# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_Complex1b _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- CIFfiles.txt' _audit_creation_date 2011-01-19 _audit_creation_method 'by CrystalStructure 4.0' _audit_update_record ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Kotohiro Nomura' _publ_contact_author_email ktnomura@tmu.ac.jp _publ_contact_author_fax +81-42-677-2547 _publ_contact_author_phone +81-42-677-2547 _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_category 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address K.Nomura ; FIRST AUTHORS FOOTNOTES ; ; 1-1 Minami Osawa, Hachioji, Tokyo192-0397, Japan ; H.Fukuda '' '' S.Katao '' '' M.Fujiki '' '' 'Hyun Joon Kim' '' '' 'Dong-Hyun Kim' '' '' 'Shu Zhang' '' '' _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku (2010). CrystalStructure. Version 4.0. Rigaku Corporation, Tokyo, Japan. M.C. Burla, R. Caliandro, M. Camalli, B. Carrozzini, G.L. Cascarano, L. De Caro, C. Giacovazzo, G. Polidori, D. Siliqi, R. Spagna (2007) SIR2008 Sheldrick, G.M. (2008), Acta Cryst. A64, 112-122. Rigaku (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #============================================================================== data_Cp-MePh _database_code_depnum_ccdc_archive 'CCDC 817925' #TrackingRef '- CIFfiles.txt' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H27 Cl2 N3 Ti' _chemical_formula_moiety 'C24 H27 Cl2 N3 Ti' _chemical_formula_weight 476.30 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 8.2728(3) _cell_length_b 9.4651(4) _cell_length_c 16.8992(6) _cell_angle_alpha 80.2807(10) _cell_angle_beta 82.6310(11) _cell_angle_gamma 62.5498(10) _cell_volume 1155.48(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9448 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 27.46 _cell_measurement_temperature 123 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.450 _exptl_crystal_size_min 0.120 _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496.00 _exptl_absorpt_coefficient_mu 0.617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.693 _exptl_absorpt_correction_T_max 0.929 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 123 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 11559 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # 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 5250 _reflns_number_gt 4496 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0997 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 5250 _refine_ls_number_parameters 295 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0452P)^2^+0.7158P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.380 _refine_diff_density_min -0.520 _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 0.0033 0.0016 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ti Ti 0.2776 0.4457 ; 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 Ti1 Ti 0.33380(4) -0.13443(4) 0.771315(18) 0.01708(9) Uani 1.0 2 d . . . Cl1 Cl 0.62540(6) -0.18322(6) 0.79403(3) 0.02457(12) Uani 1.0 2 d . . . Cl2 Cl 0.39779(7) -0.30405(6) 0.67574(3) 0.02948(12) Uani 1.0 2 d . . . N1 N 0.2446(2) 0.06495(18) 0.71980(9) 0.0181(3) Uani 1.0 2 d . . . N2 N 0.1296(3) 0.32957(18) 0.75414(9) 0.0207(4) Uani 1.0 2 d . . . N3 N 0.0901(3) 0.30296(18) 0.63220(9) 0.0210(4) Uani 1.0 2 d . . . C1 C 0.3287(3) -0.2709(3) 0.90460(12) 0.0286(5) Uani 1.0 2 d . . . C2 C 0.2280(3) -0.1038(3) 0.90673(11) 0.0269(4) Uani 1.0 2 d . . . C3 C 0.0752(3) -0.0482(3) 0.86152(12) 0.0287(5) Uani 1.0 2 d . . . C4 C 0.0833(3) -0.1802(3) 0.82898(13) 0.0297(5) Uani 1.0 2 d . . . C5 C 0.2390(4) -0.3172(3) 0.85720(12) 0.0309(5) Uani 1.0 2 d . . . C6 C 0.1605(3) 0.2212(2) 0.70329(10) 0.0163(4) Uani 1.0 2 d . . . C7 C 0.0566(3) 0.4940(3) 0.71256(11) 0.0247(4) Uani 1.0 2 d . . . C8 C -0.0066(3) 0.4765(3) 0.63508(12) 0.0272(5) Uani 1.0 2 d . . . C9 C 0.1961(3) 0.2914(2) 0.83288(10) 0.0203(4) Uani 1.0 2 d . . . C10 C 0.3817(3) 0.2392(3) 0.84125(11) 0.0236(4) Uani 1.0 2 d . . . C11 C 0.4419(3) 0.2036(3) 0.91897(13) 0.0314(5) Uani 1.0 2 d . . . C12 C 0.3198(4) 0.2235(3) 0.98529(12) 0.0351(5) Uani 1.0 2 d . . . C13 C 0.1371(4) 0.2809(3) 0.97572(12) 0.0340(5) Uani 1.0 2 d . . . C14 C 0.0697(3) 0.3163(3) 0.89906(11) 0.0259(4) Uani 1.0 2 d . . . C15 C 0.5124(3) 0.2255(3) 0.76875(13) 0.0300(5) Uani 1.0 2 d . . . C16 C -0.1317(3) 0.3817(3) 0.89014(14) 0.0362(5) Uani 1.0 2 d . . . C17 C 0.0999(3) 0.2376(2) 0.56011(10) 0.0193(4) Uani 1.0 2 d . . . C18 C -0.0521(3) 0.2265(3) 0.54106(12) 0.0268(4) Uani 1.0 2 d . . . C19 C -0.0455(4) 0.1783(3) 0.46663(13) 0.0350(5) Uani 1.0 2 d . . . C20 C 0.1064(4) 0.1429(3) 0.41444(12) 0.0367(6) Uani 1.0 2 d . . . C21 C 0.2560(4) 0.1547(3) 0.43475(12) 0.0330(5) Uani 1.0 2 d . . . C22 C 0.2545(3) 0.2044(3) 0.50789(11) 0.0243(4) Uani 1.0 2 d . . . C23 C -0.2166(4) 0.2639(4) 0.59891(16) 0.0436(6) Uani 1.0 2 d . . . C24 C 0.4088(3) 0.2306(3) 0.52916(15) 0.0373(5) Uani 1.0 2 d . . . H1 H 0.4451 -0.3404 0.9267 0.0408 Uiso 1.0 2 calc R . . H2 H 0.2638 -0.0361 0.9290 0.0367 Uiso 1.0 2 calc R . . H3 H -0.0162 0.0580 0.8536 0.0404 Uiso 1.0 2 calc R . . H4 H 0.0066 -0.1738 0.7965 0.0330 Uiso 1.0 2 calc R . . H5 H 0.2832 -0.4228 0.8449 0.0412 Uiso 1.0 2 calc R . . H6 H 0.1521 0.5313 0.7009 0.0296 Uiso 1.0 2 calc R . . H7 H -0.0465 0.5695 0.7445 0.0296 Uiso 1.0 2 calc R . . H8 H -0.1405 0.5157 0.6379 0.0326 Uiso 1.0 2 calc R . . H9 H 0.0289 0.5355 0.5877 0.0326 Uiso 1.0 2 calc R . . H10 H 0.5678 0.1652 0.9264 0.0377 Uiso 1.0 2 calc R . . H11 H 0.3628 0.1973 1.0378 0.0422 Uiso 1.0 2 calc R . . H12 H 0.0547 0.2969 1.0218 0.0408 Uiso 1.0 2 calc R . . H13 H 0.4703 0.3293 0.7349 0.0360 Uiso 1.0 2 calc R . . H14 H 0.5176 0.1445 0.7379 0.0360 Uiso 1.0 2 calc R . . H15 H 0.6341 0.1936 0.7863 0.0360 Uiso 1.0 2 calc R . . H16 H -0.1511 0.3516 0.8408 0.0434 Uiso 1.0 2 calc R . . H17 H -0.1898 0.4989 0.8873 0.0434 Uiso 1.0 2 calc R . . H18 H -0.1854 0.3372 0.9365 0.0434 Uiso 1.0 2 calc R . . H19 H -0.1473 0.1698 0.4517 0.0421 Uiso 1.0 2 calc R . . H20 H 0.1084 0.1101 0.3641 0.0441 Uiso 1.0 2 calc R . . H21 H 0.3606 0.1287 0.3985 0.0396 Uiso 1.0 2 calc R . . H22 H -0.2818 0.2052 0.5889 0.0524 Uiso 1.0 2 calc R . . H23 H -0.2977 0.3795 0.5914 0.0524 Uiso 1.0 2 calc R . . H24 H -0.1774 0.2315 0.6542 0.0524 Uiso 1.0 2 calc R . . H25 H 0.3663 0.3451 0.5317 0.0448 Uiso 1.0 2 calc R . . H26 H 0.5093 0.1939 0.4881 0.0448 Uiso 1.0 2 calc R . . H27 H 0.4514 0.1699 0.5816 0.0448 Uiso 1.0 2 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti1 0.01971(17) 0.01685(17) 0.01339(16) -0.00739(13) -0.00197(11) -0.00032(11) Cl1 0.0186(3) 0.0287(3) 0.0219(3) -0.00663(19) -0.00467(16) -0.00111(17) Cl2 0.0422(3) 0.0295(3) 0.0210(3) -0.0186(3) 0.00117(19) -0.00914(18) N1 0.0205(8) 0.0195(8) 0.0138(7) -0.0087(7) -0.0039(6) 0.0003(6) N2 0.0286(9) 0.0144(7) 0.0147(8) -0.0061(7) -0.0049(6) 0.0009(6) N3 0.0284(9) 0.0157(8) 0.0152(8) -0.0066(7) -0.0072(6) 0.0018(6) C1 0.0340(11) 0.0302(11) 0.0167(9) -0.0134(10) -0.0003(8) 0.0053(8) C2 0.0362(11) 0.0308(11) 0.0163(9) -0.0181(10) 0.0048(8) -0.0047(8) C3 0.0266(10) 0.0272(11) 0.0262(10) -0.0094(9) 0.0062(8) -0.0017(8) C4 0.0302(11) 0.0448(13) 0.0236(10) -0.0270(10) 0.0018(8) -0.0006(9) C5 0.0455(13) 0.0281(11) 0.0244(10) -0.0236(10) 0.0089(9) -0.0038(8) C6 0.0148(8) 0.0202(9) 0.0134(8) -0.0081(7) -0.0016(6) 0.0003(7) C7 0.0336(11) 0.0160(9) 0.0197(9) -0.0073(8) -0.0049(8) 0.0010(7) C8 0.0369(11) 0.0165(9) 0.0223(10) -0.0069(9) -0.0084(8) 0.0019(7) C9 0.0296(10) 0.0172(9) 0.0144(9) -0.0105(8) -0.0033(7) -0.0013(7) C10 0.0290(10) 0.0210(9) 0.0205(9) -0.0111(8) -0.0038(8) -0.0003(7) C11 0.0389(12) 0.0314(11) 0.0275(11) -0.0170(10) -0.0129(9) -0.0010(9) C12 0.0556(15) 0.0327(12) 0.0181(10) -0.0186(11) -0.0127(10) -0.0014(8) C13 0.0526(14) 0.0288(11) 0.0163(10) -0.0159(11) 0.0050(9) -0.0040(8) C14 0.0341(11) 0.0200(10) 0.0201(10) -0.0103(9) 0.0015(8) -0.0009(7) C15 0.0270(10) 0.0322(11) 0.0299(11) -0.0138(9) -0.0013(8) 0.0001(9) C16 0.0317(12) 0.0321(12) 0.0344(12) -0.0089(10) 0.0066(9) -0.0007(9) C17 0.0258(9) 0.0181(9) 0.0126(8) -0.0090(8) -0.0061(7) 0.0029(7) C18 0.0320(11) 0.0262(10) 0.0246(10) -0.0161(9) -0.0060(8) 0.0029(8) C19 0.0519(14) 0.0333(12) 0.0307(12) -0.0265(11) -0.0195(10) 0.0039(9) C20 0.0692(17) 0.0248(11) 0.0177(10) -0.0215(11) -0.0103(10) 0.0008(8) C21 0.0457(13) 0.0202(10) 0.0208(10) -0.0071(10) 0.0045(9) 0.0005(8) C22 0.0254(10) 0.0190(9) 0.0213(10) -0.0054(8) -0.0032(8) 0.0037(7) C23 0.0362(13) 0.0523(15) 0.0510(15) -0.0284(12) 0.0039(11) -0.0076(12) C24 0.0254(11) 0.0394(13) 0.0413(13) -0.0120(10) -0.0008(9) 0.0012(10) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _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 'CrystalStructure 4.0' #============================================================================== # 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 Ti1 Cl1 2.3088(7) yes . . Ti1 Cl2 2.3106(7) yes . . Ti1 N1 1.7860(15) yes . . Ti1 C1 2.406(2) yes . . Ti1 C2 2.3586(19) yes . . Ti1 C3 2.354(2) yes . . Ti1 C4 2.367(3) yes . . Ti1 C5 2.414(3) yes . . N1 C6 1.308(3) yes . . N2 C6 1.362(3) yes . . N2 C7 1.468(3) yes . . N2 C9 1.430(3) yes . . N3 C6 1.353(3) yes . . N3 C8 1.465(3) yes . . N3 C17 1.434(3) yes . . C1 C2 1.412(3) yes . . C1 C5 1.398(4) yes . . C2 C3 1.399(4) yes . . C3 C4 1.419(4) yes . . C4 C5 1.406(3) yes . . C7 C8 1.531(4) yes . . C9 C10 1.398(3) yes . . C9 C14 1.400(3) yes . . C10 C11 1.397(3) yes . . C10 C15 1.507(3) yes . . C11 C12 1.385(3) yes . . C12 C13 1.372(4) yes . . C13 C14 1.403(3) yes . . C14 C16 1.505(4) yes . . C17 C18 1.391(4) yes . . C17 C22 1.395(3) yes . . C18 C19 1.395(4) yes . . C18 C23 1.504(4) yes . . C19 C20 1.377(4) yes . . C20 C21 1.382(5) yes . . C21 C22 1.391(4) yes . . C22 C24 1.504(4) yes . . C1 H1 0.962 no . . C2 H2 0.962 no . . C3 H3 0.938 no . . C4 H4 0.866 no . . C5 H5 0.943 no . . C7 H6 0.990 no . . C7 H7 0.990 no . . C8 H8 0.990 no . . C8 H9 0.990 no . . C11 H10 0.950 no . . C12 H11 0.950 no . . C13 H12 0.950 no . . C15 H13 0.980 no . . C15 H14 0.980 no . . C15 H15 0.980 no . . C16 H16 0.980 no . . C16 H17 0.980 no . . C16 H18 0.980 no . . C19 H19 0.950 no . . C20 H20 0.950 no . . C21 H21 0.950 no . . C23 H22 0.980 no . . C23 H23 0.980 no . . C23 H24 0.980 no . . C24 H25 0.980 no . . C24 H26 0.980 no . . C24 H27 0.980 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 Cl1 Ti1 Cl2 100.27(3) yes . . . Cl1 Ti1 N1 101.84(7) yes . . . Cl1 Ti1 C1 86.21(7) yes . . . Cl1 Ti1 C2 93.72(7) yes . . . Cl1 Ti1 C3 127.25(7) yes . . . Cl1 Ti1 C4 143.13(6) yes . . . Cl1 Ti1 C5 112.22(6) yes . . . Cl2 Ti1 N1 106.80(6) yes . . . Cl2 Ti1 C1 110.72(7) yes . . . Cl2 Ti1 C2 141.55(7) yes . . . Cl2 Ti1 C3 126.19(8) yes . . . Cl2 Ti1 C4 92.07(7) yes . . . Cl2 Ti1 C5 84.69(6) yes . . . N1 Ti1 C1 139.47(7) yes . . . N1 Ti1 C2 105.02(7) yes . . . N1 Ti1 C3 88.45(7) yes . . . N1 Ti1 C4 107.62(8) yes . . . N1 Ti1 C5 141.56(8) yes . . . C1 Ti1 C2 34.46(7) yes . . . C1 Ti1 C3 57.06(7) yes . . . C1 Ti1 C4 56.96(9) yes . . . C1 Ti1 C5 33.73(10) yes . . . C2 Ti1 C3 34.54(8) yes . . . C2 Ti1 C4 57.74(10) yes . . . C2 Ti1 C5 56.89(9) yes . . . C3 Ti1 C4 34.99(10) yes . . . C3 Ti1 C5 57.02(8) yes . . . C4 Ti1 C5 34.20(7) yes . . . Ti1 N1 C6 163.23(14) yes . . . C6 N2 C7 111.70(15) yes . . . C6 N2 C9 125.44(14) yes . . . C7 N2 C9 121.42(18) yes . . . C6 N3 C8 112.08(17) yes . . . C6 N3 C17 127.34(15) yes . . . C8 N3 C17 120.57(14) yes . . . Ti1 C1 C2 70.95(11) yes . . . Ti1 C1 C5 73.45(13) yes . . . C2 C1 C5 108.03(19) yes . . . Ti1 C2 C1 74.60(12) yes . . . Ti1 C2 C3 72.55(12) yes . . . C1 C2 C3 108.0(3) yes . . . Ti1 C3 C2 72.92(12) yes . . . Ti1 C3 C4 73.00(13) yes . . . C2 C3 C4 108.11(18) yes . . . Ti1 C4 C3 72.01(15) yes . . . Ti1 C4 C5 74.73(16) yes . . . C3 C4 C5 107.3(3) yes . . . Ti1 C5 C1 72.82(15) yes . . . Ti1 C5 C4 71.08(15) yes . . . C1 C5 C4 108.5(3) yes . . . N1 C6 N2 126.13(16) yes . . . N1 C6 N3 125.64(19) yes . . . N2 C6 N3 108.23(15) yes . . . N2 C7 C8 102.13(18) yes . . . N3 C8 C7 102.52(15) yes . . . N2 C9 C10 119.42(16) yes . . . N2 C9 C14 118.23(18) yes . . . C10 C9 C14 122.25(18) yes . . . C9 C10 C11 117.95(18) yes . . . C9 C10 C15 121.15(18) yes . . . C11 C10 C15 120.9(2) yes . . . C10 C11 C12 120.6(3) yes . . . C11 C12 C13 120.5(2) yes . . . C12 C13 C14 121.2(2) yes . . . C9 C14 C13 117.4(2) yes . . . C9 C14 C16 122.49(19) yes . . . C13 C14 C16 120.10(19) yes . . . N3 C17 C18 118.71(17) yes . . . N3 C17 C22 118.2(2) yes . . . C18 C17 C22 122.72(19) yes . . . C17 C18 C19 117.4(2) yes . . . C17 C18 C23 121.1(3) yes . . . C19 C18 C23 121.5(3) yes . . . C18 C19 C20 121.0(3) yes . . . C19 C20 C21 120.6(3) yes . . . C20 C21 C22 120.4(2) yes . . . C17 C22 C21 117.9(3) yes . . . C17 C22 C24 120.3(2) yes . . . C21 C22 C24 121.8(2) yes . . . Ti1 C1 H1 116.543 no . . . C2 C1 H1 126.795 no . . . C5 C1 H1 124.882 no . . . Ti1 C2 H2 112.787 no . . . C1 C2 H2 126.919 no . . . C3 C2 H2 124.661 no . . . Ti1 C3 H3 119.491 no . . . C2 C3 H3 126.076 no . . . C4 C3 H3 125.816 no . . . Ti1 C4 H4 117.243 no . . . C3 C4 H4 124.750 no . . . C5 C4 H4 127.878 no . . . Ti1 C5 H5 119.301 no . . . C1 C5 H5 123.837 no . . . C4 C5 H5 127.554 no . . . N2 C7 H6 111.340 no . . . N2 C7 H7 111.340 no . . . C8 C7 H6 111.349 no . . . C8 C7 H7 111.343 no . . . H6 C7 H7 109.217 no . . . N3 C8 H8 111.259 no . . . N3 C8 H9 111.267 no . . . C7 C8 H8 111.255 no . . . C7 C8 H9 111.263 no . . . H8 C8 H9 109.176 no . . . C10 C11 H10 119.691 no . . . C12 C11 H10 119.700 no . . . C11 C12 H11 119.727 no . . . C13 C12 H11 119.732 no . . . C12 C13 H12 119.424 no . . . C14 C13 H12 119.422 no . . . C10 C15 H13 109.465 no . . . C10 C15 H14 109.473 no . . . C10 C15 H15 109.466 no . . . H13 C15 H14 109.483 no . . . H13 C15 H15 109.469 no . . . H14 C15 H15 109.471 no . . . C14 C16 H16 109.468 no . . . C14 C16 H17 109.475 no . . . C14 C16 H18 109.478 no . . . H16 C16 H17 109.466 no . . . H16 C16 H18 109.464 no . . . H17 C16 H18 109.478 no . . . C18 C19 H19 119.509 no . . . C20 C19 H19 119.512 no . . . C19 C20 H20 119.724 no . . . C21 C20 H20 119.722 no . . . C20 C21 H21 119.782 no . . . C22 C21 H21 119.770 no . . . C18 C23 H22 109.480 no . . . C18 C23 H23 109.470 no . . . C18 C23 H24 109.468 no . . . H22 C23 H23 109.474 no . . . H22 C23 H24 109.469 no . . . H23 C23 H24 109.466 no . . . C22 C24 H25 109.474 no . . . C22 C24 H26 109.464 no . . . C22 C24 H27 109.477 no . . . H25 C24 H26 109.469 no . . . H25 C24 H27 109.470 no . . . H26 C24 H27 109.472 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 Cl1 Ti1 C1 C2 102.21(11) no . . . . Cl1 Ti1 C1 C5 -141.42(7) no . . . . Cl1 Ti1 C2 C1 -77.77(10) no . . . . Cl1 Ti1 C2 C3 167.26(9) no . . . . Cl1 Ti1 C3 C2 -16.05(14) no . . . . Cl1 Ti1 C3 C4 -131.77(7) no . . . . Cl1 Ti1 C4 C3 81.64(11) no . . . . Cl1 Ti1 C4 C5 -32.79(17) no . . . . Cl1 Ti1 C5 C1 42.23(9) no . . . . Cl1 Ti1 C5 C4 159.45(7) no . . . . Cl2 Ti1 C1 C2 -158.24(8) no . . . . Cl2 Ti1 C1 C5 -41.86(9) no . . . . Cl2 Ti1 C2 C1 33.90(16) no . . . . Cl2 Ti1 C2 C3 -81.07(10) no . . . . Cl2 Ti1 C3 C2 130.44(9) no . . . . Cl2 Ti1 C3 C4 14.73(10) no . . . . Cl2 Ti1 C4 C3 -168.15(7) no . . . . Cl2 Ti1 C4 C5 77.42(10) no . . . . Cl2 Ti1 C5 C1 141.18(8) no . . . . Cl2 Ti1 C5 C4 -101.60(9) no . . . . N1 Ti1 C1 C2 -1.6(2) no . . . . N1 Ti1 C1 C5 114.76(14) no . . . . N1 Ti1 C2 C1 178.91(11) no . . . . N1 Ti1 C2 C3 63.94(13) no . . . . N1 Ti1 C3 C2 -119.78(12) no . . . . N1 Ti1 C3 C4 124.50(10) no . . . . N1 Ti1 C4 C3 -59.80(11) no . . . . N1 Ti1 C4 C5 -174.23(10) no . . . . N1 Ti1 C5 C1 -108.35(14) no . . . . N1 Ti1 C5 C4 8.87(19) no . . . . C1 Ti1 C2 C1 0.00(12) no . . . . C1 Ti1 C2 C3 -115.0(2) no . . . . C2 Ti1 C1 C2 -0.00(12) no . . . . C2 Ti1 C1 C5 116.37(18) no . . . . C1 Ti1 C3 C2 37.67(10) no . . . . C1 Ti1 C3 C4 -78.04(11) no . . . . C3 Ti1 C1 C2 -37.76(11) no . . . . C3 Ti1 C1 C5 78.61(12) no . . . . C1 Ti1 C4 C3 78.34(11) no . . . . C1 Ti1 C4 C5 -36.09(9) no . . . . C4 Ti1 C1 C2 -79.78(11) no . . . . C4 Ti1 C1 C5 36.60(9) no . . . . C1 Ti1 C5 C1 0.00(8) no . . . . C1 Ti1 C5 C4 117.22(15) no . . . . C5 Ti1 C1 C2 -116.37(16) no . . . . C5 Ti1 C1 C5 0.00(9) no . . . . C2 Ti1 C3 C2 0.00(11) no . . . . C2 Ti1 C3 C4 -115.72(17) no . . . . C3 Ti1 C2 C1 115.0(2) no . . . . C3 Ti1 C2 C3 0.00(12) no . . . . C2 Ti1 C4 C3 37.16(8) no . . . . C2 Ti1 C4 C5 -77.27(11) no . . . . C4 Ti1 C2 C1 77.31(12) no . . . . C4 Ti1 C2 C3 -37.66(9) no . . . . C2 Ti1 C5 C1 -37.24(8) no . . . . C2 Ti1 C5 C4 79.98(10) no . . . . C5 Ti1 C2 C1 36.43(10) no . . . . C5 Ti1 C2 C3 -78.54(12) no . . . . C3 Ti1 C4 C3 0.00(8) no . . . . C3 Ti1 C4 C5 -114.43(16) no . . . . C4 Ti1 C3 C2 115.72(15) no . . . . C4 Ti1 C3 C4 0.00(9) no . . . . C3 Ti1 C5 C1 -78.72(11) no . . . . C3 Ti1 C5 C4 38.50(9) no . . . . C5 Ti1 C3 C2 78.13(11) no . . . . C5 Ti1 C3 C4 -37.59(9) no . . . . C4 Ti1 C5 C1 -117.22(17) no . . . . C4 Ti1 C5 C4 0.00(12) no . . . . C5 Ti1 C4 C3 114.43(18) no . . . . C5 Ti1 C4 C5 0.00(11) no . . . . C6 N2 C7 C8 16.5(2) no . . . . C7 N2 C6 N1 171.36(18) no . . . . C7 N2 C6 N3 -8.3(3) no . . . . C6 N2 C9 C10 72.0(3) no . . . . C6 N2 C9 C14 -111.4(2) no . . . . C9 N2 C6 N1 5.0(4) no . . . . C9 N2 C6 N3 -174.62(18) no . . . . C7 N2 C9 C10 -93.1(2) no . . . . C7 N2 C9 C14 83.4(3) no . . . . C9 N2 C7 C8 -176.54(15) no . . . . C6 N3 C8 C7 14.2(3) no . . . . C8 N3 C6 N1 175.95(18) no . . . . C8 N3 C6 N2 -4.4(3) no . . . . C6 N3 C17 C18 101.7(2) no . . . . C6 N3 C17 C22 -85.2(3) no . . . . C17 N3 C6 N1 -3.2(4) no . . . . C17 N3 C6 N2 176.43(18) no . . . . C8 N3 C17 C18 -77.4(3) no . . . . C8 N3 C17 C22 95.7(2) no . . . . C17 N3 C8 C7 -166.56(17) no . . . . Ti1 C1 C2 Ti1 0.0 no . . . . Ti1 C1 C2 C3 65.39(12) no . . . . Ti1 C1 C5 Ti1 0.0 no . . . . Ti1 C1 C5 C4 -62.52(13) no . . . . C2 C1 C5 Ti1 62.94(16) no . . . . C2 C1 C5 C4 0.4(3) no . . . . C5 C1 C2 Ti1 -64.57(16) no . . . . C5 C1 C2 C3 0.8(3) no . . . . Ti1 C2 C3 Ti1 0.000(10) no . . . . Ti1 C2 C3 C4 65.02(12) no . . . . C1 C2 C3 Ti1 -66.75(15) no . . . . C1 C2 C3 C4 -1.7(3) no . . . . Ti1 C3 C4 Ti1 0.0 no . . . . Ti1 C3 C4 C5 66.95(13) no . . . . C2 C3 C4 Ti1 -64.97(16) no . . . . C2 C3 C4 C5 2.0(3) no . . . . Ti1 C4 C5 Ti1 0.0 no . . . . Ti1 C4 C5 C1 63.64(14) no . . . . C3 C4 C5 Ti1 -65.12(17) no . . . . C3 C4 C5 C1 -1.5(3) no . . . . N2 C7 C8 N3 -17.35(19) no . . . . N2 C9 C10 C11 179.76(17) no . . . . N2 C9 C10 C15 1.1(3) no . . . . N2 C9 C14 C13 -178.88(17) no . . . . N2 C9 C14 C16 -0.2(3) no . . . . C10 C9 C14 C13 -2.4(3) no . . . . C10 C9 C14 C16 176.27(18) no . . . . C14 C9 C10 C11 3.3(3) no . . . . C14 C9 C10 C15 -175.29(18) no . . . . C9 C10 C11 C12 -1.6(4) no . . . . C15 C10 C11 C12 177.0(2) no . . . . C10 C11 C12 C13 -0.9(4) no . . . . C11 C12 C13 C14 1.9(4) no . . . . C12 C13 C14 C9 -0.2(4) no . . . . C12 C13 C14 C16 -179.0(2) no . . . . N3 C17 C18 C19 173.45(14) no . . . . N3 C17 C18 C23 -7.0(3) no . . . . N3 C17 C22 C21 -174.34(13) no . . . . N3 C17 C22 C24 2.5(3) no . . . . C18 C17 C22 C21 -1.5(3) no . . . . C18 C17 C22 C24 175.32(15) no . . . . C22 C17 C18 C19 0.7(3) no . . . . C22 C17 C18 C23 -179.76(15) no . . . . C17 C18 C19 C20 0.2(3) no . . . . C23 C18 C19 C20 -179.39(18) no . . . . C18 C19 C20 C21 -0.1(3) no . . . . C19 C20 C21 C22 -0.8(3) no . . . . C20 C21 C22 C17 1.5(3) no . . . . C20 C21 C22 C24 -175.25(16) no . . . . 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 Cl1 C15 3.497(3) no . . N1 C9 2.966(3) no . . N1 C10 3.418(4) no . . N1 C15 3.449(4) no . . N1 C17 2.987(3) no . . N2 C15 2.881(3) no . . N2 C16 2.885(3) no . . N2 C17 3.597(3) no . . N3 C9 3.582(3) no . . N3 C23 2.862(4) no . . N3 C24 2.831(3) no . . C2 C14 3.552(3) no . . C3 C14 3.591(4) no . . C6 C10 3.214(3) no . . C6 C14 3.473(3) no . . C6 C15 3.263(4) no . . C6 C18 3.424(3) no . . C6 C22 3.307(3) no . . C6 C24 3.379(3) no . . C7 C10 3.395(3) no . . C7 C14 3.302(3) no . . C7 C15 3.584(3) no . . C7 C16 3.437(3) no . . C8 C18 3.242(4) no . . C8 C22 3.387(3) no . . C8 C23 3.369(5) no . . C8 C24 3.590(3) no . . C9 C12 2.758(3) no . . C10 C13 2.793(3) no . . C11 C14 2.801(4) no . . C17 C20 2.744(3) no . . C18 C21 2.798(3) no . . C19 C22 2.788(4) no . . C7 C20 3.495(3) no . 2_566 C8 C20 3.282(3) no . 2_566 C8 C21 3.229(3) no . 2_566 C8 C22 3.501(3) no . 2_566 C15 C23 3.485(4) no . 1_655 C18 C19 3.555(4) no . 2_556 C19 C18 3.555(4) no . 2_556 C19 C19 3.134(4) no . 2_556 C19 C20 3.554(4) no . 2_556 C20 C7 3.495(3) no . 2_566 C20 C8 3.282(3) no . 2_566 C20 C19 3.554(4) no . 2_556 C20 C23 3.566(4) no . 2_556 C21 C8 3.229(3) no . 2_566 C21 C24 3.424(3) no . 2_656 C22 C8 3.501(3) no . 2_566 C23 C15 3.485(4) no . 1_455 C23 C20 3.566(4) no . 2_556 C24 C21 3.424(3) no . 2_656 Ti1 H14 3.5462 no . . Cl1 H1 3.0863 no . . Cl1 H2 3.4016 no . . Cl1 H14 2.8263 no . . Cl1 H15 3.5811 no . . Cl2 H4 3.4110 no . . Cl2 H5 3.0875 no . . N1 H2 3.5071 no . . N1 H3 2.9326 no . . N1 H14 2.7537 no . . N1 H24 3.3512 no . . N1 H27 3.0214 no . . N2 H3 3.4306 no . . N2 H8 2.8776 no . . N2 H9 3.1084 no . . N2 H13 2.7945 no . . N2 H14 2.8634 no . . N2 H16 2.5228 no . . N2 H17 3.2259 no . . N3 H6 2.8821 no . . N3 H7 3.1117 no . . N3 H23 3.0896 no . . N3 H24 2.5642 no . . N3 H25 2.8077 no . . N3 H27 2.7371 no . . C1 H3 3.1797 no . . C1 H4 3.1159 no . . C2 H4 3.1106 no . . C2 H5 3.1757 no . . C3 H1 3.2033 no . . C3 H5 3.1932 no . . C3 H16 3.3375 no . . C4 H1 3.1981 no . . C4 H2 3.2021 no . . C5 H2 3.2017 no . . C5 H3 3.1811 no . . C6 H3 3.2831 no . . C6 H6 2.8973 no . . C6 H7 3.0906 no . . C6 H8 2.9079 no . . C6 H9 3.0744 no . . C6 H13 3.2950 no . . C6 H14 2.8140 no . . C6 H16 3.1725 no . . C6 H24 2.9713 no . . C6 H25 3.4801 no . . C6 H27 2.8722 no . . C7 H13 3.0821 no . . C7 H16 3.1080 no . . C7 H17 3.3611 no . . C8 H23 3.1482 no . . C8 H24 3.1829 no . . C8 H25 3.1514 no . . C9 H2 3.0811 no . . C9 H3 3.3535 no . . C9 H6 2.8277 no . . C9 H7 2.7854 no . . C9 H10 3.2569 no . . C9 H12 3.2569 no . . C9 H13 2.7577 no . . C9 H14 2.7990 no . . C9 H15 3.3212 no . . C9 H16 2.6478 no . . C9 H17 2.9952 no . . C9 H18 3.2849 no . . C10 H2 3.2573 no . . C10 H6 3.3123 no . . C10 H11 3.2708 no . . C11 H2 3.1990 no . . C11 H12 3.2470 no . . C11 H13 3.1573 no . . C11 H14 3.1357 no . . C11 H15 2.5652 no . . C12 H2 3.0184 no . . C13 H2 2.9005 no . . C13 H10 3.2469 no . . C13 H16 3.2777 no . . C13 H17 2.9414 no . . C13 H18 2.6198 no . . C14 H2 2.9429 no . . C14 H3 3.0744 no . . C14 H7 3.1458 no . . C14 H11 3.2708 no . . C15 H6 3.2211 no . . C15 H10 2.6822 no . . C15 H27 3.4283 no . . C16 H3 2.9111 no . . C16 H7 2.9908 no . . C16 H12 2.6666 no . . C17 H8 2.8783 no . . C17 H9 2.7126 no . . C17 H19 3.2425 no . . C17 H21 3.2495 no . . C17 H22 3.2785 no . . C17 H23 2.9363 no . . C17 H24 2.6359 no . . C17 H25 2.7847 no . . C17 H26 3.3081 no . . C17 H27 2.7335 no . . C18 H8 3.1730 no . . C18 H9 3.5133 no . . C18 H20 3.2663 no . . C19 H21 3.2505 no . . C19 H22 2.6146 no . . C19 H23 2.9979 no . . C19 H24 3.2608 no . . C21 H19 3.2496 no . . C21 H25 3.1081 no . . C21 H26 2.5798 no . . C21 H27 3.1863 no . . C22 H9 3.2418 no . . C22 H20 3.2624 no . . C23 H8 2.9204 no . . C23 H19 2.6871 no . . C24 H9 3.3147 no . . C24 H21 2.6949 no . . H1 H2 2.5660 no . . H1 H5 2.4736 no . . H2 H3 2.5010 no . . H2 H11 3.5164 no . . H2 H12 3.3667 no . . H3 H4 2.4628 no . . H3 H16 2.4531 no . . H3 H18 2.8718 no . . H4 H5 2.5134 no . . H6 H8 2.8388 no . . H6 H9 2.2680 no . . H6 H13 2.5081 no . . H6 H14 3.5274 no . . H6 H25 3.4567 no . . H7 H8 2.2674 no . . H7 H9 2.6830 no . . H7 H16 2.7926 no . . H7 H17 2.6699 no . . H8 H16 3.5237 no . . H8 H23 2.4742 no . . H8 H24 2.8090 no . . H9 H25 2.6823 no . . H10 H11 2.3267 no . . H10 H13 3.3696 no . . H10 H14 3.3147 no . . H10 H15 2.3590 no . . H11 H12 2.3098 no . . H12 H16 3.5383 no . . H12 H17 3.0098 no . . H12 H18 2.4537 no . . H13 H27 3.2648 no . . H14 H27 2.7152 no . . H16 H24 3.5911 no . . H19 H20 2.3161 no . . H19 H22 2.4452 no . . H19 H23 3.0998 no . . H19 H24 3.5254 no . . H20 H21 2.3251 no . . H21 H25 3.3067 no . . H21 H26 2.3830 no . . H21 H27 3.3996 no . . Ti1 H21 3.5842 no . 2_656 Cl1 H4 3.2011 no . 1_655 Cl1 H7 2.7868 no . 1_645 Cl1 H11 2.8339 no . 2_657 Cl1 H17 2.9412 no . 1_645 Cl1 H20 3.4259 no . 2_656 Cl1 H21 3.2032 no . 2_656 Cl2 H6 3.0357 no . 1_545 Cl2 H8 3.4122 no . 1_645 Cl2 H13 3.2350 no . 1_545 Cl2 H19 2.8884 no . 2_556 Cl2 H21 3.1683 no . 2_656 Cl2 H23 3.3038 no . 1_645 Cl2 H26 2.9259 no . 2_656 N1 H21 3.4742 no . 2_656 C1 H10 3.5030 no . 2_657 C1 H11 3.2324 no . 2_657 C1 H12 3.3572 no . 2_557 C1 H17 3.5518 no . 1_645 C1 H18 2.8827 no . 2_557 C2 H10 3.3024 no . 2_657 C2 H11 3.3001 no . 2_657 C2 H12 3.5690 no . 2_557 C2 H18 3.2443 no . 2_557 C3 H12 3.2870 no . 2_557 C3 H15 3.5602 no . 1_455 C4 H6 3.5646 no . 1_545 C4 H7 3.5608 no . 1_545 C4 H12 2.8918 no . 2_557 C5 H6 3.5017 no . 1_545 C5 H12 2.9239 no . 2_557 C5 H18 3.4416 no . 2_557 C7 H4 3.4959 no . 1_565 C7 H5 3.4875 no . 1_565 C7 H20 3.4171 no . 2_566 C8 H21 3.5330 no . 2_566 C9 H5 3.1467 no . 1_565 C10 H5 2.9246 no . 1_565 C11 H1 3.4973 no . 2_657 C11 H2 3.4224 no . 2_657 C11 H5 3.2323 no . 1_565 C11 H11 3.3550 no . 2_657 C12 H1 3.2398 no . 2_657 C12 H2 3.4485 no . 2_657 C12 H10 3.4609 no . 2_657 C12 H17 3.3764 no . 2_567 C13 H12 3.5613 no . 2_567 C13 H17 3.5516 no . 2_567 C14 H5 3.5918 no . 1_565 C15 H5 3.3671 no . 1_565 C15 H22 3.2781 no . 1_655 C15 H24 3.0271 no . 1_655 C16 H1 3.3256 no . 1_465 C17 H9 2.9572 no . 2_566 C18 H9 2.9121 no . 2_566 C18 H19 3.3167 no . 2_556 C18 H20 3.5200 no . 2_556 C19 H6 3.4828 no . 2_566 C19 H9 2.7692 no . 2_566 C19 H19 3.0807 no . 2_556 C19 H22 3.5815 no . 2_556 C19 H26 3.5909 no . 1_455 C20 H6 3.2932 no . 2_566 C20 H7 3.3910 no . 2_566 C20 H8 3.3340 no . 2_566 C20 H9 2.7114 no . 2_566 C20 H19 3.3175 no . 2_556 C20 H22 2.9328 no . 2_556 C20 H27 3.4873 no . 2_656 C21 H8 2.9008 no . 2_566 C21 H9 2.7890 no . 2_566 C21 H22 3.4027 no . 2_556 C21 H26 3.1062 no . 2_656 C21 H27 2.9379 no . 2_656 C22 H8 3.1734 no . 2_566 C22 H9 2.9104 no . 2_566 C22 H21 3.5965 no . 2_656 C22 H26 3.3455 no . 2_656 C23 H13 3.1382 no . 1_455 C23 H14 3.4208 no . 1_455 C23 H15 3.3230 no . 1_455 C23 H20 3.1940 no . 2_556 C23 H25 3.4720 no . 1_455 C23 H26 3.4618 no . 1_455 C23 H27 3.3124 no . 1_455 C24 H19 3.5504 no . 1_655 C24 H21 3.1482 no . 2_656 C24 H22 2.7642 no . 1_655 H1 C11 3.4973 no . 2_657 H1 C12 3.2398 no . 2_657 H1 C16 3.3256 no . 1_645 H1 H1 3.4075 no . 2_647 H1 H10 3.1744 no . 2_657 H1 H11 2.6862 no . 2_657 H1 H17 2.7330 no . 1_645 H1 H18 3.1688 no . 1_645 H1 H18 2.9412 no . 2_557 H2 C11 3.4224 no . 2_657 H2 C12 3.4485 no . 2_657 H2 H10 2.7749 no . 2_657 H2 H11 2.8272 no . 2_657 H2 H18 3.5847 no . 2_557 H3 H10 3.2405 no . 1_455 H3 H15 2.8697 no . 1_455 H4 Cl1 3.2011 no . 1_455 H4 C7 3.4959 no . 1_545 H4 H6 3.1264 no . 1_545 H4 H7 2.9447 no . 1_545 H4 H12 3.1594 no . 2_557 H4 H15 3.4165 no . 1_455 H4 H20 2.8651 no . 2_556 H5 C7 3.4875 no . 1_545 H5 C9 3.1467 no . 1_545 H5 C10 2.9246 no . 1_545 H5 C11 3.2323 no . 1_545 H5 C14 3.5918 no . 1_545 H5 C15 3.3671 no . 1_545 H5 H6 2.9581 no . 1_545 H5 H7 3.4257 no . 1_545 H5 H12 3.2449 no . 2_557 H5 H13 2.9569 no . 1_545 H6 Cl2 3.0357 no . 1_565 H6 C4 3.5646 no . 1_565 H6 C5 3.5017 no . 1_565 H6 C19 3.4828 no . 2_566 H6 C20 3.2932 no . 2_566 H6 H4 3.1264 no . 1_565 H6 H5 2.9581 no . 1_565 H6 H19 3.4812 no . 2_566 H6 H20 3.1587 no . 2_566 H7 Cl1 2.7868 no . 1_465 H7 C4 3.5608 no . 1_565 H7 C20 3.3910 no . 2_566 H7 H4 2.9447 no . 1_565 H7 H5 3.4257 no . 1_565 H7 H20 3.1232 no . 2_566 H8 Cl2 3.4122 no . 1_465 H8 C20 3.3340 no . 2_566 H8 C21 2.9008 no . 2_566 H8 C22 3.1734 no . 2_566 H8 H21 2.9938 no . 2_566 H8 H25 3.3574 no . 2_566 H9 C17 2.9572 no . 2_566 H9 C18 2.9121 no . 2_566 H9 C19 2.7692 no . 2_566 H9 C20 2.7114 no . 2_566 H9 C21 2.7890 no . 2_566 H9 C22 2.9104 no . 2_566 H9 H9 3.2845 no . 2_566 H9 H19 3.3023 no . 2_566 H9 H20 3.2219 no . 2_566 H9 H21 3.3398 no . 2_566 H10 C1 3.5030 no . 2_657 H10 C2 3.3024 no . 2_657 H10 C12 3.4609 no . 2_657 H10 H1 3.1744 no . 2_657 H10 H2 2.7749 no . 2_657 H10 H3 3.2405 no . 1_655 H10 H11 3.1692 no . 2_657 H10 H16 3.5595 no . 1_655 H10 H18 3.1772 no . 1_655 H11 Cl1 2.8339 no . 2_657 H11 C1 3.2324 no . 2_657 H11 C2 3.3001 no . 2_657 H11 C11 3.3550 no . 2_657 H11 H1 2.6862 no . 2_657 H11 H2 2.8272 no . 2_657 H11 H10 3.1692 no . 2_657 H11 H17 2.9802 no . 2_567 H12 C1 3.3572 no . 2_557 H12 C2 3.5690 no . 2_557 H12 C3 3.2870 no . 2_557 H12 C4 2.8918 no . 2_557 H12 C5 2.9239 no . 2_557 H12 C13 3.5613 no . 2_567 H12 H4 3.1594 no . 2_557 H12 H5 3.2449 no . 2_557 H12 H12 3.4857 no . 2_567 H12 H17 3.2820 no . 2_567 H13 Cl2 3.2350 no . 1_565 H13 C23 3.1382 no . 1_655 H13 H5 2.9569 no . 1_565 H13 H22 3.0223 no . 1_655 H13 H23 3.0079 no . 1_655 H13 H24 2.8514 no . 1_655 H14 C23 3.4208 no . 1_655 H14 H20 3.3923 no . 2_656 H14 H21 3.4682 no . 2_656 H14 H22 2.9574 no . 1_655 H14 H24 3.1071 no . 1_655 H15 C3 3.5602 no . 1_655 H15 C23 3.3230 no . 1_655 H15 H3 2.8697 no . 1_655 H15 H4 3.4165 no . 1_655 H15 H16 3.0937 no . 1_655 H15 H22 3.3141 no . 1_655 H15 H23 3.5700 no . 1_655 H15 H24 2.6267 no . 1_655 H16 H10 3.5595 no . 1_455 H16 H15 3.0937 no . 1_455 H17 Cl1 2.9412 no . 1_465 H17 C1 3.5518 no . 1_465 H17 C12 3.3764 no . 2_567 H17 C13 3.5516 no . 2_567 H17 H1 2.7330 no . 1_465 H17 H11 2.9802 no . 2_567 H17 H12 3.2820 no . 2_567 H18 C1 2.8827 no . 2_557 H18 C2 3.2443 no . 2_557 H18 C5 3.4416 no . 2_557 H18 H1 3.1688 no . 1_465 H18 H1 2.9412 no . 2_557 H18 H2 3.5847 no . 2_557 H18 H10 3.1772 no . 1_455 H19 Cl2 2.8884 no . 2_556 H19 C18 3.3167 no . 2_556 H19 C19 3.0807 no . 2_556 H19 C20 3.3175 no . 2_556 H19 C24 3.5504 no . 1_455 H19 H6 3.4812 no . 2_566 H19 H9 3.3023 no . 2_566 H19 H19 3.3108 no . 2_556 H19 H26 2.7396 no . 1_455 H20 Cl1 3.4259 no . 2_656 H20 C7 3.4171 no . 2_566 H20 C18 3.5200 no . 2_556 H20 C23 3.1940 no . 2_556 H20 H4 2.8651 no . 2_556 H20 H6 3.1587 no . 2_566 H20 H7 3.1232 no . 2_566 H20 H9 3.2219 no . 2_566 H20 H14 3.3923 no . 2_656 H20 H22 2.6728 no . 2_556 H20 H24 3.0765 no . 2_556 H20 H27 3.5024 no . 2_656 H21 Ti1 3.5842 no . 2_656 H21 Cl1 3.2032 no . 2_656 H21 Cl2 3.1683 no . 2_656 H21 N1 3.4742 no . 2_656 H21 C8 3.5330 no . 2_566 H21 C22 3.5965 no . 2_656 H21 C24 3.1482 no . 2_656 H21 H8 2.9938 no . 2_566 H21 H9 3.3398 no . 2_566 H21 H14 3.4682 no . 2_656 H21 H22 3.4779 no . 2_556 H21 H26 3.1108 no . 2_656 H21 H27 2.5057 no . 2_656 H22 C15 3.2781 no . 1_455 H22 C19 3.5815 no . 2_556 H22 C20 2.9328 no . 2_556 H22 C21 3.4027 no . 2_556 H22 C24 2.7642 no . 1_455 H22 H13 3.0223 no . 1_455 H22 H14 2.9574 no . 1_455 H22 H15 3.3141 no . 1_455 H22 H20 2.6728 no . 2_556 H22 H21 3.4779 no . 2_556 H22 H25 2.8102 no . 1_455 H22 H26 2.6241 no . 1_455 H22 H27 2.4007 no . 1_455 H23 Cl2 3.3038 no . 1_465 H23 H13 3.0079 no . 1_455 H23 H15 3.5700 no . 1_455 H23 H25 3.2429 no . 1_455 H23 H25 2.9245 no . 2_566 H23 H27 3.5027 no . 1_455 H24 C15 3.0271 no . 1_455 H24 H13 2.8514 no . 1_455 H24 H14 3.1071 no . 1_455 H24 H15 2.6267 no . 1_455 H24 H20 3.0765 no . 2_556 H25 C23 3.4720 no . 1_655 H25 H8 3.3574 no . 2_566 H25 H22 2.8102 no . 1_655 H25 H23 3.2429 no . 1_655 H25 H23 2.9245 no . 2_566 H26 Cl2 2.9259 no . 2_656 H26 C19 3.5909 no . 1_655 H26 C21 3.1062 no . 2_656 H26 C22 3.3455 no . 2_656 H26 C23 3.4618 no . 1_655 H26 H19 2.7396 no . 1_655 H26 H21 3.1108 no . 2_656 H26 H22 2.6241 no . 1_655 H27 C20 3.4873 no . 2_656 H27 C21 2.9379 no . 2_656 H27 C23 3.3124 no . 1_655 H27 H20 3.5024 no . 2_656 H27 H21 2.5057 no . 2_656 H27 H22 2.4007 no . 1_655 H27 H23 3.5027 no . 1_655 #============================================================================== data__Cp-25Cy2NHC _database_code_depnum_ccdc_archive 'CCDC 817926' #TrackingRef '- CIFfiles.txt' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C20 H31 Cl2 N3 Ti ' _chemical_formula_moiety 'C20 H31 Cl2 N3 Ti ' _chemical_formula_weight 432.29 _chemical_melting_point ? #============================================================================== # 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 9.0816(3) _cell_length_b 12.7130(5) _cell_length_c 18.7394(7) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 2163.54(13) _cell_formula_units_Z 4 _cell_measurement_reflns_used 16967 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 123.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912.00 _exptl_absorpt_coefficient_mu 0.651 _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 0.693 _exptl_absorpt_correction_T_max 0.889 #============================================================================== # 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 21288 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_ambient_temperature 123.1 #============================================================================== # 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 4941 _reflns_number_gt 4746 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0854 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 4941 _refine_ls_number_parameters 237 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0348P)^2^+1.0996P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.24 _refine_diff_density_min -0.42 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 2141 Friedel Pairs' _refine_ls_abs_structure_Flack 0.01(2) 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) ; 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) ; 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 0.02906(4) 0.13329(3) 0.65777(2) 0.02446(10) Uani 1.00 1 d . . . Cl(1) Cl -0.09192(6) 0.28576(5) 0.62537(4) 0.03686(14) Uani 1.00 1 d . . . Cl(2) Cl -0.11695(6) -0.00230(5) 0.61501(3) 0.03421(14) Uani 1.00 1 d . . . N(1) N 0.18247(18) 0.13264(15) 0.59995(9) 0.0242(3) Uani 1.00 1 d . . . N(2) N 0.3724(2) 0.04788(14) 0.53619(11) 0.0265(4) Uani 1.00 1 d . . . N(3) N 0.4294(2) 0.19438(14) 0.59483(11) 0.0274(4) Uani 1.00 1 d . . . C(1) C -0.0330(4) 0.0699(4) 0.77412(17) 0.0872(16) Uani 1.00 1 d . . . C(2) C 0.1114(4) 0.0353(2) 0.75703(16) 0.0548(8) Uani 1.00 1 d . . . C(3) C 0.1977(3) 0.1240(2) 0.75266(15) 0.0496(7) Uani 1.00 1 d . . . C(4) C 0.1134(5) 0.2102(2) 0.76329(17) 0.0673(11) Uani 1.00 1 d . . . C(5) C -0.0271(5) 0.1804(4) 0.77759(18) 0.0876(15) Uani 1.00 1 d . . . C(6) C 0.3211(2) 0.12635(18) 0.57821(11) 0.0241(4) Uani 1.00 1 d . . . C(7) C 0.5331(2) 0.05600(18) 0.52943(15) 0.0338(5) Uani 1.00 1 d . . . C(8) C 0.5627(2) 0.16968(18) 0.55268(15) 0.0334(5) Uani 1.00 1 d . . . C(9) C 0.2897(2) -0.04944(16) 0.52497(12) 0.0236(4) Uani 1.00 1 d . . . C(10) C 0.3209(2) -0.13061(19) 0.58293(12) 0.0293(4) Uani 1.00 1 d . . . C(11) C 0.2292(2) -0.23017(18) 0.57034(12) 0.0314(5) Uani 1.00 1 d . . . C(12) C 0.2541(2) -0.27420(17) 0.49599(13) 0.0304(4) Uani 1.00 1 d . . . C(13) C 0.2231(2) -0.19205(18) 0.43927(13) 0.0319(5) Uani 1.00 1 d . . . C(14) C 0.3179(2) -0.09360(18) 0.45045(12) 0.0280(4) Uani 1.00 1 d . . . C(15) C 0.4015(2) 0.29920(16) 0.62453(12) 0.0249(4) Uani 1.00 1 d . . . C(16) C 0.4969(2) 0.32094(18) 0.68968(12) 0.0299(4) Uani 1.00 1 d . . . C(17) C 0.4546(2) 0.42728(18) 0.72290(13) 0.0325(5) Uani 1.00 1 d . . . C(18) C 0.4649(2) 0.51540(18) 0.66819(13) 0.0349(5) Uani 1.00 1 d . . . C(19) C 0.3754(3) 0.49148(18) 0.60173(14) 0.0357(5) Uani 1.00 1 d . . . C(20) C 0.4188(2) 0.38582(17) 0.56928(13) 0.0305(4) Uani 1.00 1 d . . . H(1) H -0.1230 0.0243 0.7831 0.112 Uiso 1.00 1 c R . . H(2) H 0.1285 -0.0426 0.7531 0.030 Uiso 1.00 1 c R . . H(3) H 0.3095 0.1267 0.7398 0.030 Uiso 1.00 1 c R . . H(4) H 0.1680 0.2878 0.7555 0.030 Uiso 1.00 1 c R . . H(5) H -0.1150 0.2327 0.7887 0.100 Uiso 1.00 1 c R . . H(6) H 0.5651 0.0439 0.4796 0.040 Uiso 1.00 1 c R . . H(7) H 0.5836 0.0052 0.5611 0.040 Uiso 1.00 1 c R . . H(8) H 0.6528 0.1747 0.5822 0.040 Uiso 1.00 1 c R . . H(9) H 0.5723 0.2170 0.5110 0.040 Uiso 1.00 1 c R . . H(10) H 0.1827 -0.0314 0.5279 0.028 Uiso 1.00 1 c R . . H(11) H 0.2966 -0.1006 0.6302 0.035 Uiso 1.00 1 c R . . H(12) H 0.4269 -0.1488 0.5827 0.035 Uiso 1.00 1 c R . . H(13) H 0.2562 -0.2840 0.6062 0.038 Uiso 1.00 1 c R . . H(14) H 0.1235 -0.2135 0.5765 0.038 Uiso 1.00 1 c R . . H(15) H 0.3573 -0.2984 0.4916 0.036 Uiso 1.00 1 c R . . H(16) H 0.1889 -0.3356 0.4885 0.036 Uiso 1.00 1 c R . . H(17) H 0.1177 -0.1723 0.4409 0.038 Uiso 1.00 1 c R . . H(18) H 0.2437 -0.2221 0.3916 0.038 Uiso 1.00 1 c R . . H(19) H 0.4234 -0.1118 0.4452 0.034 Uiso 1.00 1 c R . . H(20) H 0.2930 -0.0400 0.4140 0.034 Uiso 1.00 1 c R . . H(21) H 0.2967 0.3004 0.6408 0.030 Uiso 1.00 1 c R . . H(22) H 0.6019 0.3221 0.6755 0.036 Uiso 1.00 1 c R . . H(23) H 0.4832 0.2642 0.7253 0.036 Uiso 1.00 1 c R . . H(24) H 0.3528 0.4234 0.7416 0.039 Uiso 1.00 1 c R . . H(25) H 0.5212 0.4427 0.7634 0.039 Uiso 1.00 1 c R . . H(26) H 0.4289 0.5816 0.6898 0.042 Uiso 1.00 1 c R . . H(27) H 0.5693 0.5258 0.6547 0.042 Uiso 1.00 1 c R . . H(28) H 0.3912 0.5478 0.5661 0.043 Uiso 1.00 1 c R . . H(29) H 0.2695 0.4904 0.6141 0.043 Uiso 1.00 1 c R . . H(30) H 0.3554 0.3706 0.5275 0.037 Uiso 1.00 1 c R . . H(31) H 0.5222 0.3887 0.5528 0.037 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) 0.01435(16) 0.03095(19) 0.02809(19) -0.00162(16) 0.00203(15) -0.00526(16) Cl(1) 0.0228(2) 0.0317(2) 0.0561(3) 0.0041(2) 0.0013(2) -0.0074(2) Cl(2) 0.0251(2) 0.0339(2) 0.0437(3) -0.0089(2) -0.0021(2) -0.0038(2) N(1) 0.0162(7) 0.0274(8) 0.0291(9) -0.0006(7) 0.0021(7) -0.0051(8) N(2) 0.0144(8) 0.0223(8) 0.0427(10) -0.0003(6) 0.0051(7) -0.0066(7) N(3) 0.0152(8) 0.0246(8) 0.0425(10) -0.0018(6) 0.0055(7) -0.0081(8) C(1) 0.064(2) 0.171(4) 0.0266(14) -0.069(3) 0.0020(16) 0.022(2) C(2) 0.088(2) 0.0455(15) 0.0308(13) -0.0088(17) -0.0044(16) 0.0076(11) C(3) 0.0391(13) 0.073(2) 0.0364(13) -0.0126(15) -0.0139(12) 0.0154(14) C(4) 0.110(3) 0.0555(19) 0.0366(15) -0.010(2) -0.024(2) -0.0090(13) C(5) 0.090(3) 0.144(4) 0.0287(15) 0.049(3) 0.0133(19) -0.016(2) C(6) 0.0172(9) 0.0256(10) 0.0295(10) 0.0007(8) 0.0005(8) -0.0018(8) C(7) 0.0174(10) 0.0285(11) 0.0553(15) -0.0026(9) 0.0100(11) -0.0123(10) C(8) 0.0141(10) 0.0301(11) 0.0560(15) -0.0017(8) 0.0061(10) -0.0088(10) C(9) 0.0197(9) 0.0222(10) 0.0290(11) -0.0019(8) 0.0024(8) -0.0020(8) C(10) 0.0294(11) 0.0321(11) 0.0264(10) -0.0008(10) -0.0002(9) -0.0010(9) C(11) 0.0338(12) 0.0280(11) 0.0326(11) 0.0007(10) 0.0062(10) 0.0029(9) C(12) 0.0314(11) 0.0225(10) 0.0372(11) -0.0018(9) 0.0039(10) -0.0028(9) C(13) 0.0342(12) 0.0318(11) 0.0296(11) -0.0042(10) 0.0009(10) -0.0034(9) C(14) 0.0279(10) 0.0287(11) 0.0276(11) -0.0030(9) 0.0038(9) -0.0014(8) C(15) 0.0161(9) 0.0233(10) 0.0353(11) 0.0009(7) 0.0017(9) -0.0053(8) C(16) 0.0258(11) 0.0321(11) 0.0318(11) -0.0003(8) -0.0025(9) 0.0008(9) C(17) 0.0280(12) 0.0351(12) 0.0343(11) -0.0022(10) -0.0010(10) -0.0056(9) C(18) 0.0330(11) 0.0291(11) 0.0425(12) -0.0008(10) -0.0042(11) -0.0049(9) C(19) 0.0384(12) 0.0270(11) 0.0417(13) 0.0049(10) -0.0058(11) -0.0016(10) C(20) 0.0287(10) 0.0280(11) 0.0349(11) 0.0013(9) -0.0028(9) -0.0006(9) #============================================================================== _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) 2.3093(7) yes . . Ti(1) Cl(2) 2.3177(7) yes . . Ti(1) N(1) 1.7650(16) yes . . Ti(1) C(1) 2.392(3) yes . . Ti(1) C(2) 2.360(3) yes . . Ti(1) C(3) 2.350(2) yes . . Ti(1) C(4) 2.335(3) yes . . Ti(1) C(5) 2.379(3) yes . . N(1) C(6) 1.325(2) yes . . N(2) C(6) 1.354(2) yes . . N(2) C(7) 1.468(2) yes . . N(2) C(9) 1.462(2) yes . . N(3) C(6) 1.346(2) yes . . N(3) C(8) 1.480(3) yes . . N(3) C(15) 1.466(2) yes . . C(1) C(2) 1.420(5) yes . . C(1) C(5) 1.407(8) yes . . C(2) C(3) 1.376(4) yes . . C(3) C(4) 1.351(5) yes . . C(4) C(5) 1.358(7) yes . . C(7) C(8) 1.533(3) yes . . C(9) C(10) 1.525(3) yes . . C(9) C(14) 1.527(3) yes . . C(10) C(11) 1.534(3) yes . . C(11) C(12) 1.518(3) yes . . C(12) C(13) 1.517(3) yes . . C(13) C(14) 1.534(3) yes . . C(15) C(16) 1.522(3) yes . . C(15) C(20) 1.520(3) yes . . C(16) C(17) 1.537(3) yes . . C(17) C(18) 1.521(3) yes . . C(18) C(19) 1.518(3) yes . . C(19) C(20) 1.526(3) yes . . C(1) H(1) 1.016 no . . C(2) H(2) 1.006 no . . C(3) H(3) 1.044 no . . C(4) H(4) 1.114 no . . C(5) H(5) 1.059 no . . C(7) H(6) 0.990 no . . C(7) H(7) 0.990 no . . C(8) H(8) 0.990 no . . C(8) H(9) 0.990 no . . C(9) H(10) 1.000 no . . C(10) H(11) 0.990 no . . C(10) H(12) 0.990 no . . C(11) H(13) 0.990 no . . C(11) H(14) 0.990 no . . C(12) H(15) 0.990 no . . C(12) H(16) 0.990 no . . C(13) H(17) 0.990 no . . C(13) H(18) 0.990 no . . C(14) H(19) 0.990 no . . C(14) H(20) 0.990 no . . C(15) H(21) 1.000 no . . C(16) H(22) 0.990 no . . C(16) H(23) 0.990 no . . C(17) H(24) 0.990 no . . C(17) H(25) 0.990 no . . C(18) H(26) 0.990 no . . C(18) H(27) 0.990 no . . C(19) H(28) 0.990 no . . C(19) H(29) 0.990 no . . C(20) H(30) 0.990 no . . C(20) H(31) 0.990 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) 105.14(2) yes . . . Cl(1) Ti(1) N(1) 102.60(6) yes . . . Cl(1) Ti(1) C(1) 114.22(12) yes . . . Cl(1) Ti(1) C(2) 143.21(8) yes . . . Cl(1) Ti(1) C(3) 123.44(8) yes . . . Cl(1) Ti(1) C(4) 91.56(9) yes . . . Cl(1) Ti(1) C(5) 86.27(13) yes . . . Cl(2) Ti(1) N(1) 103.64(6) yes . . . Cl(2) Ti(1) C(1) 85.97(11) yes . . . Cl(2) Ti(1) C(2) 93.52(8) yes . . . Cl(2) Ti(1) C(3) 126.68(8) yes . . . Cl(2) Ti(1) C(4) 142.36(9) yes . . . Cl(2) Ti(1) C(5) 113.00(13) yes . . . N(1) Ti(1) C(1) 138.08(12) yes . . . N(1) Ti(1) C(2) 103.37(11) yes . . . N(1) Ti(1) C(3) 87.12(8) yes . . . N(1) Ti(1) C(4) 105.24(13) yes . . . N(1) Ti(1) C(5) 138.58(14) yes . . . C(1) Ti(1) C(2) 34.77(14) yes . . . C(1) Ti(1) C(3) 56.43(12) yes . . . C(1) Ti(1) C(4) 56.39(15) yes . . . C(1) Ti(1) C(5) 34.29(19) yes . . . C(2) Ti(1) C(3) 33.97(12) yes . . . C(2) Ti(1) C(4) 56.60(11) yes . . . C(2) Ti(1) C(5) 57.11(15) yes . . . C(3) Ti(1) C(4) 33.52(13) yes . . . C(3) Ti(1) C(5) 55.82(14) yes . . . C(4) Ti(1) C(5) 33.48(17) yes . . . Ti(1) N(1) C(6) 159.82(15) yes . . . C(6) N(2) C(7) 109.90(17) yes . . . C(6) N(2) C(9) 122.05(18) yes . . . C(7) N(2) C(9) 123.86(17) yes . . . C(6) N(3) C(8) 109.76(18) yes . . . C(6) N(3) C(15) 123.08(17) yes . . . C(8) N(3) C(15) 122.46(17) yes . . . Ti(1) C(1) C(2) 71.39(18) yes . . . Ti(1) C(1) C(5) 72.4(2) yes . . . C(2) C(1) C(5) 106.5(3) yes . . . Ti(1) C(2) C(1) 73.8(2) yes . . . Ti(1) C(2) C(3) 72.61(17) yes . . . C(1) C(2) C(3) 106.6(3) yes . . . Ti(1) C(3) C(2) 73.42(18) yes . . . Ti(1) C(3) C(4) 72.6(2) yes . . . C(2) C(3) C(4) 109.4(3) yes . . . Ti(1) C(4) C(3) 73.84(18) yes . . . Ti(1) C(4) C(5) 75.0(2) yes . . . C(3) C(4) C(5) 109.6(3) yes . . . Ti(1) C(5) C(1) 73.3(2) yes . . . Ti(1) C(5) C(4) 71.5(2) yes . . . C(1) C(5) C(4) 107.8(4) yes . . . N(1) C(6) N(2) 123.37(19) yes . . . N(1) C(6) N(3) 125.7(2) yes . . . N(2) C(6) N(3) 110.91(17) yes . . . N(2) C(7) C(8) 102.49(17) yes . . . N(3) C(8) C(7) 102.00(17) yes . . . N(2) C(9) C(10) 112.02(18) yes . . . N(2) C(9) C(14) 110.89(18) yes . . . C(10) C(9) C(14) 111.81(17) yes . . . C(9) C(10) C(11) 110.37(18) yes . . . C(10) C(11) C(12) 111.37(19) yes . . . C(11) C(12) C(13) 111.19(18) yes . . . C(12) C(13) C(14) 111.21(19) yes . . . C(9) C(14) C(13) 109.31(18) yes . . . N(3) C(15) C(16) 111.80(17) yes . . . N(3) C(15) C(20) 112.47(18) yes . . . C(16) C(15) C(20) 110.87(17) yes . . . C(15) C(16) C(17) 110.02(18) yes . . . C(16) C(17) C(18) 111.06(19) yes . . . C(17) C(18) C(19) 111.86(19) yes . . . C(18) C(19) C(20) 111.4(2) yes . . . C(15) C(20) C(19) 109.87(19) yes . . . Ti(1) C(1) H(1) 122.2 no . . . C(2) C(1) H(1) 127.1 no . . . C(5) C(1) H(1) 126.4 no . . . Ti(1) C(2) H(2) 120.7 no . . . C(1) C(2) H(2) 117.6 no . . . C(3) C(2) H(2) 135.7 no . . . Ti(1) C(3) H(3) 117.2 no . . . C(2) C(3) H(3) 126.5 no . . . C(4) C(3) H(3) 124.0 no . . . Ti(1) C(4) H(4) 114.0 no . . . C(3) C(4) H(4) 116.5 no . . . C(5) C(4) H(4) 133.7 no . . . Ti(1) C(5) H(5) 120.4 no . . . C(1) C(5) H(5) 127.4 no . . . C(4) C(5) H(5) 124.8 no . . . N(2) C(7) H(6) 111.3 no . . . N(2) C(7) H(7) 111.3 no . . . C(8) C(7) H(6) 111.3 no . . . C(8) C(7) H(7) 111.3 no . . . H(6) C(7) H(7) 109.2 no . . . N(3) C(8) H(8) 111.4 no . . . N(3) C(8) H(9) 111.4 no . . . C(7) C(8) H(8) 111.4 no . . . C(7) C(8) H(9) 111.4 no . . . H(8) C(8) H(9) 109.2 no . . . N(2) C(9) H(10) 107.3 no . . . C(10) C(9) H(10) 107.3 no . . . C(14) C(9) H(10) 107.3 no . . . C(9) C(10) H(11) 109.6 no . . . C(9) C(10) H(12) 109.6 no . . . C(11) C(10) H(11) 109.6 no . . . C(11) C(10) H(12) 109.6 no . . . H(11) C(10) H(12) 108.1 no . . . C(10) C(11) H(13) 109.4 no . . . C(10) C(11) H(14) 109.4 no . . . C(12) C(11) H(13) 109.4 no . . . C(12) C(11) H(14) 109.3 no . . . H(13) C(11) H(14) 108.0 no . . . C(11) C(12) H(15) 109.4 no . . . C(11) C(12) H(16) 109.4 no . . . C(13) C(12) H(15) 109.4 no . . . C(13) C(12) H(16) 109.4 no . . . H(15) C(12) H(16) 108.0 no . . . C(12) C(13) H(17) 109.4 no . . . C(12) C(13) H(18) 109.4 no . . . C(14) C(13) H(17) 109.4 no . . . C(14) C(13) H(18) 109.4 no . . . H(17) C(13) H(18) 108.0 no . . . C(9) C(14) H(19) 109.8 no . . . C(9) C(14) H(20) 109.8 no . . . C(13) C(14) H(19) 109.8 no . . . C(13) C(14) H(20) 109.8 no . . . H(19) C(14) H(20) 108.3 no . . . N(3) C(15) H(21) 107.1 no . . . C(16) C(15) H(21) 107.1 no . . . C(20) C(15) H(21) 107.1 no . . . C(15) C(16) H(22) 109.7 no . . . C(15) C(16) H(23) 109.7 no . . . C(17) C(16) H(22) 109.7 no . . . C(17) C(16) H(23) 109.7 no . . . H(22) C(16) H(23) 108.2 no . . . C(16) C(17) H(24) 109.4 no . . . C(16) C(17) H(25) 109.4 no . . . C(18) C(17) H(24) 109.4 no . . . C(18) C(17) H(25) 109.4 no . . . H(24) C(17) H(25) 108.0 no . . . C(17) C(18) H(26) 109.3 no . . . C(17) C(18) H(27) 109.2 no . . . C(19) C(18) H(26) 109.2 no . . . C(19) C(18) H(27) 109.2 no . . . H(26) C(18) H(27) 107.9 no . . . C(18) C(19) H(28) 109.3 no . . . C(18) C(19) H(29) 109.3 no . . . C(20) C(19) H(28) 109.3 no . . . C(20) C(19) H(29) 109.3 no . . . H(28) C(19) H(29) 108.0 no . . . C(15) C(20) H(30) 109.7 no . . . C(15) C(20) H(31) 109.7 no . . . C(19) C(20) H(30) 109.7 no . . . C(19) C(20) H(31) 109.7 no . . . H(30) C(20) H(31) 108.2 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) N(1) C(6) 130.1(4) ? . . . . Cl(1) Ti(1) C(1) C(2) -153.12(19) ? . . . . Cl(1) Ti(1) C(1) C(5) -38.2(2) ? . . . . Cl(1) Ti(1) C(2) C(1) 43.5(3) ? . . . . Cl(1) Ti(1) C(2) C(3) -70.2(2) ? . . . . Cl(1) Ti(1) C(3) C(2) 137.52(17) ? . . . . Cl(1) Ti(1) C(3) C(4) 20.3(2) ? . . . . Cl(1) Ti(1) C(4) C(3) -163.1(2) ? . . . . Cl(1) Ti(1) C(4) C(5) 80.8(2) ? . . . . Cl(1) Ti(1) C(5) C(1) 145.6(2) ? . . . . Cl(1) Ti(1) C(5) C(4) -98.5(2) ? . . . . Cl(2) Ti(1) N(1) C(6) -120.6(4) ? . . . . Cl(2) Ti(1) C(1) C(2) 102.1(2) ? . . . . Cl(2) Ti(1) C(1) C(5) -143.0(2) ? . . . . Cl(2) Ti(1) C(2) C(1) -77.8(2) ? . . . . Cl(2) Ti(1) C(2) C(3) 168.49(18) ? . . . . Cl(2) Ti(1) C(3) C(2) -14.4(2) ? . . . . Cl(2) Ti(1) C(3) C(4) -131.6(2) ? . . . . Cl(2) Ti(1) C(4) C(3) 79.3(2) ? . . . . Cl(2) Ti(1) C(4) C(5) -36.8(3) ? . . . . Cl(2) Ti(1) C(5) C(1) 40.7(2) ? . . . . Cl(2) Ti(1) C(5) C(4) 156.6(2) ? . . . . N(1) Ti(1) C(1) C(2) -3.9(3) ? . . . . N(1) Ti(1) C(1) C(5) 111.0(3) ? . . . . C(1) Ti(1) N(1) C(6) -21.3(5) ? . . . . N(1) Ti(1) C(2) C(1) 177.3(2) ? . . . . N(1) Ti(1) C(2) C(3) 63.57(19) ? . . . . C(2) Ti(1) N(1) C(6) -23.6(5) ? . . . . N(1) Ti(1) C(3) C(2) -119.3(2) ? . . . . N(1) Ti(1) C(3) C(4) 123.5(2) ? . . . . C(3) Ti(1) N(1) C(6) 6.5(5) ? . . . . N(1) Ti(1) C(4) C(3) -59.6(2) ? . . . . N(1) Ti(1) C(4) C(5) -175.7(2) ? . . . . C(4) Ti(1) N(1) C(6) 35.0(5) ? . . . . N(1) Ti(1) C(5) C(1) -109.5(2) ? . . . . N(1) Ti(1) C(5) C(4) 6.3(4) ? . . . . C(5) Ti(1) N(1) C(6) 31.4(5) ? . . . . C(1) Ti(1) C(2) C(3) -113.7(3) ? . . . . C(2) Ti(1) C(1) C(5) 114.9(3) ? . . . . C(1) Ti(1) C(3) C(2) 38.8(2) ? . . . . C(1) Ti(1) C(3) C(4) -78.4(2) ? . . . . C(3) Ti(1) C(1) C(2) -37.9(2) ? . . . . C(3) Ti(1) C(1) C(5) 77.1(2) ? . . . . C(1) Ti(1) C(4) C(3) 78.5(2) ? . . . . C(1) Ti(1) C(4) C(5) -37.5(2) ? . . . . C(4) Ti(1) C(1) C(2) -78.4(2) ? . . . . C(4) Ti(1) C(1) C(5) 36.6(2) ? . . . . C(1) Ti(1) C(5) C(4) 115.9(4) ? . . . . C(5) Ti(1) C(1) C(2) -114.9(3) ? . . . . C(2) Ti(1) C(3) C(4) -117.2(3) ? . . . . C(3) Ti(1) C(2) C(1) 113.7(3) ? . . . . C(2) Ti(1) C(4) C(3) 36.5(2) ? . . . . C(2) Ti(1) C(4) C(5) -79.5(3) ? . . . . C(4) Ti(1) C(2) C(1) 77.7(2) ? . . . . C(4) Ti(1) C(2) C(3) -36.0(2) ? . . . . C(2) Ti(1) C(5) C(1) -38.0(2) ? . . . . C(2) Ti(1) C(5) C(4) 77.9(2) ? . . . . C(5) Ti(1) C(2) C(1) 37.5(2) ? . . . . C(5) Ti(1) C(2) C(3) -76.3(2) ? . . . . C(3) Ti(1) C(4) C(5) -116.0(3) ? . . . . C(4) Ti(1) C(3) C(2) 117.2(3) ? . . . . C(3) Ti(1) C(5) C(1) -79.0(2) ? . . . . C(3) Ti(1) C(5) C(4) 36.9(2) ? . . . . C(5) Ti(1) C(3) C(2) 80.4(2) ? . . . . C(5) Ti(1) C(3) C(4) -36.8(2) ? . . . . C(4) Ti(1) C(5) C(1) -115.9(4) ? . . . . C(5) Ti(1) C(4) C(3) 116.0(3) ? . . . . Ti(1) N(1) C(6) N(2) 113.7(4) ? . . . . Ti(1) N(1) C(6) N(3) -65.4(5) ? . . . . C(6) N(2) C(7) C(8) -18.0(2) ? . . . . C(7) N(2) C(6) N(1) -172.7(2) ? . . . . C(7) N(2) C(6) N(3) 6.6(2) ? . . . . C(6) N(2) C(9) C(10) -86.3(2) ? . . . . C(6) N(2) C(9) C(14) 148.0(2) ? . . . . C(9) N(2) C(6) N(1) -14.9(3) ? . . . . C(9) N(2) C(6) N(3) 164.36(19) ? . . . . C(7) N(2) C(9) C(10) 68.3(2) ? . . . . C(7) N(2) C(9) C(14) -57.4(2) ? . . . . C(9) N(2) C(7) C(8) -175.3(2) ? . . . . C(6) N(3) C(8) C(7) -19.1(2) ? . . . . C(8) N(3) C(6) N(1) -172.1(2) ? . . . . C(8) N(3) C(6) N(2) 8.6(2) ? . . . . C(6) N(3) C(15) C(16) 131.5(2) ? . . . . C(6) N(3) C(15) C(20) -103.0(2) ? . . . . C(15) N(3) C(6) N(1) -16.0(3) ? . . . . C(15) N(3) C(6) N(2) 164.79(19) ? . . . . C(8) N(3) C(15) C(16) -75.3(2) ? . . . . C(8) N(3) C(15) C(20) 50.2(2) ? . . . . C(15) N(3) C(8) C(7) -175.41(19) ? . . . . Ti(1) C(1) C(2) C(3) 65.7(2) ? . . . . Ti(1) C(1) C(5) C(4) -63.6(2) ? . . . . C(2) C(1) C(5) Ti(1) 63.7(2) ? . . . . C(2) C(1) C(5) C(4) 0.0(3) ? . . . . C(5) C(1) C(2) Ti(1) -64.3(2) ? . . . . C(5) C(1) C(2) C(3) 1.4(3) ? . . . . Ti(1) C(2) C(3) C(4) 64.2(2) ? . . . . C(1) C(2) C(3) Ti(1) -66.6(2) ? . . . . C(1) C(2) C(3) C(4) -2.4(3) ? . . . . Ti(1) C(3) C(4) C(5) 67.1(2) ? . . . . C(2) C(3) C(4) Ti(1) -64.7(2) ? . . . . C(2) C(3) C(4) C(5) 2.4(3) ? . . . . Ti(1) C(4) C(5) C(1) 64.9(2) ? . . . . C(3) C(4) C(5) Ti(1) -66.4(2) ? . . . . C(3) C(4) C(5) C(1) -1.5(3) ? . . . . N(2) C(7) C(8) N(3) 21.3(2) ? . . . . N(2) C(9) C(10) C(11) 178.49(17) ? . . . . N(2) C(9) C(14) C(13) -176.92(17) ? . . . . C(10) C(9) C(14) C(13) 57.3(2) ? . . . . C(14) C(9) C(10) C(11) -56.3(2) ? . . . . C(9) C(10) C(11) C(12) 54.8(2) ? . . . . C(10) C(11) C(12) C(13) -55.5(2) ? . . . . C(11) C(12) C(13) C(14) 57.0(2) ? . . . . C(12) C(13) C(14) C(9) -57.2(2) ? . . . . N(3) C(15) C(16) C(17) -175.04(17) ? . . . . N(3) C(15) C(20) C(19) 175.08(18) ? . . . . C(16) C(15) C(20) C(19) -58.9(2) ? . . . . C(20) C(15) C(16) C(17) 58.6(2) ? . . . . C(15) C(16) C(17) C(18) -55.7(2) ? . . . . C(16) C(17) C(18) C(19) 54.0(2) ? . . . . C(17) C(18) C(19) C(20) -54.7(2) ? . . . . C(18) C(19) C(20) C(15) 56.5(2) ? . . . . 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 C(5) C(11) 3.575(4) ? . 3_556 C(11) C(5) 3.575(4) ? . 3_546 Cl(1) H(2) 3.171 ? . 3_556 Cl(1) H(6) 3.255 ? . 2_456 Cl(1) H(8) 2.833 ? . 1_455 Cl(1) H(9) 2.959 ? . 2_456 Cl(1) H(20) 3.477 ? . 2_456 Cl(1) H(22) 2.971 ? . 1_455 Cl(1) H(30) 3.520 ? . 2_456 Cl(2) H(7) 2.903 ? . 1_455 Cl(2) H(8) 3.132 ? . 1_455 Cl(2) H(15) 3.235 ? . 2_446 Cl(2) H(16) 3.334 ? . 2_446 Cl(2) H(24) 3.564 ? . 3_546 Cl(2) H(28) 3.444 ? . 2_456 Cl(2) H(30) 3.163 ? . 2_456 N(1) H(9) 2.996 ? . 2_456 N(1) H(31) 3.222 ? . 2_456 C(1) H(13) 3.548 ? . 3_556 C(1) H(19) 3.399 ? . 4_555 C(1) H(20) 3.431 ? . 4_555 C(1) H(24) 3.463 ? . 3_546 C(1) H(29) 3.166 ? . 3_546 C(2) H(20) 3.068 ? . 4_555 C(2) H(25) 3.558 ? . 3_646 C(2) H(27) 3.340 ? . 3_646 C(3) H(18) 2.935 ? . 4_555 C(3) H(20) 3.209 ? . 4_555 C(3) H(25) 3.452 ? . 3_646 C(3) H(26) 3.598 ? . 3_646 C(3) H(27) 3.009 ? . 3_646 C(4) H(18) 2.736 ? . 4_555 C(5) H(13) 3.045 ? . 3_556 C(5) H(14) 3.172 ? . 3_556 C(5) H(18) 3.387 ? . 4_555 C(5) H(19) 3.393 ? . 4_555 C(6) H(9) 3.444 ? . 2_456 C(7) H(16) 3.157 ? . 2_546 C(7) H(29) 3.492 ? . 2_556 C(7) H(30) 3.253 ? . 2_556 C(8) H(30) 3.096 ? . 2_556 C(9) H(31) 3.493 ? . 2_456 C(10) H(5) 3.507 ? . 3_546 C(10) H(25) 3.349 ? . 3_646 C(11) H(5) 2.876 ? . 3_546 C(11) H(15) 3.590 ? . 2_446 C(11) H(19) 3.440 ? . 2_446 C(11) H(28) 3.183 ? . 1_545 C(12) H(7) 3.489 ? . 2_446 C(12) H(12) 3.459 ? . 2_446 C(12) H(17) 3.572 ? . 2_546 C(12) H(19) 3.512 ? . 2_446 C(12) H(28) 2.897 ? . 1_545 C(13) H(12) 3.391 ? . 2_446 C(13) H(15) 3.567 ? . 2_446 C(13) H(27) 3.085 ? . 2_456 C(13) H(28) 3.529 ? . 2_456 C(14) H(27) 3.118 ? . 2_456 C(17) H(1) 3.257 ? . 3_556 C(17) H(3) 3.392 ? . 3_656 C(17) H(11) 3.578 ? . 3_656 C(18) H(1) 3.239 ? . 3_556 C(18) H(3) 3.028 ? . 3_656 C(18) H(13) 3.384 ? . 1_565 C(18) H(17) 3.176 ? . 2_556 C(18) H(20) 3.369 ? . 2_556 C(19) H(1) 3.177 ? . 3_556 C(19) H(6) 3.236 ? . 2_456 C(19) H(13) 3.054 ? . 1_565 C(19) H(15) 3.379 ? . 1_565 C(19) H(16) 3.494 ? . 1_565 C(19) H(17) 3.281 ? . 2_556 C(20) H(6) 3.457 ? . 2_456 C(20) H(10) 3.534 ? . 2_556 H(1) C(17) 3.257 ? . 3_546 H(1) C(18) 3.239 ? . 3_546 H(1) C(19) 3.177 ? . 3_546 H(1) H(4) 3.119 ? . 3_546 H(1) H(13) 3.422 ? . 3_556 H(1) H(21) 3.553 ? . 3_546 H(1) H(24) 2.493 ? . 3_546 H(1) H(26) 2.917 ? . 3_546 H(1) H(29) 2.381 ? . 3_546 H(2) Cl(1) 3.171 ? . 3_546 H(2) H(4) 3.453 ? . 3_546 H(2) H(5) 2.965 ? . 3_546 H(2) H(20) 3.272 ? . 4_555 H(2) H(22) 3.277 ? . 3_646 H(2) H(25) 3.202 ? . 3_646 H(2) H(27) 3.358 ? . 3_646 H(3) C(17) 3.392 ? . 3_646 H(3) C(18) 3.028 ? . 3_646 H(3) H(18) 3.129 ? . 4_555 H(3) H(20) 3.570 ? . 4_555 H(3) H(25) 2.799 ? . 3_646 H(3) H(26) 2.777 ? . 3_646 H(3) H(27) 2.601 ? . 3_646 H(4) H(1) 3.119 ? . 3_556 H(4) H(2) 3.453 ? . 3_556 H(4) H(18) 2.800 ? . 4_555 H(5) C(10) 3.507 ? . 3_556 H(5) C(11) 2.876 ? . 3_556 H(5) H(2) 2.965 ? . 3_556 H(5) H(11) 3.086 ? . 3_556 H(5) H(13) 2.359 ? . 3_556 H(5) H(14) 2.617 ? . 3_556 H(5) H(22) 3.521 ? . 1_455 H(5) H(26) 3.461 ? . 3_546 H(6) Cl(1) 3.255 ? . 2_556 H(6) C(19) 3.236 ? . 2_556 H(6) C(20) 3.457 ? . 2_556 H(6) H(16) 2.938 ? . 2_546 H(6) H(28) 3.296 ? . 2_556 H(6) H(29) 2.592 ? . 2_556 H(6) H(30) 2.855 ? . 2_556 H(7) Cl(2) 2.903 ? . 1_655 H(7) C(12) 3.489 ? . 2_546 H(7) H(16) 2.535 ? . 2_546 H(7) H(25) 3.514 ? . 3_646 H(7) H(30) 3.369 ? . 2_556 H(8) Cl(1) 2.833 ? . 1_655 H(8) Cl(2) 3.132 ? . 1_655 H(8) H(30) 2.819 ? . 2_556 H(9) Cl(1) 2.959 ? . 2_556 H(9) N(1) 2.996 ? . 2_556 H(9) C(6) 3.444 ? . 2_556 H(9) H(21) 3.506 ? . 2_556 H(9) H(30) 2.893 ? . 2_556 H(10) C(20) 3.534 ? . 2_456 H(10) H(27) 3.573 ? . 2_456 H(10) H(28) 3.187 ? . 2_456 H(10) H(31) 2.775 ? . 2_456 H(11) C(17) 3.578 ? . 3_646 H(11) H(5) 3.086 ? . 3_546 H(11) H(25) 2.649 ? . 3_646 H(12) C(12) 3.459 ? . 2_546 H(12) C(13) 3.391 ? . 2_546 H(12) H(16) 2.735 ? . 2_546 H(12) H(17) 2.893 ? . 2_546 H(12) H(18) 3.347 ? . 2_546 H(12) H(25) 3.146 ? . 3_646 H(13) C(1) 3.548 ? . 3_546 H(13) C(5) 3.045 ? . 3_546 H(13) C(18) 3.384 ? . 1_545 H(13) C(19) 3.054 ? . 1_545 H(13) H(1) 3.422 ? . 3_546 H(13) H(5) 2.359 ? . 3_546 H(13) H(17) 3.445 ? . 2_546 H(13) H(19) 3.438 ? . 2_446 H(13) H(26) 2.799 ? . 1_545 H(13) H(28) 2.577 ? . 1_545 H(13) H(29) 2.875 ? . 1_545 H(14) C(5) 3.172 ? . 3_546 H(14) H(5) 2.617 ? . 3_546 H(14) H(15) 2.738 ? . 2_446 H(14) H(18) 3.595 ? . 2_446 H(14) H(19) 2.899 ? . 2_446 H(15) Cl(2) 3.235 ? . 2_546 H(15) C(11) 3.590 ? . 2_546 H(15) C(13) 3.567 ? . 2_546 H(15) C(19) 3.379 ? . 1_545 H(15) H(14) 2.738 ? . 2_546 H(15) H(16) 3.480 ? . 2_546 H(15) H(17) 2.707 ? . 2_546 H(15) H(28) 2.421 ? . 1_545 H(16) Cl(2) 3.334 ? . 2_546 H(16) C(7) 3.157 ? . 2_446 H(16) C(19) 3.494 ? . 1_545 H(16) H(6) 2.938 ? . 2_446 H(16) H(7) 2.535 ? . 2_446 H(16) H(12) 2.735 ? . 2_446 H(16) H(15) 3.480 ? . 2_446 H(16) H(19) 2.794 ? . 2_446 H(16) H(28) 2.772 ? . 1_545 H(16) H(29) 3.312 ? . 1_545 H(17) C(12) 3.572 ? . 2_446 H(17) C(18) 3.176 ? . 2_456 H(17) C(19) 3.281 ? . 2_456 H(17) H(12) 2.893 ? . 2_446 H(17) H(13) 3.445 ? . 2_446 H(17) H(15) 2.707 ? . 2_446 H(17) H(26) 3.205 ? . 2_456 H(17) H(27) 2.622 ? . 2_456 H(17) H(28) 2.599 ? . 2_456 H(18) C(3) 2.935 ? . 4_554 H(18) C(4) 2.736 ? . 4_554 H(18) C(5) 3.387 ? . 4_554 H(18) H(3) 3.129 ? . 4_554 H(18) H(4) 2.800 ? . 4_554 H(18) H(12) 3.347 ? . 2_446 H(18) H(14) 3.595 ? . 2_546 H(18) H(27) 3.080 ? . 2_456 H(19) C(1) 3.399 ? . 4_554 H(19) C(5) 3.393 ? . 4_554 H(19) C(11) 3.440 ? . 2_546 H(19) C(12) 3.512 ? . 2_546 H(19) H(13) 3.438 ? . 2_546 H(19) H(14) 2.899 ? . 2_546 H(19) H(16) 2.794 ? . 2_546 H(20) Cl(1) 3.477 ? . 2_556 H(20) C(1) 3.431 ? . 4_554 H(20) C(2) 3.068 ? . 4_554 H(20) C(3) 3.209 ? . 4_554 H(20) C(18) 3.369 ? . 2_456 H(20) H(2) 3.272 ? . 4_554 H(20) H(3) 3.570 ? . 4_554 H(20) H(27) 2.412 ? . 2_456 H(20) H(31) 3.184 ? . 2_456 H(21) H(1) 3.553 ? . 3_556 H(21) H(9) 3.506 ? . 2_456 H(22) Cl(1) 2.971 ? . 1_655 H(22) H(2) 3.277 ? . 3_656 H(22) H(5) 3.521 ? . 1_655 H(23) H(26) 2.925 ? . 3_646 H(24) Cl(2) 3.564 ? . 3_556 H(24) C(1) 3.463 ? . 3_556 H(24) H(1) 2.493 ? . 3_556 H(25) C(2) 3.558 ? . 3_656 H(25) C(3) 3.452 ? . 3_656 H(25) C(10) 3.349 ? . 3_656 H(25) H(2) 3.202 ? . 3_656 H(25) H(3) 2.799 ? . 3_656 H(25) H(7) 3.514 ? . 3_656 H(25) H(11) 2.649 ? . 3_656 H(25) H(12) 3.146 ? . 3_656 H(26) C(3) 3.598 ? . 3_656 H(26) H(1) 2.917 ? . 3_556 H(26) H(3) 2.777 ? . 3_656 H(26) H(5) 3.461 ? . 3_556 H(26) H(13) 2.799 ? . 1_565 H(26) H(17) 3.205 ? . 2_556 H(26) H(23) 2.925 ? . 3_656 H(27) C(2) 3.340 ? . 3_656 H(27) C(3) 3.009 ? . 3_656 H(27) C(13) 3.085 ? . 2_556 H(27) C(14) 3.118 ? . 2_556 H(27) H(2) 3.358 ? . 3_656 H(27) H(3) 2.601 ? . 3_656 H(27) H(10) 3.573 ? . 2_556 H(27) H(17) 2.622 ? . 2_556 H(27) H(18) 3.080 ? . 2_556 H(27) H(20) 2.412 ? . 2_556 H(28) Cl(2) 3.444 ? . 2_556 H(28) C(11) 3.183 ? . 1_565 H(28) C(12) 2.897 ? . 1_565 H(28) C(13) 3.529 ? . 2_556 H(28) H(6) 3.296 ? . 2_456 H(28) H(10) 3.187 ? . 2_556 H(28) H(13) 2.577 ? . 1_565 H(28) H(15) 2.421 ? . 1_565 H(28) H(16) 2.772 ? . 1_565 H(28) H(17) 2.599 ? . 2_556 H(29) C(1) 3.166 ? . 3_556 H(29) C(7) 3.492 ? . 2_456 H(29) H(1) 2.381 ? . 3_556 H(29) H(6) 2.592 ? . 2_456 H(29) H(13) 2.875 ? . 1_565 H(29) H(16) 3.312 ? . 1_565 H(30) Cl(1) 3.520 ? . 2_556 H(30) Cl(2) 3.163 ? . 2_556 H(30) C(7) 3.253 ? . 2_456 H(30) C(8) 3.096 ? . 2_456 H(30) H(6) 2.855 ? . 2_456 H(30) H(7) 3.369 ? . 2_456 H(30) H(8) 2.819 ? . 2_456 H(30) H(9) 2.893 ? . 2_456 H(31) N(1) 3.222 ? . 2_556 H(31) C(9) 3.493 ? . 2_556 H(31) H(10) 2.775 ? . 2_556 H(31) H(20) 3.184 ? . 2_556 #============================================================================== data__Cp-25tBu2NHC _database_code_depnum_ccdc_archive 'CCDC 817927' #TrackingRef '- CIFfiles.txt' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C16 H27 Cl2 N3 Ti ' _chemical_formula_moiety 'C16 H27 Cl2 N3 Ti ' _chemical_formula_weight 380.22 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2+Z 3 +X,1/2-Y,+Z 4 1/2-X,-Y,1/2+Z 5 -X,-Y,-Z 6 1/2+X,1/2-Y,1/2-Z 7 -X,1/2+Y,-Z 8 1/2+X,+Y,1/2-Z #------------------------------------------------------------------------------ _cell_length_a 12.8021(3) _cell_length_b 17.5227(4) _cell_length_c 8.7440(2) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 1961.53(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 14534 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 123.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800.00 _exptl_absorpt_coefficient_mu 0.709 _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 0.736 _exptl_absorpt_correction_T_max 0.893 #============================================================================== # 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 18393 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_theta_max 27.44 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_ambient_temperature 123.1 #============================================================================== # 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 2310 _reflns_number_gt 2181 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0993 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2310 _refine_ls_number_parameters 107 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0496P)^2^+1.9236P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.65 _refine_diff_density_min -0.53 _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) ; 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) ; 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 0.52564(3) 0.2500 0.67414(4) 0.01865(13) Uani 1.00 2 d S . . Cl(1) Cl 0.63592(3) 0.35164(3) 0.62534(5) 0.02867(14) Uani 1.00 1 d . . . N(1) N 0.43722(15) 0.2500 0.5167(2) 0.0197(3) Uani 1.00 2 d S . . N(2) N 0.31548(14) 0.18710(9) 0.3545(2) 0.0358(4) Uani 1.00 1 d . . . C(1) C 0.3860(3) 0.2500 0.8469(4) 0.0598(12) Uani 1.00 2 d S . . C(2) C 0.4441(2) 0.31288(18) 0.8792(2) 0.0662(9) Uani 1.00 1 d . . . C(3) C 0.5396(2) 0.2889(2) 0.9368(2) 0.0669(9) Uani 1.00 1 d . . . C(4) C 0.36136(17) 0.2500 0.4144(3) 0.0181(4) Uani 1.00 2 d S . . C(5) C 0.24340(14) 0.20718(10) 0.2338(2) 0.0264(3) Uani 1.00 1 d . . . C(6) C 0.35009(16) 0.10620(10) 0.3742(2) 0.0352(4) Uani 1.00 1 d . . . C(7) C 0.45925(19) 0.09597(12) 0.3072(2) 0.0400(5) Uani 1.00 1 d . . . C(8) C 0.34869(18) 0.08373(12) 0.5419(3) 0.0452(5) Uani 1.00 1 d . . . C(9) C 0.2725(2) 0.05498(13) 0.2897(5) 0.1005(16) Uani 1.00 1 d . . . H(1) H 0.3097 0.2500 0.8005 0.023 Uiso 1.00 2 c R . . H(2) H 0.4081 0.3586 0.8444 0.023 Uiso 1.00 1 c R . . H(3) H 0.6036 0.3232 0.9701 0.023 Uiso 1.00 1 c R . . H(4) H 0.2669 0.1878 0.1379 0.032 Uiso 1.00 1 c R . . H(5) H 0.1753 0.1878 0.2541 0.032 Uiso 1.00 1 c R . . H(6) H 0.4792 0.0420 0.3127 0.048 Uiso 1.00 1 c R . . H(7) H 0.5092 0.1267 0.3657 0.048 Uiso 1.00 1 c R . . H(8) H 0.4594 0.1126 0.2002 0.048 Uiso 1.00 1 c R . . H(9) H 0.3592 0.0285 0.5511 0.054 Uiso 1.00 1 c R . . H(10) H 0.2812 0.0976 0.5869 0.054 Uiso 1.00 1 c R . . H(11) H 0.4048 0.1105 0.5960 0.054 Uiso 1.00 1 c R . . H(12) H 0.2938 0.0015 0.3005 0.121 Uiso 1.00 1 c R . . H(13) H 0.2713 0.0688 0.1811 0.121 Uiso 1.00 1 c R . . H(14) H 0.2026 0.0618 0.3333 0.121 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) 0.0130(2) 0.0304(2) 0.0126(2) 0.0000 -0.00106(14) 0.0000 Cl(1) 0.0242(2) 0.0326(2) 0.0292(2) -0.00700(16) -0.00150(16) -0.00301(17) N(1) 0.0190(9) 0.0229(9) 0.0171(8) 0.0000 -0.0040(7) 0.0000 N(2) 0.0389(9) 0.0174(7) 0.0512(10) -0.0008(6) -0.0304(8) -0.0002(6) C(1) 0.0269(14) 0.129(4) 0.0232(14) 0.0000 0.0102(12) 0.0000 C(2) 0.103(2) 0.0694(18) 0.0264(11) 0.0316(18) 0.0278(13) -0.0027(11) C(3) 0.0578(14) 0.126(2) 0.0169(9) -0.0389(15) 0.0071(9) -0.0204(11) C(4) 0.0180(10) 0.0197(10) 0.0167(9) 0.0000 -0.0019(8) 0.0000 C(5) 0.0295(8) 0.0274(8) 0.0222(8) -0.0038(7) -0.0113(6) -0.0008(6) C(6) 0.0354(10) 0.0164(7) 0.0539(12) -0.0015(7) -0.0216(9) 0.0011(7) C(7) 0.0619(14) 0.0286(9) 0.0296(9) 0.0072(9) 0.0061(9) -0.0023(7) C(8) 0.0389(10) 0.0283(9) 0.0683(15) 0.0028(8) 0.0203(10) 0.0204(10) C(9) 0.098(2) 0.0192(10) 0.184(4) -0.0016(12) -0.102(2) -0.0099(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) 2.3124(5) yes . . Ti(1) Cl(1) 2.3124(5) yes . 3_555 Ti(1) N(1) 1.7823(18) yes . . Ti(1) C(1) 2.340(3) yes . . Ti(1) C(2) 2.350(2) yes . . Ti(1) C(2) 2.350(2) yes . 3_555 Ti(1) C(3) 2.403(2) yes . . Ti(1) C(3) 2.403(2) yes . 3_555 N(1) C(4) 1.320(3) yes . . N(2) C(4) 1.354(2) yes . . N(2) C(5) 1.446(2) yes . . N(2) C(6) 1.495(2) yes . . C(1) C(2) 1.359(3) yes . . C(1) C(2) 1.359(3) yes . 3_555 C(2) C(3) 1.387(4) yes . . C(3) C(3) 1.364(4) yes . 3_555 C(5) C(5) 1.501(2) yes . 3_555 C(6) C(7) 1.526(3) yes . . C(6) C(8) 1.519(3) yes . . C(6) C(9) 1.529(4) yes . . C(5) H(4) 0.953 no . . C(5) H(5) 0.952 no . . C(7) H(6) 0.980 no . . C(7) H(7) 0.980 no . . C(7) H(8) 0.980 no . . C(8) H(9) 0.980 no . . C(8) H(10) 0.980 no . . C(8) H(11) 0.980 no . . C(9) H(12) 0.980 no . . C(9) H(13) 0.980 no . . C(9) H(14) 0.980 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(1) 100.74(2) yes . . 3_555 Cl(1) Ti(1) N(1) 104.20(3) yes . . . Cl(1) Ti(1) C(1) 125.83(3) yes . . . Cl(1) Ti(1) C(2) 92.92(8) yes . . . Cl(1) Ti(1) C(2) 140.66(7) yes . . 3_555 Cl(1) Ti(1) C(3) 84.98(7) yes . . . Cl(1) Ti(1) C(3) 110.47(7) yes . . 3_555 Cl(1) Ti(1) N(1) 104.20(3) yes 3_555 . . Cl(1) Ti(1) C(1) 125.83(3) yes 3_555 . . Cl(1) Ti(1) C(2) 140.66(7) yes 3_555 . . Cl(1) Ti(1) C(2) 92.92(8) yes 3_555 . 3_555 Cl(1) Ti(1) C(3) 110.47(7) yes 3_555 . . Cl(1) Ti(1) C(3) 84.98(7) yes 3_555 . 3_555 N(1) Ti(1) C(1) 90.77(10) yes . . . N(1) Ti(1) C(2) 107.89(9) yes . . . N(1) Ti(1) C(2) 107.89(9) yes . . 3_555 N(1) Ti(1) C(3) 141.77(8) yes . . . N(1) Ti(1) C(3) 141.77(8) yes . . 3_555 C(1) Ti(1) C(2) 33.68(9) yes . . . C(1) Ti(1) C(2) 33.68(9) yes . . 3_555 C(1) Ti(1) C(3) 55.92(10) yes . . . C(1) Ti(1) C(3) 55.92(10) yes . . 3_555 C(2) Ti(1) C(2) 55.93(10) yes . . 3_555 C(2) Ti(1) C(3) 33.92(10) yes . . . C(2) Ti(1) C(3) 55.70(10) yes . . 3_555 C(2) Ti(1) C(3) 55.70(10) yes 3_555 . . C(2) Ti(1) C(3) 33.92(10) yes 3_555 . 3_555 C(3) Ti(1) C(3) 32.98(11) yes . . 3_555 Ti(1) N(1) C(4) 172.08(17) yes . . . C(4) N(2) C(5) 111.17(15) yes . . . C(4) N(2) C(6) 126.77(17) yes . . . C(5) N(2) C(6) 120.26(16) yes . . . Ti(1) C(1) C(2) 73.5(2) yes . . . Ti(1) C(1) C(2) 73.5(2) yes . . 3_555 C(2) C(1) C(2) 108.4(3) yes . . 3_555 Ti(1) C(2) C(1) 72.79(19) yes . . . Ti(1) C(2) C(3) 75.14(17) yes . . . C(1) C(2) C(3) 108.2(2) yes . . . Ti(1) C(3) C(2) 70.94(14) yes . . . Ti(1) C(3) C(3) 73.51(14) yes . . 3_555 C(2) C(3) C(3) 107.6(2) yes . . 3_555 N(1) C(4) N(2) 125.52(11) yes . . . N(1) C(4) N(2) 125.52(11) yes . . 3_555 N(2) C(4) N(2) 108.95(19) yes . . 3_555 N(2) C(5) C(5) 104.09(14) yes . . 3_555 N(2) C(6) C(7) 109.79(16) yes . . . N(2) C(6) C(8) 110.70(17) yes . . . N(2) C(6) C(9) 107.95(18) yes . . . C(7) C(6) C(8) 110.55(17) yes . . . C(7) C(6) C(9) 109.9(2) yes . . . C(8) C(6) C(9) 107.9(2) yes . . . Ti(1) C(1) H(1) 117.2 no . . . C(2) C(1) H(1) 125.8 no . . . C(2) C(1) H(1) 125.8 no 3_555 . . Ti(1) C(2) H(2) 111.0 no . . . C(1) C(2) H(2) 110.1 no . . . C(3) C(2) H(2) 141.3 no . . . Ti(1) C(3) H(3) 118.8 no . . . C(2) C(3) H(3) 127.7 no . . . C(3) C(3) H(3) 124.6 no 3_555 . . N(2) C(5) H(4) 110.7 no . . . N(2) C(5) H(5) 111.2 no . . . C(5) C(5) H(4) 110.9 no 3_555 . . C(5) C(5) H(5) 110.9 no 3_555 . . H(4) C(5) H(5) 109.0 no . . . C(6) C(7) H(6) 109.5 no . . . C(6) C(7) H(7) 109.5 no . . . C(6) C(7) H(8) 109.5 no . . . H(6) C(7) H(7) 109.5 no . . . H(6) C(7) H(8) 109.5 no . . . H(7) C(7) H(8) 109.5 no . . . C(6) C(8) H(9) 109.5 no . . . C(6) C(8) H(10) 109.5 no . . . C(6) C(8) H(11) 109.5 no . . . H(9) C(8) H(10) 109.5 no . . . H(9) C(8) H(11) 109.5 no . . . H(10) C(8) H(11) 109.5 no . . . C(6) C(9) H(12) 109.5 no . . . C(6) C(9) H(13) 109.5 no . . . C(6) C(9) H(14) 109.5 no . . . H(12) C(9) H(13) 109.5 no . . . H(12) C(9) H(14) 109.5 no . . . H(13) C(9) H(14) 109.5 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) N(1) C(4) -127.397(19) ? . . . . Cl(1) Ti(1) C(1) C(2) -14.1(2) ? . . . . Cl(1) Ti(1) C(1) C(2) -129.54(14) ? . . . 3_555 Cl(1) Ti(1) C(2) C(1) 168.61(17) ? . . . . Cl(1) Ti(1) C(2) C(3) -76.53(18) ? . . . . Cl(1) Ti(1) C(2) C(3) -34.4(2) ? . . 3_555 3_555 Cl(1) Ti(1) C(2) C(1) 80.5(2) ? . . 3_555 . Cl(1) Ti(1) C(3) C(2) 102.85(18) ? . . . . Cl(1) Ti(1) C(3) C(3) -141.29(16) ? . . . 3_555 Cl(1) Ti(1) C(3) C(2) 157.54(16) ? . . 3_555 3_555 Cl(1) Ti(1) C(3) C(3) 41.68(17) ? . . 3_555 . Cl(1) Ti(1) N(1) C(4) 127.397(19) ? 3_555 . . . Cl(1) Ti(1) C(1) C(2) 129.54(14) ? 3_555 . . . Cl(1) Ti(1) C(1) C(2) 14.1(2) ? 3_555 . . 3_555 Cl(1) Ti(1) C(2) C(1) -80.5(2) ? 3_555 . . . Cl(1) Ti(1) C(2) C(3) 34.4(2) ? 3_555 . . . Cl(1) Ti(1) C(2) C(3) 76.53(18) ? 3_555 . 3_555 3_555 Cl(1) Ti(1) C(2) C(1) -168.61(17) ? 3_555 . 3_555 . Cl(1) Ti(1) C(3) C(2) -157.54(16) ? 3_555 . . . Cl(1) Ti(1) C(3) C(3) -41.68(17) ? 3_555 . . 3_555 Cl(1) Ti(1) C(3) C(2) -102.85(18) ? 3_555 . 3_555 3_555 Cl(1) Ti(1) C(3) C(3) 141.29(16) ? 3_555 . 3_555 . N(1) Ti(1) C(1) C(2) -122.27(17) ? . . . . N(1) Ti(1) C(1) C(2) 122.27(17) ? . . . 3_555 N(1) Ti(1) C(2) C(1) 62.68(18) ? . . . . N(1) Ti(1) C(2) C(3) 177.54(17) ? . . . . C(2) Ti(1) N(1) C(4) -29.52(8) ? . . . . N(1) Ti(1) C(2) C(3) -177.54(17) ? . . 3_555 3_555 N(1) Ti(1) C(2) C(1) -62.68(18) ? . . 3_555 . C(2) Ti(1) N(1) C(4) 29.52(8) ? 3_555 . . . N(1) Ti(1) C(3) C(2) -3.8(2) ? . . . . N(1) Ti(1) C(3) C(3) 112.07(17) ? . . . 3_555 C(3) Ti(1) N(1) C(4) -27.30(13) ? . . . . N(1) Ti(1) C(3) C(2) 3.8(2) ? . . 3_555 3_555 N(1) Ti(1) C(3) C(3) -112.07(17) ? . . 3_555 . C(3) Ti(1) N(1) C(4) 27.30(13) ? 3_555 . . . C(1) Ti(1) C(2) C(3) 114.9(2) ? . . . . C(2) Ti(1) C(1) C(2) -115.5(2) ? . . . 3_555 C(1) Ti(1) C(2) C(3) -114.9(2) ? . . 3_555 3_555 C(2) Ti(1) C(1) C(2) 115.5(2) ? 3_555 . . . C(1) Ti(1) C(3) C(2) -37.41(16) ? . . . . C(1) Ti(1) C(3) C(3) 78.45(16) ? . . . 3_555 C(3) Ti(1) C(1) C(2) 37.69(19) ? . . . . C(3) Ti(1) C(1) C(2) -77.8(2) ? . . . 3_555 C(1) Ti(1) C(3) C(2) 37.41(16) ? . . 3_555 3_555 C(1) Ti(1) C(3) C(3) -78.45(16) ? . . 3_555 . C(3) Ti(1) C(1) C(2) 77.8(2) ? 3_555 . . . C(3) Ti(1) C(1) C(2) -37.69(19) ? 3_555 . . 3_555 C(2) Ti(1) C(2) C(3) -77.7(2) ? . . 3_555 3_555 C(2) Ti(1) C(2) C(1) 37.19(18) ? . . 3_555 . C(2) Ti(1) C(2) C(1) -37.19(18) ? 3_555 . . . C(2) Ti(1) C(2) C(3) 77.7(2) ? 3_555 . . . C(2) Ti(1) C(3) C(3) 115.9(2) ? . . . 3_555 C(3) Ti(1) C(2) C(1) -114.9(2) ? . . . . C(2) Ti(1) C(3) C(2) 78.4(2) ? . . 3_555 3_555 C(2) Ti(1) C(3) C(3) -37.44(17) ? . . 3_555 . C(3) Ti(1) C(2) C(1) -78.49(19) ? 3_555 . . . C(3) Ti(1) C(2) C(3) 36.37(18) ? 3_555 . . . C(2) Ti(1) C(3) C(2) -78.4(2) ? 3_555 . . . C(2) Ti(1) C(3) C(3) 37.44(17) ? 3_555 . . 3_555 C(3) Ti(1) C(2) C(3) -36.37(18) ? . . 3_555 3_555 C(3) Ti(1) C(2) C(1) 78.49(19) ? . . 3_555 . C(2) Ti(1) C(3) C(3) -115.9(2) ? 3_555 . 3_555 . C(3) Ti(1) C(2) C(1) 114.9(2) ? 3_555 . 3_555 . C(3) Ti(1) C(3) C(2) 115.9(2) ? . . 3_555 3_555 C(3) Ti(1) C(3) C(2) -115.9(2) ? 3_555 . . . Ti(1) N(1) C(4) N(2) -89.3(2) ? . . . . Ti(1) N(1) C(4) N(2) 89.3(2) ? . . . 3_555 C(4) N(2) C(5) C(5) -4.4(2) ? . . . 3_555 C(5) N(2) C(4) N(1) -173.7(2) ? . . . . C(5) N(2) C(4) N(2) 7.4(2) ? . . . 3_555 C(4) N(2) C(6) C(7) -61.8(2) ? . . . . C(4) N(2) C(6) C(8) 60.5(2) ? . . . . C(4) N(2) C(6) C(9) 178.3(2) ? . . . . C(6) N(2) C(4) N(1) -9.1(3) ? . . . . C(6) N(2) C(4) N(2) 172.01(19) ? . . . 3_555 C(5) N(2) C(6) C(7) 101.5(2) ? . . . . C(5) N(2) C(6) C(8) -136.16(18) ? . . . . C(5) N(2) C(6) C(9) -18.3(2) ? . . . . C(6) N(2) C(5) C(5) -170.17(16) ? . . . 3_555 Ti(1) C(1) C(2) C(3) -67.39(19) ? . . . . Ti(1) C(1) C(2) C(3) 67.39(19) ? . . 3_555 3_555 C(2) C(1) C(2) Ti(1) -65.8(2) ? . . 3_555 . C(2) C(1) C(2) C(3) 1.6(3) ? . . 3_555 3_555 C(2) C(1) C(2) Ti(1) 65.8(2) ? 3_555 . . . C(2) C(1) C(2) C(3) -1.6(3) ? 3_555 . . . Ti(1) C(2) C(3) C(3) -64.86(17) ? . . . 3_555 C(1) C(2) C(3) Ti(1) 65.8(2) ? . . . . C(1) C(2) C(3) C(3) 1.0(3) ? . . . 3_555 Ti(1) C(3) C(3) C(2) -63.17(17) ? . . 3_555 3_555 C(2) C(3) C(3) Ti(1) 63.17(17) ? . . 3_555 . 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(5) 3.5797(18) ? . 6_555 C(5) Cl(1) 3.5797(18) ? . 6_455 Ti(1) H(1) 2.977 ? . . Ti(1) H(2) 2.846 ? . . Ti(1) H(2) 2.846 ? . 3_555 Ti(1) H(3) 3.056 ? . . Ti(1) H(3) 3.056 ? . 3_555 Cl(1) H(1) 2.923 ? . 6_556 Cl(1) H(2) 3.491 ? . . Cl(1) H(2) 3.497 ? . 8_556 Cl(1) H(3) 3.083 ? . . Cl(1) H(4) 2.931 ? . 6_555 Cl(1) H(5) 3.426 ? . 6_555 Cl(1) H(9) 3.463 ? . 7_656 Cl(1) H(10) 3.253 ? . 6_556 Cl(1) H(12) 2.851 ? . 7_656 Cl(1) H(13) 3.482 ? . 6_555 N(1) H(1) 2.970 ? . . N(1) H(2) 3.460 ? . . N(1) H(2) 3.460 ? . 3_555 N(2) H(3) 3.121 ? . 6_456 C(1) H(1) 1.058 ? . . C(1) H(2) 1.924 ? . . C(1) H(2) 1.924 ? . 3_555 C(1) H(3) 3.251 ? . . C(1) H(3) 3.251 ? . 3_555 C(1) H(4) 3.160 ? . 1_556 C(1) H(4) 3.160 ? . 3_556 C(2) H(1) 2.156 ? . . C(2) H(2) 0.973 ? . . C(2) H(2) 3.055 ? . 3_555 C(2) H(3) 2.199 ? . . C(2) H(3) 3.239 ? . 3_555 C(2) H(4) 3.203 ? . 3_556 C(2) H(8) 3.102 ? . 3_556 C(3) H(1) 3.247 ? . . C(3) H(2) 2.231 ? . . C(3) H(2) 3.189 ? . 3_555 C(3) H(3) 1.057 ? . . C(3) H(3) 2.149 ? . 3_555 C(3) H(5) 3.239 ? . 6_556 C(3) H(8) 3.055 ? . 3_556 C(4) H(1) 3.440 ? . . C(5) H(3) 3.193 ? . 6_456 C(5) H(7) 3.425 ? . 8_455 C(7) H(5) 3.245 ? . 8_555 C(7) H(9) 3.420 ? . 5_656 C(7) H(14) 3.402 ? . 8_555 C(8) H(2) 2.932 ? . 3_555 C(8) H(3) 3.538 ? . 6_456 C(8) H(6) 3.366 ? . 5_656 C(8) H(12) 3.267 ? . 4_555 C(8) H(13) 3.314 ? . 4_555 C(9) H(9) 3.055 ? . 4_554 C(9) H(10) 3.282 ? . 4_554 H(1) Ti(1) 2.977 ? . . H(1) Cl(1) 2.923 ? . 6_456 H(1) Cl(1) 2.923 ? . 8_456 H(1) N(1) 2.970 ? . . H(1) C(1) 1.058 ? . . H(1) C(2) 2.156 ? . . H(1) C(2) 2.156 ? . 3_555 H(1) C(3) 3.247 ? . . H(1) C(3) 3.247 ? . 3_555 H(1) C(4) 3.440 ? . . H(1) H(2) 2.314 ? . . H(1) H(2) 2.314 ? . 3_555 H(1) H(4) 3.193 ? . 1_556 H(1) H(4) 3.193 ? . 3_556 H(1) H(10) 3.279 ? . . H(1) H(10) 3.279 ? . 3_555 H(1) H(11) 3.264 ? . . H(1) H(11) 3.264 ? . 3_555 H(2) Ti(1) 2.846 ? . . H(2) Cl(1) 3.491 ? . . H(2) Cl(1) 3.497 ? . 8_456 H(2) N(1) 3.460 ? . . H(2) C(1) 1.924 ? . . H(2) C(2) 0.973 ? . . H(2) C(2) 3.055 ? . 3_555 H(2) C(3) 2.231 ? . . H(2) C(3) 3.189 ? . 3_555 H(2) C(8) 2.932 ? . 3_555 H(2) H(1) 2.314 ? . . H(2) H(3) 2.803 ? . . H(2) H(4) 3.243 ? . 3_556 H(2) H(8) 3.220 ? . 3_556 H(2) H(9) 3.299 ? . 3_555 H(2) H(10) 2.881 ? . 3_555 H(2) H(11) 2.239 ? . 3_555 H(3) Ti(1) 3.056 ? . . H(3) Cl(1) 3.083 ? . . H(3) N(2) 3.121 ? . 6_556 H(3) C(1) 3.251 ? . . H(3) C(2) 2.199 ? . . H(3) C(2) 3.239 ? . 3_555 H(3) C(3) 1.057 ? . . H(3) C(3) 2.149 ? . 3_555 H(3) C(5) 3.193 ? . 6_556 H(3) C(8) 3.538 ? . 6_556 H(3) H(2) 2.803 ? . . H(3) H(3) 2.565 ? . 3_555 H(3) H(5) 2.588 ? . 6_556 H(3) H(5) 3.506 ? . 8_556 H(3) H(8) 2.953 ? . 3_556 H(3) H(10) 2.710 ? . 6_556 H(3) H(14) 2.936 ? . 6_556 H(4) Cl(1) 2.931 ? . 6_455 H(4) C(1) 3.160 ? . 1_554 H(4) C(2) 3.203 ? . 3_554 H(4) H(1) 3.193 ? . 1_554 H(4) H(2) 3.243 ? . 3_554 H(4) H(7) 3.468 ? . 8_455 H(5) Cl(1) 3.426 ? . 6_455 H(5) C(3) 3.239 ? . 6_456 H(5) C(7) 3.245 ? . 8_455 H(5) H(3) 2.588 ? . 6_456 H(5) H(3) 3.506 ? . 8_456 H(5) H(7) 2.601 ? . 8_455 H(5) H(8) 3.088 ? . 8_455 H(6) C(8) 3.366 ? . 5_656 H(6) H(9) 2.689 ? . 5_656 H(6) H(11) 3.161 ? . 5_656 H(6) H(14) 3.151 ? . 8_555 H(7) C(5) 3.425 ? . 8_555 H(7) H(4) 3.468 ? . 8_555 H(7) H(5) 2.601 ? . 8_555 H(7) H(9) 3.280 ? . 5_656 H(7) H(13) 3.528 ? . 8_555 H(7) H(14) 3.232 ? . 8_555 H(8) C(2) 3.102 ? . 3_554 H(8) C(3) 3.055 ? . 3_554 H(8) H(2) 3.220 ? . 3_554 H(8) H(3) 2.953 ? . 3_554 H(8) H(5) 3.088 ? . 8_555 H(8) H(14) 3.251 ? . 8_555 H(9) Cl(1) 3.463 ? . 7_646 H(9) C(7) 3.420 ? . 5_656 H(9) C(9) 3.055 ? . 4_555 H(9) H(2) 3.299 ? . 3_555 H(9) H(6) 2.689 ? . 5_656 H(9) H(7) 3.280 ? . 5_656 H(9) H(12) 2.978 ? . 4_555 H(9) H(13) 2.643 ? . 4_555 H(9) H(14) 3.037 ? . 4_555 H(10) Cl(1) 3.253 ? . 6_456 H(10) C(9) 3.282 ? . 4_555 H(10) H(1) 3.279 ? . . H(10) H(2) 2.881 ? . 3_555 H(10) H(3) 2.710 ? . 6_456 H(10) H(12) 2.726 ? . 4_555 H(10) H(13) 3.103 ? . 4_555 H(10) H(14) 3.535 ? . 4_555 H(11) H(1) 3.264 ? . . H(11) H(2) 2.239 ? . 3_555 H(11) H(6) 3.161 ? . 5_656 H(12) Cl(1) 2.851 ? . 7_646 H(12) C(8) 3.267 ? . 4_554 H(12) H(9) 2.978 ? . 4_554 H(12) H(10) 2.726 ? . 4_554 H(13) Cl(1) 3.482 ? . 6_455 H(13) C(8) 3.314 ? . 4_554 H(13) H(7) 3.528 ? . 8_455 H(13) H(9) 2.643 ? . 4_554 H(13) H(10) 3.103 ? . 4_554 H(14) C(7) 3.402 ? . 8_455 H(14) H(3) 2.936 ? . 6_456 H(14) H(6) 3.151 ? . 8_455 H(14) H(7) 3.232 ? . 8_455 H(14) H(8) 3.251 ? . 8_455 H(14) H(9) 3.037 ? . 4_554 H(14) H(10) 3.535 ? . 4_554 #============================================================================== # 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 #==============================================================================