cl(3) Cl(5) C(16) -41.5(10) ? . . . . C(17) Cl(3) Cl(5) Cl(5) 146.2(9) ? . . . 3_566 Cl(5) Cl(3) C(16) Cl(4) -137.5(7) ? 3_566 . . . Cl(5) Cl(3) C(16) Cl(5) -5.4(6) ? 3_566 . . . Cl(5) Cl(3) C(16) C(17) -103.3(12) ? 3_566 . . . C(16) Cl(3) Cl(5) Cl(3) 6.2(9) ? . . 3_566 3_566 C(16) Cl(3) Cl(5) C(16) 166(2) ? . . 3_566 3_566 C(16) Cl(3) Cl(5) C(17) -43.7(17) ? . . 3_566 3_566 C(16) Cl(3) Cl(5) Cl(5) 6.2(7) ? . . 3_566 . Cl(5) Cl(3) C(17) Cl(4) 159.1(16) ? 3_566 . . . Cl(5) Cl(3) C(17) Cl(5) 23.3(5) ? 3_566 . . . Cl(5) Cl(3) C(17) C(16) 83.3(12) ? 3_566 . . . C(17) Cl(3) Cl(5) Cl(3) -31.4(10) ? . . 3_566 3_566 C(17) Cl(3) Cl(5) C(16) 128(2) ? . . 3_566 3_566 C(17) Cl(3) Cl(5) C(17) -81.2(17) ? . . 3_566 3_566 C(17) Cl(3) Cl(5) Cl(5) -31.4(8) ? . . 3_566 . C(16) Cl(3) C(17) Cl(4) 76(2) ? . . . . C(16) Cl(3) C(17) Cl(5) -60.0(12) ? . . . . C(17) Cl(3) C(16) Cl(4) -34.2(11) ? . . . . C(17) Cl(3) C(16) Cl(5) 97.9(13) ? . . . . C(16) Cl(4) C(17) Cl(3) -90(2) ? . . . . C(16) Cl(4) C(17) Cl(5) 37.8(10) ? . . . . C(17) Cl(4) C(16) Cl(3) 17.3(5) ? . . . . C(17) Cl(4) C(16) Cl(5) -49.7(13) ? . . . . Cl(3) Cl(5) Cl(5) C(16) -167.3(17) ? . . 3_566 3_566 Cl(3) Cl(5) Cl(5) C(17) 161.0(6) ? . . 3_566 3_566 Cl(3) Cl(5) C(16) Cl(4) 84.2(15) ? . . . . Cl(3) Cl(5) C(16) C(17) 32.6(6) ? . . . . Cl(3) Cl(5) C(17) Cl(4) -155.3(11) ? . . . . Cl(3) Cl(5) C(17) C(16) -118.0(12) ? . . . . Cl(3) Cl(5) Cl(5) C(16) 12.7(16) ? 3_566 . 3_566 3_566 Cl(3) Cl(5) Cl(5) C(17) -19.0(4) ? 3_566 . 3_566 3_566 Cl(3) Cl(5) C(16) Cl(3) 164(2) ? 3_566 . . . Cl(3) Cl(5) C(16) Cl(4) -111(2) ? 3_566 . . . Cl(3) Cl(5) C(16) C(17) -163(2) ? 3_566 . . . Cl(3) Cl(5) C(17) Cl(3) -76.7(16) ? 3_566 . . . Cl(3) Cl(5) C(17) Cl(4) 128.0(13) ? 3_566 . . . Cl(3) Cl(5) C(17) C(16) 165.2(17) ? 3_566 . . . Cl(5) Cl(5) C(16) Cl(3) 14.2(18) ? 3_566 . . . Cl(5) Cl(5) C(16) Cl(4) 98(2) ? 3_566 . . . Cl(5) Cl(5) C(16) C(17) 47(2) ? 3_566 . . . C(16) Cl(5) Cl(5) Cl(3) -12.7(16) ? . . 3_566 . C(16) Cl(5) Cl(5) Cl(3) 167.3(17) ? . . 3_566 3_566 C(16) Cl(5) Cl(5) C(17) 148.3(17) ? . . 3_566 3_566 Cl(5) Cl(5) C(17) Cl(3) -36.6(9) ? 3_566 . . . Cl(5) Cl(5) C(17) Cl(4) 168.1(6) ? 3_566 . . . Cl(5) Cl(5) C(17) C(16) -154.7(11) ? 3_566 . . . C(17) Cl(5) Cl(5) Cl(3) 19.0(4) ? . . 3_566 . C(17) Cl(5) Cl(5) Cl(3) -161.0(6) ? . . 3_566 3_566 C(17) Cl(5) Cl(5) C(16) -148.3(17) ? . . 3_566 3_566 C(16) Cl(5) C(17) Cl(3) 118.0(12) ? . . . . C(16) Cl(5) C(17) Cl(4) -37.2(10) ? . . . . C(17) Cl(5) C(16) Cl(3) -32.6(6) ? . . . . C(17) Cl(5) C(16) Cl(4) 51.7(13) ? . . . . Ti(1) O(1) C(10) C(11) 99.9(8) ? . . . . Ti(1) O(1) C(10) C(15) -81.5(8) ? . . . . N(2) N(1) C(1) C(2) 0.6(4) ? . . . . C(1) N(1) N(2) Ti(1) 177.1(2) ? . . . . C(1) N(1) N(2) C(3) -0.8(4) ? . . . . N(2) N(1) B(1) N(3) 58.9(3) ? . . . . N(2) N(1) B(1) N(5) -56.3(4) ? . . . . B(1) N(1) N(2) Ti(1) -1.1(4) ? . . . . B(1) N(1) N(2) C(3) -179.0(3) ? . . . . C(1) N(1) B(1) N(3) -118.9(4) ? . . . . C(1) N(1) B(1) N(5) 126.0(4) ? . . . . B(1) N(1) C(1) C(2) 178.5(3) ? . . . . Ti(1) N(2) C(3) C(2) -177.1(2) ? . . . . N(1) N(2) C(3) C(2) 0.6(4) ? . . . . N(4) N(3) C(4) C(5) 0.2(4) ? . . . . C(4) N(3) N(4) Ti(1) -179.7(2) ? . . . . C(4) N(3) N(4) C(6) -0.0(3) ? . . . . N(4) N(3) B(1) N(1) -58.4(3) ? . . . . N(4) N(3) B(1) N(5) 57.0(4) ? . . . . B(1) N(3) N(4) Ti(1) -0.0(3) ? . . . . B(1) N(3) N(4) C(6) 179.6(3) ? . . . . C(4) N(3) B(1) N(1) 121.2(4) ? . . . . C(4) N(3) B(1) N(5) -123.5(4) ? . . . . B(1) N(3) C(4) C(5) -179.4(3) ? . . . . Ti(1) N(4) C(6) C(5) 179.5(2) ? . . . . N(3) N(4) C(6) C(5) -0.2(3) ? . . . . N(6) N(5) C(7) C(8) -0.6(5) ? . . . . C(7) N(5) N(6) Ti(1) 179.4(2) ? . . . . C(7) N(5) N(6) C(9) 0.5(4) ? . . . . N(6) N(5) B(1) N(1) 58.8(4) ? . . . . N(6) N(5) B(1) N(3) -56.0(4) ? . . . . B(1) N(5) N(6) Ti(1) -2.4(4) ? . . . . B(1) N(5) N(6) C(9) 178.7(3) ? . . . . C(7) N(5) B(1) N(1) -123.4(4) ? . . . . C(7) N(5) B(1) N(3) 121.7(4) ? . . . . B(1) N(5) C(7) C(8) -178.5(4) ? . . . . Ti(1) N(6) C(9) C(8) -179.0(3) ? . . . . N(5) N(6) C(9) C(8) -0.2(4) ? . . . . N(1) C(1) C(2) C(3) -0.3(4) ? . . . . C(1) C(2) C(3) N(2) -0.2(4) ? . . . . N(3) C(4) C(5) C(6) -0.3(4) ? . . . . C(4) C(5) C(6) N(4) 0.3(4) ? . . . . N(5) C(7) C(8) C(9) 0.4(5) ? . . . . C(7) C(8) C(9) N(6) -0.1(4) ? . . . . O(1) C(10) C(11) F(1) -0.8(5) ? . . . . O(1) C(10) C(11) C(12) 179.1(3) ? . . . . O(1) C(10) C(15) F(5) -0.9(5) ? . . . . O(1) C(10) C(15) C(14) -179.2(3) ? . . . . C(11) C(10) C(15) F(5) 177.8(3) ? . . . . C(11) C(10) C(15) C(14) -0.5(5) ? . . . . C(15) C(10) C(11) F(1) -179.5(3) ? . . . . C(15) C(10) C(11) C(12) 0.4(5) ? . . . . F(1) C(11) C(12) F(2) 1.0(5) ? . . . . F(1) C(11) C(12) C(13) -180.0(2) ? . . . . C(10) C(11) C(12) F(2) -178.9(3) ? . . . . C(10) C(11) C(12) C(13) 0.1(4) ? . . . . F(2) C(12) C(13) F(3) -0.3(5) ? . . . . F(2) C(12) C(13) C(14) 178.5(3) ? . . . . C(11) C(12) C(13) F(3) -179.3(3) ? . . . . C(11) C(12) C(13) C(14) -0.5(6) ? . . . . F(3) C(13) C(14) F(4) -0.1(4) ? . . . . F(3) C(13) C(14) C(15) 179.1(3) ? . . . . C(12) C(13) C(14) F(4) -179.0(3) ? . . . . C(12) C(13) C(14) C(15) 0.3(6) ? . . . . F(4) C(14) C(15) F(5) 1.1(5) ? . . . . F(4) C(14) C(15) C(10) 179.5(3) ? . . . . C(13) C(14) C(15) F(5) -178.1(3) ? . . . . C(13) C(14) C(15) C(10) 0.2(5) ? . . . . Cl(3) C(16) C(17) Cl(4) -146.0(9) ? . . . . Cl(3) C(16) C(17) Cl(5) 69.5(10) ? . . . . Cl(4) C(16) C(17) Cl(3) 146.0(9) ? . . . . Cl(4) C(16) C(17) Cl(5) -144.5(8) ? . . . . Cl(5) C(16) C(17) Cl(3) -69.5(10) ? . . . . Cl(5) C(16) C(17) Cl(4) 144.5(8) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(1) F(2) 3.459(2) ? . 2_546 Cl(1) F(3) 3.352(3) ? . 2_546 Cl(1) C(12) 3.365(4) ? . 2_546 Cl(1) C(13) 3.307(4) ? . 2_546 Cl(2) F(2) 3.349(3) ? . 2_546 Cl(2) C(6) 3.585(4) ? . 4_554 Cl(2) C(12) 3.432(4) ? . 4_554 Cl(3) F(5) 3.133(5) ? . 2_556 Cl(3) C(10) 3.580(5) ? . . Cl(3) C(11) 3.560(5) ? . . Cl(5) F(4) 3.352(8) ? . 4_554 F(1) F(5) 3.017(3) ? . 2_556 F(1) C(1) 3.175(4) ? . 2_656 F(1) C(2) 3.164(4) ? . 2_656 F(2) Cl(1) 3.459(2) ? . 2_556 F(2) Cl(2) 3.349(3) ? . 2_556 F(2) F(2) 2.860(4) ? . 3_567 F(2) F(3) 2.887(3) ? . 3_567 F(2) F(5) 3.098(4) ? . 2_556 F(2) C(12) 3.456(5) ? . 3_567 F(2) C(13) 3.471(5) ? . 3_567 F(3) Cl(1) 3.352(3) ? . 2_556 F(3) F(2) 2.887(3) ? . 3_567 F(4) Cl(5) 3.352(8) ? . 4_555 F(4) C(4) 3.420(5) ? . 1_455 F(4) C(16) 3.313(16) ? . 4_555 F(4) B(1) 3.451(4) ? . 1_455 F(5) Cl(3) 3.133(5) ? . 2_546 F(5) F(1) 3.017(3) ? . 2_546 F(5) F(2) 3.098(4) ? . 2_546 F(5) C(11) 3.485(4) ? . 2_546 F(5) C(12) 3.529(5) ? . 2_546 C(1) F(1) 3.175(4) ? . 2_646 C(2) F(1) 3.164(4) ? . 2_646 C(2) C(4) 3.587(5) ? . 2_646 C(3) C(4) 3.570(5) ? . 2_646 C(4) F(4) 3.420(5) ? . 1_655 C(4) C(2) 3.587(5) ? . 2_656 C(4) C(3) 3.570(5) ? . 2_656 C(6) Cl(2) 3.585(4) ? . 4_555 C(10) Cl(3) 3.580(5) ? . . C(11) Cl(3) 3.560(5) ? . . C(11) F(5) 3.485(4) ? . 2_556 C(12) Cl(1) 3.365(4) ? . 2_556 C(12) Cl(2) 3.432(4) ? . 4_555 C(12) F(2) 3.456(5) ? . 3_567 C(12) F(5) 3.529(5) ? . 2_556 C(13) Cl(1) 3.307(4) ? . 2_556 C(13) F(2) 3.471(5) ? . 3_567 C(16) F(4) 3.313(16) ? . 4_554 B(1) F(4) 3.451(4) ? . 1_655 Cl(1) H(7) 2.778 ? . 2_646 Cl(1) H(10) 3.416 ? . 2_646 Cl(2) H(5) 3.426 ? . 4_554 Cl(2) H(6) 3.060 ? . 4_554 Cl(3) H(9) 3.053 ? . . Cl(4) H(1) 3.099 ? . 1_455 Cl(4) H(4) 3.421 ? . 4_454 Cl(4) H(8) 3.301 ? . 3_566 Cl(4) H(10) 3.465 ? . 1_455 Cl(5) H(9) 3.024 ? . . Cl(5) H(9) 2.891 ? . 3_566 F(1) H(1) 2.730 ? . 2_656 F(1) H(2) 2.736 ? . 2_656 F(3) H(3) 2.955 ? . 2_556 F(3) H(4) 2.826 ? . 1_455 F(4) H(1) 3.108 ? . 1_455 F(4) H(4) 2.863 ? . 1_455 F(4) H(8) 3.106 ? . 2_546 F(4) H(10) 2.787 ? . 1_455 F(5) H(1) 3.013 ? . 1_455 N(1) H(5) 2.866 ? . 4_554 N(2) H(5) 2.829 ? . 4_554 N(2) H(7) 3.410 ? . 2_646 N(3) H(2) 3.371 ? . 2_656 N(3) H(3) 3.538 ? . 2_656 N(3) H(8) 3.336 ? . 2_646 N(4) H(2) 3.544 ? . 2_656 N(4) H(7) 3.192 ? . 2_646 N(5) H(5) 2.945 ? . 4_554 N(6) H(5) 2.970 ? . 4_554 C(1) H(5) 3.247 ? . 4_554 C(2) H(3) 3.458 ? . 3_656 C(2) H(5) 3.437 ? . 4_554 C(3) H(2) 3.314 ? . 3_656 C(3) H(4) 3.382 ? . 2_646 C(3) H(5) 3.166 ? . 4_554 C(3) H(7) 3.591 ? . 2_646 C(4) H(2) 3.129 ? . 2_656 C(4) H(3) 3.057 ? . 2_656 C(4) H(8) 2.929 ? . 2_646 C(5) H(2) 3.160 ? . 2_656 C(5) H(8) 3.176 ? . 2_646 C(6) H(2) 3.404 ? . 2_656 C(6) H(7) 3.237 ? . 2_646 C(7) H(5) 3.343 ? . 4_554 C(8) H(5) 3.592 ? . 4_554 C(9) H(5) 3.356 ? . 4_554 C(9) H(6) 3.522 ? . 4_554 C(14) H(10) 3.306 ? . 1_455 C(16) H(9) 3.466 ? . . C(17) H(9) 3.316 ? . 3_566 B(1) H(5) 3.480 ? . 4_554 H(1) Cl(4) 3.099 ? . 1_655 H(1) F(1) 2.730 ? . 2_646 H(1) F(4) 3.108 ? . 1_655 H(1) F(5) 3.013 ? . 1_655 H(2) F(1) 2.736 ? . 2_646 H(2) N(3) 3.371 ? . 2_646 H(2) N(4) 3.544 ? . 2_646 H(2) C(3) 3.314 ? . 3_656 H(2) C(4) 3.129 ? . 2_646 H(2) C(5) 3.160 ? . 2_646 H(2) C(6) 3.404 ? . 2_646 H(2) H(2) 3.564 ? . 3_656 H(2) H(3) 2.958 ? . 3_656 H(2) H(4) 3.442 ? . 2_646 H(2) H(5) 3.500 ? . 2_646 H(3) F(3) 2.955 ? . 2_546 H(3) N(3) 3.538 ? . 2_646 H(3) C(2) 3.458 ? . 3_656 H(3) C(4) 3.057 ? . 2_646 H(3) H(2) 2.958 ? . 3_656 H(3) H(4) 2.663 ? . 2_646 H(3) H(10) 3.511 ? . 2_646 H(4) Cl(4) 3.421 ? . 4_655 H(4) F(3) 2.826 ? . 1_655 H(4) F(4) 2.863 ? . 1_655 H(4) C(3) 3.382 ? . 2_656 H(4) H(2) 3.442 ? . 2_656 H(4) H(3) 2.663 ? . 2_656 H(4) H(8) 3.043 ? . 2_646 H(5) Cl(2) 3.426 ? . 4_555 H(5) N(1) 2.866 ? . 4_555 H(5) N(2) 2.829 ? . 4_555 H(5) N(5) 2.945 ? . 4_555 H(5) N(6) 2.970 ? . 4_555 H(5) C(1) 3.247 ? . 4_555 H(5) C(2) 3.437 ? . 4_555 H(5) C(3) 3.166 ? . 4_555 H(5) C(7) 3.343 ? . 4_555 H(5) C(8) 3.592 ? . 4_555 H(5) C(9) 3.356 ? . 4_555 H(5) B(1) 3.480 ? . 4_555 H(5) H(2) 3.500 ? . 2_656 H(5) H(8) 3.469 ? . 2_646 H(6) Cl(2) 3.060 ? . 4_555 H(6) C(9) 3.522 ? . 4_555 H(6) H(7) 3.438 ? . 2_646 H(6) H(9) 3.413 ? . 4_555 H(7) Cl(1) 2.778 ? . 2_656 H(7) N(2) 3.410 ? . 2_656 H(7) N(4) 3.192 ? . 2_656 H(7) C(3) 3.591 ? . 2_656 H(7) C(6) 3.237 ? . 2_656 H(7) H(6) 3.438 ? . 2_656 H(8) Cl(4) 3.301 ? . 3_566 H(8) F(4) 3.106 ? . 2_556 H(8) N(3) 3.336 ? . 2_656 H(8) C(4) 2.929 ? . 2_656 H(8) C(5) 3.176 ? . 2_656 H(8) H(4) 3.043 ? . 2_656 H(8) H(5) 3.469 ? . 2_656 H(9) Cl(3) 3.053 ? . . H(9) Cl(5) 3.024 ? . . H(9) Cl(5) 2.891 ? . 3_566 H(9) C(16) 3.466 ? . . H(9) C(17) 3.316 ? . 3_566 H(9) H(6) 3.413 ? . 4_554 H(10) Cl(1) 3.416 ? . 2_656 H(10) Cl(4) 3.465 ? . 1_655 H(10) F(4) 2.787 ? . 1_655 H(10) C(14) 3.306 ? . 1_655 H(10) H(3) 3.511 ? . 2_656 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_TpTiCl2(O26Ph2C6H3) _database_code_depnum_ccdc_archive 'CCDC 731708' _audit_creation_date 2009-07-15 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C27 H23 B Cl2 N6 O Ti ' _chemical_formula_moiety 'C27 H23 B Cl2 N6 O Ti ' _chemical_formula_weight 577.13 _chemical_melting_point ? _chemical_absolute_configuration ad #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2+X,1/2-Y,-Z 3 -X,1/2+Y,1/2-Z 4 1/2-X,-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 11.6472(3) _cell_length_b 13.6516(3) _cell_length_c 17.3088(5) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 2752.14(12) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25705 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184.00 _exptl_absorpt_coefficient_mu 0.537 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.746 _exptl_absorpt_correction_T_max 0.874 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 27327 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_theta_max 27.45 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_ambient_temperature 193.1 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 1.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6279 _reflns_number_gt 6055 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0195 _refine_ls_wR_factor_ref 0.0609 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6172 _refine_ls_number_parameters 367 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0006Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.35 _refine_diff_density_min -0.36 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 2761 Friedel Pairs' _refine_ls_abs_structure_Flack -0.001(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; B B 0.001 0.001 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ti Ti 0.278 0.446 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ti(1) Ti 0.69446(2) 0.182220(10) 0.279510(10) 0.01454(4) Uani 1.00 1 d . . . Cl(1) Cl 0.74621(3) 0.06013(2) 0.36176(2) 0.02739(7) Uani 1.00 1 d . . . Cl(2) Cl 0.74821(2) 0.31026(2) 0.35783(2) 0.02334(6) Uani 1.00 1 d . . . O(1) O 0.81799(6) 0.17423(6) 0.21787(4) 0.01809(17) Uani 1.00 1 d . . . N(1) N 0.42510(8) 0.17553(8) 0.29786(6) 0.0216(2) Uani 1.00 1 d . . . N(2) N 0.52654(8) 0.17699(8) 0.33717(5) 0.0184(2) Uani 1.00 1 d . . . N(3) N 0.49820(10) 0.08633(8) 0.18313(6) 0.0238(2) Uani 1.00 1 d . . . N(4) N 0.60826(9) 0.07646(7) 0.20830(6) 0.0211(2) Uani 1.00 1 d . . . N(5) N 0.49151(9) 0.26906(8) 0.18380(6) 0.0222(2) Uani 1.00 1 d . . . N(6) N 0.60048(9) 0.28481(7) 0.21018(6) 0.0200(2) Uani 1.00 1 d . . . C(1) C 0.33743(10) 0.17596(10) 0.34796(8) 0.0281(3) Uani 1.00 1 d . . . C(2) C 0.38115(11) 0.17821(10) 0.42225(7) 0.0273(2) Uani 1.00 1 d . . . C(3) C 0.49998(11) 0.17801(9) 0.41254(6) 0.0213(2) Uani 1.00 1 d . . . C(4) C 0.46750(14) 0.00567(10) 0.14354(8) 0.0324(3) Uani 1.00 1 d . . . C(5) C 0.55915(15) -0.05794(10) 0.14230(9) 0.0356(3) Uani 1.00 1 d . . . C(6) C 0.64520(14) -0.01168(9) 0.18382(8) 0.0278(3) Uani 1.00 1 d . . . C(7) C 0.45400(13) 0.34898(10) 0.14622(8) 0.0296(3) Uani 1.00 1 d . . . C(8) C 0.53887(14) 0.41868(10) 0.14762(8) 0.0312(3) Uani 1.00 1 d . . . C(9) C 0.62930(12) 0.37629(9) 0.18770(8) 0.0264(3) Uani 1.00 1 d . . . C(10) C 0.89275(10) 0.11890(8) 0.17559(7) 0.0177(2) Uani 1.00 1 d . . . C(11) C 0.86968(10) 0.10238(8) 0.09675(7) 0.0195(2) Uani 1.00 1 d . . . C(12) C 0.93719(12) 0.03397(9) 0.05769(7) 0.0259(2) Uani 1.00 1 d . . . C(13) C 1.02837(13) -0.01245(10) 0.09378(8) 0.0292(3) Uani 1.00 1 d . . . C(14) C 1.05496(12) 0.00984(9) 0.16966(8) 0.0265(3) Uani 1.00 1 d . . . C(15) C 0.98803(10) 0.07560(8) 0.21245(7) 0.0204(2) Uani 1.00 1 d . . . C(16) C 0.78177(10) 0.15835(9) 0.05289(7) 0.0209(2) Uani 1.00 1 d . . . C(17) C 0.70226(13) 0.10985(10) 0.00605(8) 0.0285(3) Uani 1.00 1 d . . . C(18) C 0.63045(13) 0.16343(11) -0.04270(9) 0.0370(3) Uani 1.00 1 d . . . C(19) C 0.63678(13) 0.26451(12) -0.04498(9) 0.0367(3) Uani 1.00 1 d . . . C(20) C 0.71349(14) 0.31251(11) 0.00214(8) 0.0355(3) Uani 1.00 1 d . . . C(21) C 0.78574(12) 0.26024(10) 0.05084(8) 0.0290(3) Uani 1.00 1 d . . . C(22) C 1.01961(10) 0.09769(9) 0.29375(7) 0.0202(2) Uani 1.00 1 d . . . C(23) C 1.05424(11) 0.02227(10) 0.34328(8) 0.0263(3) Uani 1.00 1 d . . . C(24) C 1.08417(13) 0.04120(11) 0.41934(8) 0.0308(3) Uani 1.00 1 d . . . C(25) C 1.08024(12) 0.13631(11) 0.44766(8) 0.0302(3) Uani 1.00 1 d . . . C(26) C 1.04740(12) 0.21160(10) 0.39890(8) 0.0284(3) Uani 1.00 1 d . . . C(27) C 1.01715(10) 0.19320(10) 0.32264(7) 0.0232(2) Uani 1.00 1 d . . . B(1) B 0.42693(11) 0.17570(11) 0.20839(8) 0.0240(3) Uani 1.00 1 d . . . H(1) H 0.3444 0.1764 0.1866 0.029 Uiso 1.00 1 c R . . H(2) H 0.2558 0.1749 0.3342 0.034 Uiso 1.00 1 c R . . H(3) H 0.3382 0.1795 0.4709 0.033 Uiso 1.00 1 c R . . H(4) H 0.5561 0.1787 0.4547 0.026 Uiso 1.00 1 c R . . H(5) H 0.3919 -0.0060 0.1191 0.040 Uiso 1.00 1 c R . . H(6) H 0.5628 -0.1231 0.1173 0.043 Uiso 1.00 1 c R . . H(7) H 0.7224 -0.0392 0.1939 0.033 Uiso 1.00 1 c R . . H(8) H 0.3778 0.3563 0.1216 0.036 Uiso 1.00 1 c R . . H(9) H 0.5361 0.4851 0.1247 0.038 Uiso 1.00 1 c R . . H(10) H 0.7038 0.4085 0.1984 0.032 Uiso 1.00 1 c R . . H(11) H 0.9199 0.0186 0.0042 0.032 Uiso 1.00 1 c R . . H(12) H 1.0737 -0.0604 0.0658 0.037 Uiso 1.00 1 c R . . H(13) H 1.1210 -0.0208 0.1938 0.032 Uiso 1.00 1 c R . . H(14) H 0.6970 0.0397 0.0075 0.034 Uiso 1.00 1 c R . . H(15) H 0.5761 0.1298 -0.0749 0.045 Uiso 1.00 1 c R . . H(16) H 0.5881 0.3009 -0.0793 0.044 Uiso 1.00 1 c R . . H(17) H 0.7169 0.3828 0.0015 0.043 Uiso 1.00 1 c R . . H(18) H 0.8391 0.2947 0.0832 0.035 Uiso 1.00 1 c R . . H(19) H 1.0575 -0.0431 0.3245 0.032 Uiso 1.00 1 c R . . H(20) H 1.1074 -0.0109 0.4522 0.037 Uiso 1.00 1 c R . . H(21) H 1.0998 0.1494 0.4999 0.036 Uiso 1.00 1 c R . . H(22) H 1.0456 0.2769 0.4179 0.035 Uiso 1.00 1 c R . . H(23) H 0.9947 0.2457 0.2900 0.028 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti(1) 0.01426(9) 0.01473(9) 0.01464(9) 0.00018(8) 0.00031(7) -0.00061(7) Cl(1) 0.02499(15) 0.02713(15) 0.03005(16) 0.00267(12) -0.00173(13) 0.01141(12) Cl(2) 0.02267(14) 0.02271(13) 0.02463(14) -0.00314(12) -0.00063(11) -0.00745(11) O(1) 0.0165(3) 0.0202(3) 0.0176(3) 0.0029(3) 0.0013(3) -0.0013(3) N(1) 0.0160(4) 0.0267(4) 0.0222(4) -0.0017(4) -0.0013(3) 0.0024(4) N(2) 0.0173(4) 0.0197(4) 0.0181(4) -0.0003(4) -0.0005(3) 0.0013(3) N(3) 0.0248(5) 0.0255(5) 0.0210(5) -0.0063(4) -0.0041(4) -0.0024(4) N(4) 0.0227(4) 0.0205(4) 0.0202(5) -0.0027(4) 0.0013(4) -0.0025(3) N(5) 0.0196(4) 0.0270(5) 0.0202(5) 0.0034(4) -0.0028(4) 0.0024(4) N(6) 0.0193(4) 0.0201(4) 0.0206(4) 0.0017(3) -0.0003(4) 0.0022(3) C(1) 0.0185(5) 0.0341(6) 0.0317(6) 0.0007(5) 0.0050(4) 0.0047(5) C(2) 0.0256(5) 0.0299(6) 0.0265(6) 0.0016(5) 0.0086(4) 0.0030(5) C(3) 0.0258(5) 0.0193(4) 0.0188(5) -0.0003(5) 0.0021(4) -0.0003(4) C(4) 0.0417(8) 0.0317(6) 0.0239(6) -0.0161(6) -0.0048(6) -0.0047(5) C(5) 0.0542(9) 0.0232(6) 0.0294(7) -0.0115(6) 0.0031(6) -0.0075(5) C(6) 0.0405(7) 0.0188(5) 0.0242(6) -0.0017(5) 0.0053(5) -0.0038(4) C(7) 0.0327(6) 0.0313(6) 0.0249(6) 0.0120(5) -0.0026(5) 0.0035(5) C(8) 0.0433(8) 0.0228(6) 0.0276(6) 0.0080(5) -0.0030(6) 0.0052(5) C(9) 0.0326(6) 0.0209(5) 0.0256(6) -0.0003(5) 0.0009(5) 0.0024(4) C(10) 0.0172(5) 0.0173(5) 0.0184(5) -0.0004(4) 0.0030(4) -0.0022(4) C(11) 0.0212(5) 0.0192(5) 0.0180(5) -0.0005(4) 0.0009(4) -0.0005(4) C(12) 0.0345(6) 0.0240(5) 0.0192(5) 0.0030(5) 0.0023(5) -0.0050(4) C(13) 0.0358(7) 0.0245(6) 0.0272(6) 0.0104(5) 0.0062(5) -0.0054(4) C(14) 0.0255(6) 0.0253(5) 0.0288(6) 0.0088(5) 0.0014(5) -0.0005(5) C(15) 0.0215(5) 0.0192(5) 0.0206(6) 0.0017(4) 0.0013(4) -0.0001(4) C(16) 0.0219(5) 0.0256(5) 0.0151(4) 0.0027(4) 0.0008(4) -0.0013(4) C(17) 0.0317(6) 0.0279(6) 0.0260(6) -0.0016(5) -0.0028(5) -0.0034(4) C(18) 0.0333(6) 0.0433(8) 0.0344(7) -0.0020(6) -0.0138(6) -0.0051(6) C(19) 0.0340(7) 0.0438(8) 0.0324(7) 0.0114(6) -0.0093(6) 0.0028(6) C(20) 0.0438(7) 0.0281(6) 0.0347(7) 0.0067(6) -0.0086(6) 0.0028(5) C(21) 0.0316(7) 0.0269(6) 0.0285(6) -0.0005(5) -0.0078(5) -0.0013(5) C(22) 0.0155(5) 0.0255(5) 0.0195(5) 0.0027(4) 0.0019(4) -0.0012(4) C(23) 0.0247(6) 0.0257(6) 0.0285(6) 0.0017(5) -0.0015(5) 0.0012(4) C(24) 0.0302(6) 0.0363(6) 0.0260(6) 0.0024(5) -0.0027(5) 0.0070(5) C(25) 0.0251(6) 0.0449(7) 0.0205(6) 0.0030(5) -0.0030(5) -0.0046(5) C(26) 0.0255(6) 0.0321(6) 0.0276(6) 0.0034(5) -0.0009(5) -0.0084(5) C(27) 0.0197(5) 0.0258(5) 0.0240(5) 0.0043(5) -0.0012(4) -0.0015(5) B(1) 0.0193(5) 0.0309(6) 0.0217(6) -0.0030(5) -0.0039(4) 0.0004(5) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ti(1) Cl(1) 2.2733(3) yes . . Ti(1) Cl(2) 2.2989(3) yes . . Ti(1) O(1) 1.7945(7) yes . . Ti(1) N(2) 2.1969(9) yes . . Ti(1) N(4) 2.1475(10) yes . . Ti(1) N(6) 2.1447(10) yes . . O(1) C(10) 1.3654(13) yes . . N(1) N(2) 1.3635(13) yes . . N(1) C(1) 1.3397(15) yes . . N(1) B(1) 1.5488(17) yes . . N(2) C(3) 1.3408(13) yes . . N(3) N(4) 1.3606(15) yes . . N(3) C(4) 1.3453(17) yes . . N(3) B(1) 1.5391(18) yes . . N(4) C(6) 1.3463(16) yes . . N(5) N(6) 1.3659(14) yes . . N(5) C(7) 1.3433(17) yes . . N(5) B(1) 1.5399(18) yes . . N(6) C(9) 1.3504(15) yes . . C(1) C(2) 1.3834(18) yes . . C(2) C(3) 1.3942(18) yes . . C(4) C(5) 1.376(2) yes . . C(5) C(6) 1.386(2) yes . . C(7) C(8) 1.372(2) yes . . C(8) C(9) 1.388(2) yes . . C(10) C(11) 1.4090(17) yes . . C(10) C(15) 1.4100(16) yes . . C(11) C(12) 1.3955(17) yes . . C(11) C(16) 1.4861(16) yes . . C(12) C(13) 1.3855(19) yes . . C(13) C(14) 1.3833(19) yes . . C(14) C(15) 1.4008(17) yes . . C(15) C(22) 1.4854(17) yes . . C(16) C(17) 1.3976(18) yes . . C(16) C(21) 1.3922(18) yes . . C(17) C(18) 1.395(2) yes . . C(18) C(19) 1.382(2) yes . . C(19) C(20) 1.376(2) yes . . C(20) C(21) 1.388(2) yes . . C(22) C(23) 1.3992(18) yes . . C(22) C(27) 1.3968(18) yes . . C(23) C(24) 1.3862(19) yes . . C(24) C(25) 1.389(2) yes . . C(25) C(26) 1.3838(19) yes . . C(26) C(27) 1.3891(18) yes . . C(1) H(2) 0.980 no . . C(2) H(3) 0.980 no . . C(3) H(4) 0.980 no . . C(4) H(5) 0.990 no . . C(5) H(6) 0.990 no . . C(6) H(7) 0.990 no . . C(7) H(8) 0.990 no . . C(8) H(9) 0.990 no . . C(9) H(10) 0.990 no . . C(12) H(11) 0.970 no . . C(13) H(12) 0.970 no . . C(14) H(13) 0.970 no . . C(17) H(14) 0.960 no . . C(18) H(15) 0.960 no . . C(19) H(16) 0.960 no . . C(20) H(17) 0.960 no . . C(21) H(18) 0.960 no . . C(23) H(19) 0.950 no . . C(24) H(20) 0.950 no . . C(25) H(21) 0.950 no . . C(26) H(22) 0.950 no . . C(27) H(23) 0.950 no . . B(1) H(1) 1.033 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) Ti(1) Cl(2) 96.660(13) yes . . . Cl(1) Ti(1) O(1) 96.61(2) yes . . . Cl(1) Ti(1) N(2) 85.85(2) yes . . . Cl(1) Ti(1) N(4) 89.45(2) yes . . . Cl(1) Ti(1) N(6) 164.69(3) yes . . . Cl(2) Ti(1) O(1) 100.28(2) yes . . . Cl(2) Ti(1) N(2) 89.96(2) yes . . . Cl(2) Ti(1) N(4) 167.67(3) yes . . . Cl(2) Ti(1) N(6) 88.42(2) yes . . . O(1) Ti(1) N(2) 169.08(3) yes . . . O(1) Ti(1) N(4) 89.58(3) yes . . . O(1) Ti(1) N(6) 96.67(3) yes . . . N(2) Ti(1) N(4) 79.79(3) yes . . . N(2) Ti(1) N(6) 79.69(3) yes . . . N(4) Ti(1) N(6) 83.07(3) yes . . . Ti(1) O(1) C(10) 149.72(7) yes . . . N(2) N(1) C(1) 109.72(9) yes . . . N(2) N(1) B(1) 119.14(8) yes . . . C(1) N(1) B(1) 131.13(10) yes . . . Ti(1) N(2) N(1) 123.04(6) yes . . . Ti(1) N(2) C(3) 130.32(7) yes . . . N(1) N(2) C(3) 106.60(9) yes . . . N(4) N(3) C(4) 109.42(11) yes . . . N(4) N(3) B(1) 119.72(9) yes . . . C(4) N(3) B(1) 130.55(11) yes . . . Ti(1) N(4) N(3) 123.89(7) yes . . . Ti(1) N(4) C(6) 129.21(9) yes . . . N(3) N(4) C(6) 106.79(10) yes . . . N(6) N(5) C(7) 109.65(10) yes . . . N(6) N(5) B(1) 119.46(9) yes . . . C(7) N(5) B(1) 130.33(11) yes . . . Ti(1) N(6) N(5) 123.95(7) yes . . . Ti(1) N(6) C(9) 129.66(8) yes . . . N(5) N(6) C(9) 106.27(10) yes . . . N(1) C(1) C(2) 108.74(10) yes . . . C(1) C(2) C(3) 104.67(10) yes . . . N(2) C(3) C(2) 110.26(10) yes . . . N(3) C(4) C(5) 108.56(13) yes . . . C(4) C(5) C(6) 105.39(12) yes . . . N(4) C(6) C(5) 109.84(13) yes . . . N(5) C(7) C(8) 108.68(12) yes . . . C(7) C(8) C(9) 105.45(12) yes . . . N(6) C(9) C(8) 109.94(11) yes . . . O(1) C(10) C(11) 119.08(9) yes . . . O(1) C(10) C(15) 119.43(10) yes . . . C(11) C(10) C(15) 121.42(10) yes . . . C(10) C(11) C(12) 117.96(10) yes . . . C(10) C(11) C(16) 122.95(10) yes . . . C(12) C(11) C(16) 119.00(10) yes . . . C(11) C(12) C(13) 121.30(11) yes . . . C(12) C(13) C(14) 119.94(12) yes . . . C(13) C(14) C(15) 121.23(12) yes . . . C(10) C(15) C(14) 117.87(11) yes . . . C(10) C(15) C(22) 122.58(10) yes . . . C(14) C(15) C(22) 119.55(10) yes . . . C(11) C(16) C(17) 120.62(11) yes . . . C(11) C(16) C(21) 120.25(10) yes . . . C(17) C(16) C(21) 118.72(11) yes . . . C(16) C(17) C(18) 119.98(12) yes . . . C(17) C(18) C(19) 120.57(13) yes . . . C(18) C(19) C(20) 119.55(14) yes . . . C(19) C(20) C(21) 120.58(13) yes . . . C(16) C(21) C(20) 120.59(12) yes . . . C(15) C(22) C(23) 120.16(11) yes . . . C(15) C(22) C(27) 121.57(10) yes . . . C(23) C(22) C(27) 118.26(11) yes . . . C(22) C(23) C(24) 121.15(12) yes . . . C(23) C(24) C(25) 120.09(13) yes . . . C(24) C(25) C(26) 119.23(12) yes . . . C(25) C(26) C(27) 121.02(12) yes . . . C(22) C(27) C(26) 120.25(11) yes . . . N(1) B(1) N(3) 106.88(10) yes . . . N(1) B(1) N(5) 106.52(10) yes . . . N(3) B(1) N(5) 108.31(9) yes . . . N(1) C(1) H(2) 125.6 no . . . C(2) C(1) H(2) 125.6 no . . . C(1) C(2) H(3) 127.7 no . . . C(3) C(2) H(3) 127.7 no . . . N(2) C(3) H(4) 124.8 no . . . C(2) C(3) H(4) 124.9 no . . . N(3) C(4) H(5) 125.8 no . . . C(5) C(4) H(5) 125.6 no . . . C(4) C(5) H(6) 127.4 no . . . C(6) C(5) H(6) 127.2 no . . . N(4) C(6) H(7) 125.0 no . . . C(5) C(6) H(7) 125.1 no . . . N(5) C(7) H(8) 125.6 no . . . C(8) C(7) H(8) 125.7 no . . . C(7) C(8) H(9) 127.2 no . . . C(9) C(8) H(9) 127.4 no . . . N(6) C(9) H(10) 125.1 no . . . C(8) C(9) H(10) 124.9 no . . . C(11) C(12) H(11) 119.3 no . . . C(13) C(12) H(11) 119.4 no . . . C(12) C(13) H(12) 120.0 no . . . C(14) C(13) H(12) 120.0 no . . . C(13) C(14) H(13) 119.4 no . . . C(15) C(14) H(13) 119.3 no . . . C(16) C(17) H(14) 120.0 no . . . C(18) C(17) H(14) 120.0 no . . . C(17) C(18) H(15) 119.7 no . . . C(19) C(18) H(15) 119.8 no . . . C(18) C(19) H(16) 120.2 no . . . C(20) C(19) H(16) 120.3 no . . . C(19) C(20) H(17) 119.7 no . . . C(21) C(20) H(17) 119.7 no . . . C(16) C(21) H(18) 119.7 no . . . C(20) C(21) H(18) 119.7 no . . . C(22) C(23) H(19) 119.5 no . . . C(24) C(23) H(19) 119.3 no . . . C(23) C(24) H(20) 120.0 no . . . C(25) C(24) H(20) 119.9 no . . . C(24) C(25) H(21) 120.3 no . . . C(26) C(25) H(21) 120.5 no . . . C(25) C(26) H(22) 119.5 no . . . C(27) C(26) H(22) 119.5 no . . . C(22) C(27) H(23) 119.8 no . . . C(26) C(27) H(23) 119.9 no . . . N(1) B(1) H(1) 110.7 no . . . N(3) B(1) H(1) 113.9 no . . . N(5) B(1) H(1) 110.2 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cl(1) Ti(1) O(1) C(10) 47.48(14) ? . . . . Cl(1) Ti(1) N(2) N(1) -133.06(9) ? . . . . Cl(1) Ti(1) N(2) C(3) 49.51(10) ? . . . . Cl(1) Ti(1) N(4) N(3) 129.53(8) ? . . . . Cl(1) Ti(1) N(4) C(6) -46.14(11) ? . . . . Cl(1) Ti(1) N(6) N(5) -25.11(17) ? . . . . Cl(1) Ti(1) N(6) C(9) 150.50(9) ? . . . . Cl(2) Ti(1) O(1) C(10) 145.51(13) ? . . . . Cl(2) Ti(1) N(2) N(1) 130.26(9) ? . . . . Cl(2) Ti(1) N(2) C(3) -47.17(11) ? . . . . Cl(2) Ti(1) N(4) N(3) 9.5(2) ? . . . . Cl(2) Ti(1) N(4) C(6) -166.12(10) ? . . . . Cl(2) Ti(1) N(6) N(5) -134.90(8) ? . . . . Cl(2) Ti(1) N(6) C(9) 40.71(10) ? . . . . O(1) Ti(1) N(2) N(1) -29.5(2) ? . . . . O(1) Ti(1) N(2) C(3) 153.05(17) ? . . . . N(2) Ti(1) O(1) C(10) -55.1(2) ? . . . . O(1) Ti(1) N(4) N(3) -133.86(9) ? . . . . O(1) Ti(1) N(4) C(6) 50.48(11) ? . . . . N(4) Ti(1) O(1) C(10) -41.92(14) ? . . . . O(1) Ti(1) N(6) N(5) 124.93(9) ? . . . . O(1) Ti(1) N(6) C(9) -59.46(11) ? . . . . N(6) Ti(1) O(1) C(10) -124.89(14) ? . . . . N(2) Ti(1) N(4) N(3) 43.64(9) ? . . . . N(2) Ti(1) N(4) C(6) -132.03(11) ? . . . . N(4) Ti(1) N(2) N(1) -42.87(9) ? . . . . N(4) Ti(1) N(2) C(3) 139.70(11) ? . . . . N(2) Ti(1) N(6) N(5) -44.65(8) ? . . . . N(2) Ti(1) N(6) C(9) 130.96(11) ? . . . . N(6) Ti(1) N(2) N(1) 41.86(9) ? . . . . N(6) Ti(1) N(2) C(3) -135.57(11) ? . . . . N(4) Ti(1) N(6) N(5) 36.17(9) ? . . . . N(4) Ti(1) N(6) C(9) -148.22(11) ? . . . . N(6) Ti(1) N(4) N(3) -37.08(9) ? . . . . N(6) Ti(1) N(4) C(6) 147.25(11) ? . . . . Ti(1) O(1) C(10) C(11) 91.68(15) ? . . . . Ti(1) O(1) C(10) C(15) -85.19(16) ? . . . . N(2) N(1) C(1) C(2) 0.28(15) ? . . . . C(1) N(1) N(2) Ti(1) -177.76(8) ? . . . . C(1) N(1) N(2) C(3) 0.20(13) ? . . . . N(2) N(1) B(1) N(3) 56.99(14) ? . . . . N(2) N(1) B(1) N(5) -58.63(13) ? . . . . B(1) N(1) N(2) Ti(1) 1.11(14) ? . . . . B(1) N(1) N(2) C(3) 179.06(10) ? . . . . C(1) N(1) B(1) N(3) -124.43(13) ? . . . . C(1) N(1) B(1) N(5) 119.95(13) ? . . . . B(1) N(1) C(1) C(2) -178.41(12) ? . . . . Ti(1) N(2) C(3) C(2) 177.15(8) ? . . . . N(1) N(2) C(3) C(2) -0.60(14) ? . . . . N(4) N(3) C(4) C(5) -0.37(15) ? . . . . C(4) N(3) N(4) Ti(1) -176.62(8) ? . . . . C(4) N(3) N(4) C(6) -0.13(13) ? . . . . N(4) N(3) B(1) N(1) -57.12(13) ? . . . . N(4) N(3) B(1) N(5) 57.30(13) ? . . . . B(1) N(3) N(4) Ti(1) -2.37(14) ? . . . . B(1) N(3) N(4) C(6) 174.12(10) ? . . . . C(4) N(3) B(1) N(1) 115.73(13) ? . . . . C(4) N(3) B(1) N(5) -129.85(13) ? . . . . B(1) N(3) C(4) C(5) -173.78(12) ? . . . . Ti(1) N(4) C(6) C(5) 176.81(9) ? . . . . N(3) N(4) C(6) C(5) 0.57(14) ? . . . . N(6) N(5) C(7) C(8) -0.02(11) ? . . . . C(7) N(5) N(6) Ti(1) 176.28(8) ? . . . . C(7) N(5) N(6) C(9) -0.20(13) ? . . . . N(6) N(5) B(1) N(1) 56.47(13) ? . . . . N(6) N(5) B(1) N(3) -58.18(13) ? . . . . B(1) N(5) N(6) Ti(1) 4.01(14) ? . . . . B(1) N(5) N(6) C(9) -172.47(10) ? . . . . C(7) N(5) B(1) N(1) -113.97(13) ? . . . . C(7) N(5) B(1) N(3) 131.38(13) ? . . . . B(1) N(5) C(7) C(8) 171.15(12) ? . . . . Ti(1) N(6) C(9) C(8) -175.87(9) ? . . . . N(5) N(6) C(9) C(8) 0.34(14) ? . . . . N(1) C(1) C(2) C(3) -0.62(15) ? . . . . C(1) C(2) C(3) N(2) 0.75(14) ? . . . . N(3) C(4) C(5) C(6) 0.69(16) ? . . . . C(4) C(5) C(6) N(4) -0.78(16) ? . . . . N(5) C(7) C(8) C(9) 0.22(15) ? . . . . C(7) C(8) C(9) N(6) -0.35(15) ? . . . . O(1) C(10) C(11) C(12) -170.48(10) ? . . . . O(1) C(10) C(11) C(16) 13.09(16) ? . . . . O(1) C(10) C(15) C(14) 172.38(10) ? . . . . O(1) C(10) C(15) C(22) -8.04(16) ? . . . . C(11) C(10) C(15) C(14) -4.42(16) ? . . . . C(11) C(10) C(15) C(22) 175.16(10) ? . . . . C(15) C(10) C(11) C(12) 6.32(16) ? . . . . C(15) C(10) C(11) C(16) -170.10(10) ? . . . . C(10) C(11) C(12) C(13) -3.59(18) ? . . . . C(10) C(11) C(16) C(17) -132.41(13) ? . . . . C(10) C(11) C(16) C(21) 55.02(16) ? . . . . C(12) C(11) C(16) C(17) 51.20(16) ? . . . . C(12) C(11) C(16) C(21) -121.37(13) ? . . . . C(16) C(11) C(12) C(13) 172.98(11) ? . . . . C(11) C(12) C(13) C(14) -1.0(2) ? . . . . C(12) C(13) C(14) C(15) 3.0(2) ? . . . . C(13) C(14) C(15) C(10) -0.31(18) ? . . . . C(13) C(14) C(15) C(22) -179.90(11) ? . . . . C(10) C(15) C(22) C(23) 138.08(12) ? . . . . C(10) C(15) C(22) C(27) -42.72(16) ? . . . . C(14) C(15) C(22) C(23) -42.35(16) ? . . . . C(14) C(15) C(22) C(27) 136.85(12) ? . . . . C(11) C(16) C(17) C(18) -171.39(12) ? . . . . C(11) C(16) C(21) C(20) 171.56(12) ? . . . . C(17) C(16) C(21) C(20) -1.15(19) ? . . . . C(21) C(16) C(17) C(18) 1.3(2) ? . . . . C(16) C(17) C(18) C(19) -0.3(2) ? . . . . C(17) C(18) C(19) C(20) -1.0(2) ? . . . . C(18) C(19) C(20) C(21) 1.1(2) ? . . . . C(19) C(20) C(21) C(16) -0.05(16) ? . . . . C(15) C(22) C(23) C(24) 179.95(10) ? . . . . C(15) C(22) C(27) C(26) -179.86(11) ? . . . . C(23) C(22) C(27) C(26) -0.64(17) ? . . . . C(27) C(22) C(23) C(24) 0.73(18) ? . . . . C(22) C(23) C(24) C(25) -0.06(15) ? . . . . C(23) C(24) C(25) C(26) -0.7(2) ? . . . . C(24) C(25) C(26) C(27) 0.8(2) ? . . . . C(25) C(26) C(27) C(22) -0.10(19) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(1) C(17) 3.4616(14) ? . 4_655 Cl(2) C(14) 3.5924(13) ? . 3_755 C(1) C(25) 3.4992(18) ? . 1_455 C(1) C(26) 3.5249(18) ? . 1_455 C(2) C(25) 3.5783(18) ? . 1_455 C(4) C(9) 3.5949(19) ? . 3_645 C(9) C(4) 3.5949(19) ? . 3_655 C(14) Cl(2) 3.5924(13) ? . 3_745 C(17) Cl(1) 3.4616(14) ? . 4_654 C(25) C(1) 3.4992(18) ? . 1_655 C(25) C(2) 3.5783(18) ? . 1_655 C(26) C(1) 3.5249(18) ? . 1_655 Cl(1) H(8) 3.149 ? . 3_645 Cl(1) H(9) 3.452 ? . 3_645 Cl(1) H(11) 3.313 ? . 4_655 Cl(1) H(14) 2.942 ? . 4_655 Cl(1) H(15) 3.494 ? . 4_655 Cl(2) H(3) 3.147 ? . 2_556 Cl(2) H(5) 3.020 ? . 3_655 Cl(2) H(12) 3.028 ? . 3_755 Cl(2) H(13) 2.905 ? . 3_755 Cl(2) H(21) 3.058 ? . 2_456 N(1) H(6) 3.119 ? . 3_655 N(1) H(9) 2.960 ? . 3_645 N(2) H(6) 3.025 ? . 3_655 N(2) H(9) 2.798 ? . 3_645 N(4) H(9) 3.569 ? . 3_645 C(1) H(6) 3.039 ? . 3_655 C(1) H(9) 3.031 ? . 3_645 C(2) H(6) 2.873 ? . 3_655 C(2) H(9) 2.923 ? . 3_645 C(2) H(12) 3.007 ? . 4_655 C(2) H(21) 3.564 ? . 1_455 C(2) H(22) 3.420 ? . 2_456 C(3) H(6) 2.859 ? . 3_655 C(3) H(9) 2.744 ? . 3_645 C(3) H(11) 3.255 ? . 4_655 C(3) H(12) 3.218 ? . 4_655 C(3) H(21) 3.033 ? . 2_456 C(3) H(22) 3.045 ? . 2_456 C(4) H(20) 3.426 ? . 4_654 C(4) H(21) 3.358 ? . 4_654 C(5) H(21) 3.325 ? . 4_654 C(7) H(11) 3.195 ? . 2_455 C(8) H(11) 3.092 ? . 2_455 C(10) H(16) 3.025 ? . 2_555 C(11) H(16) 2.882 ? . 2_555 C(12) H(4) 3.407 ? . 4_654 C(12) H(8) 3.514 ? . 2_555 C(12) H(9) 3.371 ? . 2_555 C(12) H(16) 2.883 ? . 2_555 C(12) H(17) 3.599 ? . 2_555 C(12) H(22) 3.541 ? . 3_745 C(13) H(3) 3.485 ? . 4_654 C(13) H(4) 3.451 ? . 4_654 C(13) H(16) 2.981 ? . 2_555 C(13) H(17) 3.267 ? . 2_555 C(13) H(22) 3.009 ? . 3_745 C(14) H(16) 3.044 ? . 2_555 C(15) H(16) 3.084 ? . 2_555 C(16) H(8) 3.226 ? . 2_555 C(17) H(8) 3.045 ? . 2_555 C(18) H(8) 3.199 ? . 2_555 C(18) H(18) 3.512 ? . 2_455 C(18) H(19) 3.574 ? . 4_654 C(18) H(20) 3.466 ? . 4_654 C(19) H(1) 3.536 ? . 2_555 C(19) H(8) 3.515 ? . 2_555 C(20) H(20) 3.284 ? . 3_755 C(21) H(8) 3.547 ? . 2_555 C(21) H(20) 3.363 ? . 3_755 C(22) H(2) 3.029 ? . 1_655 C(23) H(2) 3.143 ? . 1_655 C(23) H(10) 3.298 ? . 3_745 C(23) H(15) 2.936 ? . 4_655 C(23) H(18) 3.580 ? . 3_745 C(24) H(2) 3.082 ? . 1_655 C(24) H(5) 3.502 ? . 4_655 C(24) H(15) 2.990 ? . 4_655 C(24) H(17) 3.453 ? . 3_745 C(24) H(18) 3.482 ? . 3_745 C(25) H(2) 2.883 ? . 1_655 C(25) H(3) 3.088 ? . 1_655 C(25) H(4) 3.052 ? . 2_556 C(25) H(5) 3.475 ? . 4_655 C(25) H(6) 3.381 ? . 4_655 C(26) H(2) 2.719 ? . 1_655 C(26) H(4) 2.945 ? . 2_556 C(26) H(12) 3.472 ? . 3_755 C(27) H(2) 2.798 ? . 1_655 H(1) C(19) 3.536 ? . 2_455 H(1) H(16) 3.529 ? . 2_455 H(2) C(22) 3.029 ? . 1_455 H(2) C(23) 3.143 ? . 1_455 H(2) C(24) 3.082 ? . 1_455 H(2) C(25) 2.883 ? . 1_455 H(2) C(26) 2.719 ? . 1_455 H(2) C(27) 2.798 ? . 1_455 H(2) H(6) 3.573 ? . 3_655 H(2) H(21) 3.413 ? . 1_455 H(2) H(22) 3.167 ? . 1_455 H(2) H(23) 3.282 ? . 1_455 H(3) Cl(2) 3.147 ? . 2_456 H(3) C(13) 3.485 ? . 4_655 H(3) C(25) 3.088 ? . 1_455 H(3) H(6) 3.305 ? . 3_655 H(3) H(9) 3.454 ? . 3_645 H(3) H(12) 2.530 ? . 4_655 H(3) H(21) 2.851 ? . 1_455 H(3) H(22) 3.146 ? . 2_456 H(4) C(12) 3.407 ? . 4_655 H(4) C(13) 3.451 ? . 4_655 H(4) C(25) 3.052 ? . 2_456 H(4) C(26) 2.945 ? . 2_456 H(4) H(6) 3.286 ? . 3_655 H(4) H(9) 3.166 ? . 3_645 H(4) H(11) 2.840 ? . 4_655 H(4) H(12) 2.931 ? . 4_655 H(4) H(21) 2.527 ? . 2_456 H(4) H(22) 2.290 ? . 2_456 H(5) Cl(2) 3.020 ? . 3_645 H(5) C(24) 3.502 ? . 4_654 H(5) C(25) 3.475 ? . 4_654 H(5) H(10) 3.548 ? . 3_645 H(5) H(13) 3.416 ? . 1_455 H(5) H(17) 3.367 ? . 2_455 H(5) H(20) 2.898 ? . 4_654 H(5) H(21) 2.846 ? . 4_654 H(6) N(1) 3.119 ? . 3_645 H(6) N(2) 3.025 ? . 3_645 H(6) C(1) 3.039 ? . 3_645 H(6) C(2) 2.873 ? . 3_645 H(6) C(3) 2.859 ? . 3_645 H(6) C(25) 3.381 ? . 4_654 H(6) H(2) 3.573 ? . 3_645 H(6) H(3) 3.305 ? . 3_645 H(6) H(4) 3.286 ? . 3_645 H(6) H(21) 2.801 ? . 4_654 H(8) Cl(1) 3.149 ? . 3_655 H(8) C(12) 3.514 ? . 2_455 H(8) C(16) 3.226 ? . 2_455 H(8) C(17) 3.045 ? . 2_455 H(8) C(18) 3.199 ? . 2_455 H(8) C(19) 3.515 ? . 2_455 H(8) C(21) 3.547 ? . 2_455 H(8) H(11) 2.810 ? . 2_455 H(8) H(14) 3.382 ? . 2_455 H(9) Cl(1) 3.452 ? . 3_655 H(9) N(1) 2.960 ? . 3_655 H(9) N(2) 2.798 ? . 3_655 H(9) N(4) 3.569 ? . 3_655 H(9) C(1) 3.031 ? . 3_655 H(9) C(2) 2.923 ? . 3_655 H(9) C(3) 2.744 ? . 3_655 H(9) C(12) 3.371 ? . 2_455 H(9) H(3) 3.454 ? . 3_655 H(9) H(4) 3.166 ? . 3_655 H(9) H(11) 2.610 ? . 2_455 H(9) H(12) 3.482 ? . 2_455 H(10) C(23) 3.298 ? . 3_755 H(10) H(5) 3.548 ? . 3_655 H(10) H(13) 2.929 ? . 3_755 H(10) H(19) 2.886 ? . 3_755 H(10) H(20) 3.583 ? . 3_755 H(11) Cl(1) 3.313 ? . 4_654 H(11) C(3) 3.255 ? . 4_654 H(11) C(7) 3.195 ? . 2_555 H(11) C(8) 3.092 ? . 2_555 H(11) H(4) 2.840 ? . 4_654 H(11) H(8) 2.810 ? . 2_555 H(11) H(9) 2.610 ? . 2_555 H(11) H(16) 3.406 ? . 2_555 H(11) H(22) 3.587 ? . 3_745 H(12) Cl(2) 3.028 ? . 3_745 H(12) C(2) 3.007 ? . 4_654 H(12) C(3) 3.218 ? . 4_654 H(12) C(26) 3.472 ? . 3_745 H(12) H(3) 2.530 ? . 4_654 H(12) H(4) 2.931 ? . 4_654 H(12) H(9) 3.482 ? . 2_555 H(12) H(16) 3.554 ? . 2_555 H(12) H(17) 3.165 ? . 2_555 H(12) H(22) 2.636 ? . 3_745 H(13) Cl(2) 2.905 ? . 3_745 H(13) H(5) 3.416 ? . 1_655 H(13) H(10) 2.929 ? . 3_745 H(13) H(23) 3.472 ? . 3_745 H(14) Cl(1) 2.942 ? . 4_654 H(14) H(8) 3.382 ? . 2_555 H(15) Cl(1) 3.494 ? . 4_654 H(15) C(23) 2.936 ? . 4_654 H(15) C(24) 2.990 ? . 4_654 H(15) H(18) 2.950 ? . 2_455 H(15) H(19) 2.618 ? . 4_654 H(15) H(20) 2.724 ? . 4_654 H(16) C(10) 3.025 ? . 2_455 H(16) C(11) 2.882 ? . 2_455 H(16) C(12) 2.883 ? . 2_455 H(16) C(13) 2.981 ? . 2_455 H(16) C(14) 3.044 ? . 2_455 H(16) C(15) 3.084 ? . 2_455 H(16) H(1) 3.529 ? . 2_555 H(16) H(11) 3.406 ? . 2_455 H(16) H(12) 3.554 ? . 2_455 H(16) H(18) 3.181 ? . 2_455 H(17) C(12) 3.599 ? . 2_455 H(17) C(13) 3.267 ? . 2_455 H(17) C(24) 3.453 ? . 3_755 H(17) H(5) 3.367 ? . 2_555 H(17) H(12) 3.165 ? . 2_455 H(17) H(20) 2.634 ? . 3_755 H(18) C(18) 3.512 ? . 2_555 H(18) C(23) 3.580 ? . 3_755 H(18) C(24) 3.482 ? . 3_755 H(18) H(15) 2.950 ? . 2_555 H(18) H(16) 3.181 ? . 2_555 H(18) H(19) 2.985 ? . 3_755 H(18) H(20) 2.794 ? . 3_755 H(19) C(18) 3.574 ? . 4_655 H(19) H(10) 2.886 ? . 3_745 H(19) H(15) 2.618 ? . 4_655 H(19) H(18) 2.985 ? . 3_745 H(19) H(23) 3.551 ? . 3_745 H(20) C(4) 3.426 ? . 4_655 H(20) C(18) 3.466 ? . 4_655 H(20) C(20) 3.284 ? . 3_745 H(20) C(21) 3.363 ? . 3_745 H(20) H(5) 2.898 ? . 4_655 H(20) H(10) 3.583 ? . 3_745 H(20) H(15) 2.724 ? . 4_655 H(20) H(17) 2.634 ? . 3_745 H(20) H(18) 2.794 ? . 3_745 H(21) Cl(2) 3.058 ? . 2_556 H(21) C(2) 3.564 ? . 1_655 H(21) C(3) 3.033 ? . 2_556 H(21) C(4) 3.358 ? . 4_655 H(21) C(5) 3.325 ? . 4_655 H(21) H(2) 3.413 ? . 1_655 H(21) H(3) 2.851 ? . 1_655 H(21) H(4) 2.527 ? . 2_556 H(21) H(5) 2.846 ? . 4_655 H(21) H(6) 2.801 ? . 4_655 H(22) C(2) 3.420 ? . 2_556 H(22) C(3) 3.045 ? . 2_556 H(22) C(12) 3.541 ? . 3_755 H(22) C(13) 3.009 ? . 3_755 H(22) H(2) 3.167 ? . 1_655 H(22) H(3) 3.146 ? . 2_556 H(22) H(4) 2.290 ? . 2_556 H(22) H(11) 3.587 ? . 3_755 H(22) H(12) 2.636 ? . 3_755 H(23) H(2) 3.282 ? . 1_655 H(23) H(13) 3.472 ? . 3_755 H(23) H(19) 3.551 ? . 3_755 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================