# 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 ? loop_ _publ_author_name 'Lutz Gade' 'S. Doye' 'Raphael Kubiak' 'Carsten Muller' 'Hubert Wadepohl' 'Benjamin D. Ward' 'Katharina Weitershaus' _publ_contact_author_name 'Lutz Gade' _publ_contact_author_email LUTZ.GADE@UNI-HD.DE _publ_section_title ; Titanium Hydroamination Catalysts Bearing a 2-Aminopyrrolinato Spectator Ligand: Monitoring the Individual Reaction Steps ; # Attachment 'ga_kw3a-ga_kw18-ga_kw11-ga_kw7-ga_kw16.cif' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 718799' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H36 N2 Ti' _chemical_formula_weight 400.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6070(17) _cell_length_b 9.2070(18) _cell_length_c 15.015(3) _cell_angle_alpha 91.00(3) _cell_angle_beta 100.98(3) _cell_angle_gamma 106.19(3) _cell_volume 1118.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 0.393 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8347 _exptl_absorpt_correction_T_max 0.9095 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004-2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector (NONIUS Kappa CCD)' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6832 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 30.62 _reflns_number_total 6832 _reflns_number_gt 5821 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'HKL-2000 (Otwinowski & Minor, 2000)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF (Beurskens, 1999-2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+0.5033P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6832 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1036 _refine_ls_wR_factor_gt 0.0991 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.60698(17) 0.28888(18) 0.43299(11) 0.0306(3) Uani 1 1 d . . . H1A H 0.6780 0.2278 0.4181 0.037 Uiso 1 1 calc R . . H1B H 0.5826 0.2655 0.4939 0.037 Uiso 1 1 calc R . . C2 C 0.6912(2) 0.4566(2) 0.43110(14) 0.0460(5) Uani 1 1 d . . . H2A H 0.8091 0.4739 0.4288 0.055 Uiso 1 1 calc R . . H2B H 0.6844 0.5134 0.4862 0.055 Uiso 1 1 calc R . . C3 C 0.6009(2) 0.50839(18) 0.34629(12) 0.0374(4) Uani 1 1 d . . . H3A H 0.5750 0.6037 0.3597 0.045 Uiso 1 1 calc R . . H3B H 0.6661 0.5231 0.2978 0.045 Uiso 1 1 calc R . . C4 C 0.44610(16) 0.37732(14) 0.32027(9) 0.0207(2) Uani 1 1 d . . . C5 C 0.27027(17) 0.46813(14) 0.20395(9) 0.0210(2) Uani 1 1 d . . . C6 C 0.11792(17) 0.49980(15) 0.18959(9) 0.0233(3) Uani 1 1 d . . . H6 H 0.0387 0.4533 0.2244 0.028 Uiso 1 1 calc R . . C7 C 0.08047(18) 0.59816(15) 0.12522(10) 0.0253(3) Uani 1 1 d . . . C8 C 0.19856(19) 0.66766(16) 0.07563(9) 0.0275(3) Uani 1 1 d . . . H8 H 0.1745 0.7365 0.0324 0.033 Uiso 1 1 calc R . . C9 C 0.35064(19) 0.63840(16) 0.08819(9) 0.0265(3) Uani 1 1 d . . . C10 C 0.38513(17) 0.53678(15) 0.15182(9) 0.0235(3) Uani 1 1 d . . . H10 H 0.4878 0.5141 0.1597 0.028 Uiso 1 1 calc R . . C11 C -0.0858(2) 0.62828(18) 0.10885(11) 0.0327(3) Uani 1 1 d . . . H11A H -0.1480 0.5853 0.0480 0.049 Uiso 1 1 calc R . . H11B H -0.0702 0.7379 0.1133 0.049 Uiso 1 1 calc R . . H11C H -0.1472 0.5812 0.1546 0.049 Uiso 1 1 calc R . . C12 C 0.4753(2) 0.7119(2) 0.03206(11) 0.0381(4) Uani 1 1 d . . . H12A H 0.5360 0.8147 0.0587 0.057 Uiso 1 1 calc R . . H12B H 0.4179 0.7168 -0.0303 0.057 Uiso 1 1 calc R . . H12C H 0.5529 0.6518 0.0313 0.057 Uiso 1 1 calc R . . C13 C 0.23458(16) -0.06962(14) 0.27186(9) 0.0199(2) Uani 1 1 d . . . C14 C 0.08640(15) -0.11363(14) 0.30561(8) 0.0188(2) Uani 1 1 d . . . C15 C -0.02934(15) -0.04886(14) 0.25292(9) 0.0199(2) Uani 1 1 d . . . C16 C 0.04726(17) 0.03368(15) 0.18644(9) 0.0214(2) Uani 1 1 d . . . C17 C 0.21056(17) 0.02097(15) 0.19819(9) 0.0216(2) Uani 1 1 d . . . C18 C 0.38780(18) -0.11536(17) 0.30630(11) 0.0289(3) Uani 1 1 d . . . H18A H 0.3805 -0.2114 0.2742 0.043 Uiso 1 1 calc R . . H18B H 0.3989 -0.1280 0.3717 0.043 Uiso 1 1 calc R . . H18C H 0.4843 -0.0366 0.2956 0.043 Uiso 1 1 calc R . . C19 C 0.04944(18) -0.22672(16) 0.37487(10) 0.0263(3) Uani 1 1 d . . . H19A H 0.0134 -0.3295 0.3451 0.039 Uiso 1 1 calc R . . H19B H -0.0384 -0.2096 0.4030 0.039 Uiso 1 1 calc R . . H19C H 0.1492 -0.2150 0.4218 0.039 Uiso 1 1 calc R . . C20 C -0.20688(17) -0.07901(17) 0.26008(11) 0.0290(3) Uani 1 1 d . . . H20A H -0.2722 -0.1753 0.2260 0.044 Uiso 1 1 calc R . . H20B H -0.2489 0.0033 0.2348 0.044 Uiso 1 1 calc R . . H20C H -0.2155 -0.0847 0.3241 0.044 Uiso 1 1 calc R . . C21 C -0.0343(2) 0.11289(18) 0.11331(10) 0.0318(3) Uani 1 1 d . . . H21A H 0.0499 0.1948 0.0940 0.048 Uiso 1 1 calc R . . H21B H -0.1122 0.1554 0.1369 0.048 Uiso 1 1 calc R . . H21C H -0.0939 0.0402 0.0612 0.048 Uiso 1 1 calc R . . C22 C 0.3362(2) 0.08893(18) 0.14234(11) 0.0324(3) Uani 1 1 d . . . H22A H 0.4442 0.1326 0.1826 0.049 Uiso 1 1 calc R . . H22B H 0.3031 0.1686 0.1079 0.049 Uiso 1 1 calc R . . H22C H 0.3433 0.0099 0.1000 0.049 Uiso 1 1 calc R . . C23 C 0.23589(18) 0.09943(16) 0.46877(9) 0.0254(3) Uani 1 1 d . . . H23A H 0.2783 0.1929 0.5090 0.038 Uiso 1 1 calc R . . H23B H 0.3167 0.0415 0.4779 0.038 Uiso 1 1 calc R . . H23C H 0.1317 0.0384 0.4828 0.038 Uiso 1 1 calc R . . C24 C 0.00306(18) 0.24285(17) 0.35836(10) 0.0277(3) Uani 1 1 d . . . H24A H 0.0519 0.3432 0.3911 0.042 Uiso 1 1 calc R . . H24B H -0.0616 0.1743 0.3958 0.042 Uiso 1 1 calc R . . H24C H -0.0693 0.2514 0.3010 0.042 Uiso 1 1 calc R . . N1 N 0.45437(14) 0.25675(13) 0.36446(8) 0.0233(2) Uani 1 1 d . . . N2 N 0.29937(14) 0.36278(12) 0.26682(8) 0.0216(2) Uani 1 1 d . . . Ti Ti 0.19438(3) 0.15527(2) 0.330417(15) 0.01699(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0187(6) 0.0361(8) 0.0314(7) 0.0106(6) -0.0022(5) 0.0033(6) C2 0.0337(9) 0.0342(8) 0.0517(11) 0.0101(8) -0.0155(8) -0.0043(7) C3 0.0300(8) 0.0300(8) 0.0382(8) 0.0107(6) -0.0046(6) -0.0067(6) C4 0.0201(6) 0.0196(6) 0.0217(6) 0.0029(5) 0.0048(5) 0.0040(5) C5 0.0247(6) 0.0162(5) 0.0204(6) 0.0020(5) 0.0013(5) 0.0053(5) C6 0.0243(6) 0.0203(6) 0.0246(6) 0.0010(5) 0.0025(5) 0.0068(5) C7 0.0289(7) 0.0205(6) 0.0247(6) -0.0021(5) -0.0029(5) 0.0097(5) C8 0.0376(8) 0.0224(6) 0.0206(6) 0.0044(5) -0.0011(6) 0.0104(6) C9 0.0350(8) 0.0223(6) 0.0205(6) 0.0036(5) 0.0047(5) 0.0060(6) C10 0.0260(7) 0.0223(6) 0.0225(6) 0.0028(5) 0.0042(5) 0.0077(5) C11 0.0331(8) 0.0299(7) 0.0345(8) -0.0002(6) -0.0041(6) 0.0158(6) C12 0.0443(9) 0.0400(9) 0.0311(8) 0.0146(7) 0.0126(7) 0.0097(7) C13 0.0184(6) 0.0193(6) 0.0216(6) -0.0002(5) 0.0044(5) 0.0049(5) C14 0.0188(6) 0.0175(5) 0.0190(5) 0.0019(4) 0.0032(5) 0.0037(4) C15 0.0174(6) 0.0193(6) 0.0207(6) -0.0001(5) 0.0015(5) 0.0030(4) C16 0.0250(6) 0.0191(6) 0.0175(6) 0.0010(5) 0.0006(5) 0.0048(5) C17 0.0245(6) 0.0204(6) 0.0190(6) 0.0001(5) 0.0075(5) 0.0031(5) C18 0.0230(7) 0.0305(7) 0.0353(8) -0.0002(6) 0.0046(6) 0.0119(6) C19 0.0296(7) 0.0218(6) 0.0263(7) 0.0072(5) 0.0067(5) 0.0042(5) C20 0.0167(6) 0.0303(7) 0.0367(8) 0.0008(6) 0.0025(6) 0.0034(5) C21 0.0405(8) 0.0295(7) 0.0215(6) 0.0037(6) -0.0036(6) 0.0104(6) C22 0.0382(8) 0.0307(7) 0.0300(7) 0.0029(6) 0.0195(6) 0.0041(6) C23 0.0267(7) 0.0279(7) 0.0190(6) 0.0015(5) 0.0040(5) 0.0040(5) C24 0.0256(7) 0.0310(7) 0.0296(7) 0.0009(6) 0.0081(6) 0.0116(6) N1 0.0178(5) 0.0225(5) 0.0272(6) 0.0074(4) 0.0009(4) 0.0038(4) N2 0.0193(5) 0.0192(5) 0.0253(5) 0.0062(4) 0.0026(4) 0.0051(4) Ti 0.01581(11) 0.01675(11) 0.01768(11) 0.00205(8) 0.00330(8) 0.00349(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.4592(18) . ? C1 C2 1.516(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.518(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.508(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N1 1.3150(17) . ? C4 N2 1.3314(18) . ? C5 C10 1.3975(19) . ? C5 C6 1.3995(19) . ? C5 N2 1.4044(17) . ? C6 C7 1.3902(19) . ? C6 H6 0.9500 . ? C7 C8 1.393(2) . ? C7 C11 1.508(2) . ? C8 C9 1.388(2) . ? C8 H8 0.9500 . ? C9 C10 1.3981(19) . ? C9 C12 1.510(2) . ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C17 1.4154(18) . ? C13 C14 1.4187(18) . ? C13 C18 1.4971(19) . ? C13 Ti 2.3731(14) . ? C14 C15 1.4218(18) . ? C14 C19 1.4986(18) . ? C14 Ti 2.3843(14) . ? C15 C16 1.4165(19) . ? C15 C20 1.5003(19) . ? C15 Ti 2.3762(17) . ? C16 C17 1.4206(19) . ? C16 C21 1.5002(19) . ? C16 Ti 2.3691(16) . ? C17 C22 1.5001(19) . ? C17 Ti 2.3677(14) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 Ti 2.1364(14) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 Ti 2.1283(15) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? N1 Ti 2.1269(13) . ? N2 Ti 2.1927(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 105.52(12) . . ? N1 C1 H1A 110.6 . . ? C2 C1 H1A 110.6 . . ? N1 C1 H1B 110.6 . . ? C2 C1 H1B 110.6 . . ? H1A C1 H1B 108.8 . . ? C1 C2 C3 106.50(13) . . ? C1 C2 H2A 110.4 . . ? C3 C2 H2A 110.4 . . ? C1 C2 H2B 110.4 . . ? C3 C2 H2B 110.4 . . ? H2A C2 H2B 108.6 . . ? C4 C3 C2 101.83(12) . . ? C4 C3 H3A 111.4 . . ? C2 C3 H3A 111.4 . . ? C4 C3 H3B 111.4 . . ? C2 C3 H3B 111.4 . . ? H3A C3 H3B 109.3 . . ? N1 C4 N2 113.77(12) . . ? N1 C4 C3 113.08(12) . . ? N2 C4 C3 132.95(13) . . ? C10 C5 C6 118.77(12) . . ? C10 C5 N2 122.18(12) . . ? C6 C5 N2 118.98(12) . . ? C7 C6 C5 121.14(13) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C8 118.92(13) . . ? C6 C7 C11 120.57(14) . . ? C8 C7 C11 120.51(13) . . ? C9 C8 C7 121.30(13) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 119.09(13) . . ? C8 C9 C12 120.48(13) . . ? C10 C9 C12 120.41(14) . . ? C5 C10 C9 120.75(13) . . ? C5 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C17 C13 C14 108.15(11) . . ? C17 C13 C18 125.96(12) . . ? C14 C13 C18 125.86(12) . . ? C17 C13 Ti 72.42(8) . . ? C14 C13 Ti 73.08(8) . . ? C18 C13 Ti 121.85(10) . . ? C13 C14 C15 107.92(11) . . ? C13 C14 C19 125.95(12) . . ? C15 C14 C19 125.55(12) . . ? C13 C14 Ti 72.22(8) . . ? C15 C14 Ti 72.31(8) . . ? C19 C14 Ti 127.93(9) . . ? C16 C15 C14 107.88(11) . . ? C16 C15 C20 126.41(12) . . ? C14 C15 C20 125.34(12) . . ? C16 C15 Ti 72.36(8) . . ? C14 C15 Ti 72.93(8) . . ? C20 C15 Ti 125.85(10) . . ? C15 C16 C17 108.13(11) . . ? C15 C16 C21 125.49(13) . . ? C17 C16 C21 126.30(13) . . ? C15 C16 Ti 72.91(8) . . ? C17 C16 Ti 72.49(8) . . ? C21 C16 Ti 123.02(9) . . ? C13 C17 C16 107.92(11) . . ? C13 C17 C22 125.39(13) . . ? C16 C17 C22 126.68(13) . . ? C13 C17 Ti 72.84(7) . . ? C16 C17 Ti 72.60(8) . . ? C22 C17 Ti 120.92(10) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Ti C23 H23A 109.5 . . ? Ti C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Ti C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Ti C24 H24A 109.5 . . ? Ti C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Ti C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C4 N1 C1 110.92(12) . . ? C4 N1 Ti 93.18(9) . . ? C1 N1 Ti 147.89(10) . . ? C4 N2 C5 123.14(12) . . ? C4 N2 Ti 89.83(8) . . ? C5 N2 Ti 146.97(9) . . ? N1 Ti C24 128.60(6) . . ? N1 Ti C23 81.66(6) . . ? C24 Ti C23 88.11(6) . . ? N1 Ti N2 61.72(5) . . ? C24 Ti N2 90.57(6) . . ? C23 Ti N2 131.01(6) . . ? N1 Ti C17 92.81(6) . . ? C24 Ti C17 130.24(6) . . ? C23 Ti C17 129.08(5) . . ? N2 Ti C17 86.59(5) . . ? N1 Ti C16 124.67(5) . . ? C24 Ti C16 95.60(6) . . ? C23 Ti C16 138.12(5) . . ? N2 Ti C16 90.74(5) . . ? C17 Ti C16 34.91(5) . . ? N1 Ti C13 90.39(5) . . ? C24 Ti C13 140.77(6) . . ? C23 Ti C13 94.44(6) . . ? N2 Ti C13 115.71(5) . . ? C17 Ti C13 34.74(5) . . ? C16 Ti C13 57.84(5) . . ? N1 Ti C15 147.58(5) . . ? C24 Ti C15 83.69(6) . . ? C23 Ti C15 105.18(6) . . ? N2 Ti C15 123.33(5) . . ? C17 Ti C15 57.92(5) . . ? C16 Ti C15 34.73(5) . . ? C13 Ti C15 57.84(5) . . ? N1 Ti C14 119.79(5) . . ? C24 Ti C14 108.01(6) . . ? C23 Ti C14 81.42(6) . . ? N2 Ti C14 143.99(5) . . ? C17 Ti C14 57.76(5) . . ? C16 Ti C14 57.72(5) . . ? C13 Ti C14 34.70(4) . . ? C15 Ti C14 34.75(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -12.2(2) . . . . ? C1 C2 C3 C4 14.4(2) . . . . ? C2 C3 C4 N1 -12.54(19) . . . . ? C2 C3 C4 N2 161.74(17) . . . . ? C10 C5 C6 C7 -0.3(2) . . . . ? N2 C5 C6 C7 -177.16(12) . . . . ? C5 C6 C7 C8 -1.1(2) . . . . ? C5 C6 C7 C11 178.49(13) . . . . ? C6 C7 C8 C9 1.2(2) . . . . ? C11 C7 C8 C9 -178.39(13) . . . . ? C7 C8 C9 C10 0.1(2) . . . . ? C7 C8 C9 C12 178.45(14) . . . . ? C6 C5 C10 C9 1.7(2) . . . . ? N2 C5 C10 C9 178.40(12) . . . . ? C8 C9 C10 C5 -1.6(2) . . . . ? C12 C9 C10 C5 -179.91(13) . . . . ? C17 C13 C14 C15 -0.45(14) . . . . ? C18 C13 C14 C15 -178.61(13) . . . . ? Ti C13 C14 C15 63.96(9) . . . . ? C17 C13 C14 C19 171.20(12) . . . . ? C18 C13 C14 C19 -7.0(2) . . . . ? Ti C13 C14 C19 -124.39(13) . . . . ? C17 C13 C14 Ti -64.41(9) . . . . ? C18 C13 C14 Ti 117.43(13) . . . . ? C13 C14 C15 C16 0.49(14) . . . . ? C19 C14 C15 C16 -171.19(12) . . . . ? Ti C14 C15 C16 64.39(9) . . . . ? C13 C14 C15 C20 173.87(12) . . . . ? C19 C14 C15 C20 2.2(2) . . . . ? Ti C14 C15 C20 -122.23(13) . . . . ? C13 C14 C15 Ti -63.90(9) . . . . ? C19 C14 C15 Ti 124.41(13) . . . . ? C14 C15 C16 C17 -0.35(15) . . . . ? C20 C15 C16 C17 -173.64(13) . . . . ? Ti C15 C16 C17 64.42(9) . . . . ? C14 C15 C16 C21 176.48(12) . . . . ? C20 C15 C16 C21 3.2(2) . . . . ? Ti C15 C16 C21 -118.75(13) . . . . ? C14 C15 C16 Ti -64.77(9) . . . . ? C20 C15 C16 Ti 121.94(14) . . . . ? C14 C13 C17 C16 0.23(15) . . . . ? C18 C13 C17 C16 178.39(12) . . . . ? Ti C13 C17 C16 -64.61(10) . . . . ? C14 C13 C17 C22 -179.04(13) . . . . ? C18 C13 C17 C22 -0.9(2) . . . . ? Ti C13 C17 C22 116.12(14) . . . . ? C14 C13 C17 Ti 64.84(9) . . . . ? C18 C13 C17 Ti -117.00(14) . . . . ? C15 C16 C17 C13 0.08(15) . . . . ? C21 C16 C17 C13 -176.72(13) . . . . ? Ti C16 C17 C13 64.77(9) . . . . ? C15 C16 C17 C22 179.33(13) . . . . ? C21 C16 C17 C22 2.5(2) . . . . ? Ti C16 C17 C22 -115.98(14) . . . . ? C15 C16 C17 Ti -64.69(9) . . . . ? C21 C16 C17 Ti 118.51(14) . . . . ? N2 C4 N1 C1 -170.17(12) . . . . ? C3 C4 N1 C1 5.26(17) . . . . ? N2 C4 N1 Ti -11.82(12) . . . . ? C3 C4 N1 Ti 163.61(11) . . . . ? C2 C1 N1 C4 4.55(18) . . . . ? C2 C1 N1 Ti -131.59(17) . . . . ? N1 C4 N2 C5 -170.53(12) . . . . ? C3 C4 N2 C5 15.2(2) . . . . ? N1 C4 N2 Ti 11.44(12) . . . . ? C3 C4 N2 Ti -162.81(16) . . . . ? C10 C5 N2 C4 39.50(19) . . . . ? C6 C5 N2 C4 -143.80(13) . . . . ? C10 C5 N2 Ti -144.11(14) . . . . ? C6 C5 N2 Ti 32.6(2) . . . . ? C4 N1 Ti C24 -58.06(11) . . . . ? C1 N1 Ti C24 81.5(2) . . . . ? C4 N1 Ti C23 -138.88(9) . . . . ? C1 N1 Ti C23 0.71(19) . . . . ? C4 N1 Ti N2 7.42(8) . . . . ? C1 N1 Ti N2 147.0(2) . . . . ? C4 N1 Ti C17 92.02(9) . . . . ? C1 N1 Ti C17 -128.39(19) . . . . ? C4 N1 Ti C16 76.68(10) . . . . ? C1 N1 Ti C16 -143.73(18) . . . . ? C4 N1 Ti C13 126.70(9) . . . . ? C1 N1 Ti C13 -93.72(19) . . . . ? C4 N1 Ti C15 115.89(10) . . . . ? C1 N1 Ti C15 -104.5(2) . . . . ? C4 N1 Ti C14 146.06(8) . . . . ? C1 N1 Ti C14 -74.4(2) . . . . ? C4 N2 Ti N1 -7.32(8) . . . . ? C5 N2 Ti N1 175.71(18) . . . . ? C4 N2 Ti C24 127.35(9) . . . . ? C5 N2 Ti C24 -49.62(17) . . . . ? C4 N2 Ti C23 39.36(11) . . . . ? C5 N2 Ti C23 -137.62(16) . . . . ? C4 N2 Ti C17 -102.37(9) . . . . ? C5 N2 Ti C17 80.66(17) . . . . ? C4 N2 Ti C16 -137.04(9) . . . . ? C5 N2 Ti C16 45.99(17) . . . . ? C4 N2 Ti C13 -82.82(9) . . . . ? C5 N2 Ti C13 100.21(17) . . . . ? C4 N2 Ti C15 -149.84(8) . . . . ? C5 N2 Ti C15 33.19(19) . . . . ? C4 N2 Ti C14 -109.99(10) . . . . ? C5 N2 Ti C14 73.04(19) . . . . ? C13 C17 Ti N1 86.62(8) . . . . ? C16 C17 Ti N1 -157.65(8) . . . . ? C22 C17 Ti N1 -34.83(12) . . . . ? C13 C17 Ti C24 -124.09(9) . . . . ? C16 C17 Ti C24 -8.35(11) . . . . ? C22 C17 Ti C24 114.47(12) . . . . ? C13 C17 Ti C23 5.08(10) . . . . ? C16 C17 Ti C23 120.82(9) . . . . ? C22 C17 Ti C23 -116.36(12) . . . . ? C13 C17 Ti N2 148.06(8) . . . . ? C16 C17 Ti N2 -96.21(8) . . . . ? C22 C17 Ti N2 26.61(12) . . . . ? C13 C17 Ti C16 -115.74(11) . . . . ? C22 C17 Ti C16 122.82(15) . . . . ? C16 C17 Ti C13 115.74(11) . . . . ? C22 C17 Ti C13 -121.44(15) . . . . ? C13 C17 Ti C15 -78.55(8) . . . . ? C16 C17 Ti C15 37.19(7) . . . . ? C22 C17 Ti C15 160.01(13) . . . . ? C13 C17 Ti C14 -37.24(7) . . . . ? C16 C17 Ti C14 78.50(8) . . . . ? C22 C17 Ti C14 -158.68(13) . . . . ? C15 C16 Ti N1 143.50(8) . . . . ? C17 C16 Ti N1 27.51(9) . . . . ? C21 C16 Ti N1 -94.86(13) . . . . ? C15 C16 Ti C24 -70.40(9) . . . . ? C17 C16 Ti C24 173.60(8) . . . . ? C21 C16 Ti C24 51.24(13) . . . . ? C15 C16 Ti C23 23.03(12) . . . . ? C17 C16 Ti C23 -92.97(10) . . . . ? C21 C16 Ti C23 144.67(11) . . . . ? C15 C16 Ti N2 -161.05(8) . . . . ? C17 C16 Ti N2 82.96(8) . . . . ? C21 C16 Ti N2 -39.41(12) . . . . ? C15 C16 Ti C17 115.99(11) . . . . ? C21 C16 Ti C17 -122.37(15) . . . . ? C15 C16 Ti C13 78.67(8) . . . . ? C17 C16 Ti C13 -37.33(7) . . . . ? C21 C16 Ti C13 -159.69(13) . . . . ? C17 C16 Ti C15 -115.99(11) . . . . ? C21 C16 Ti C15 121.64(15) . . . . ? C15 C16 Ti C14 37.39(7) . . . . ? C17 C16 Ti C14 -78.61(8) . . . . ? C21 C16 Ti C14 159.03(14) . . . . ? C17 C13 Ti N1 -94.38(8) . . . . ? C14 C13 Ti N1 149.64(8) . . . . ? C18 C13 Ti N1 27.51(11) . . . . ? C17 C13 Ti C24 91.50(11) . . . . ? C14 C13 Ti C24 -24.47(12) . . . . ? C18 C13 Ti C24 -146.61(11) . . . . ? C17 C13 Ti C23 -176.05(8) . . . . ? C14 C13 Ti C23 67.98(9) . . . . ? C18 C13 Ti C23 -54.15(12) . . . . ? C17 C13 Ti N2 -35.89(9) . . . . ? C14 C13 Ti N2 -151.86(7) . . . . ? C18 C13 Ti N2 86.01(11) . . . . ? C14 C13 Ti C17 -115.97(11) . . . . ? C18 C13 Ti C17 121.89(14) . . . . ? C17 C13 Ti C16 37.51(8) . . . . ? C14 C13 Ti C16 -78.46(8) . . . . ? C18 C13 Ti C16 159.40(12) . . . . ? C17 C13 Ti C15 78.80(9) . . . . ? C14 C13 Ti C15 -37.17(7) . . . . ? C18 C13 Ti C15 -159.30(13) . . . . ? C17 C13 Ti C14 115.97(11) . . . . ? C18 C13 Ti C14 -122.13(14) . . . . ? C16 C15 Ti N1 -65.86(12) . . . . ? C14 C15 Ti N1 49.90(12) . . . . ? C20 C15 Ti N1 171.55(10) . . . . ? C16 C15 Ti C24 109.39(9) . . . . ? C14 C15 Ti C24 -134.85(8) . . . . ? C20 C15 Ti C24 -13.20(12) . . . . ? C16 C15 Ti C23 -164.30(8) . . . . ? C14 C15 Ti C23 -48.54(9) . . . . ? C20 C15 Ti C23 73.11(12) . . . . ? C16 C15 Ti N2 22.87(9) . . . . ? C14 C15 Ti N2 138.64(7) . . . . ? C20 C15 Ti N2 -99.72(12) . . . . ? C16 C15 Ti C17 -37.37(8) . . . . ? C14 C15 Ti C17 78.39(8) . . . . ? C20 C15 Ti C17 -159.96(13) . . . . ? C14 C15 Ti C16 115.77(11) . . . . ? C20 C15 Ti C16 -122.59(15) . . . . ? C16 C15 Ti C13 -78.65(8) . . . . ? C14 C15 Ti C13 37.11(7) . . . . ? C20 C15 Ti C13 158.76(13) . . . . ? C16 C15 Ti C14 -115.77(11) . . . . ? C20 C15 Ti C14 121.64(15) . . . . ? C13 C14 Ti N1 -35.61(9) . . . . ? C15 C14 Ti N1 -151.80(7) . . . . ? C19 C14 Ti N1 86.51(12) . . . . ? C13 C14 Ti C24 164.01(8) . . . . ? C15 C14 Ti C24 47.82(9) . . . . ? C19 C14 Ti C24 -73.87(13) . . . . ? C13 C14 Ti C23 -110.81(9) . . . . ? C15 C14 Ti C23 132.99(9) . . . . ? C19 C14 Ti C23 11.31(12) . . . . ? C13 C14 Ti N2 46.29(11) . . . . ? C15 C14 Ti N2 -69.90(11) . . . . ? C19 C14 Ti N2 168.41(10) . . . . ? C13 C14 Ti C17 37.28(8) . . . . ? C15 C14 Ti C17 -78.91(8) . . . . ? C19 C14 Ti C17 159.40(13) . . . . ? C13 C14 Ti C16 78.83(8) . . . . ? C15 C14 Ti C16 -37.37(8) . . . . ? C19 C14 Ti C16 -159.05(13) . . . . ? C15 C14 Ti C13 -116.19(11) . . . . ? C19 C14 Ti C13 122.12(15) . . . . ? C13 C14 Ti C15 116.19(11) . . . . ? C19 C14 Ti C15 -121.68(15) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 30.62 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.364 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.055 _audit_block_code ga_kw3 _audit_block_refno 356 _chemical_absolute_configuration ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' #==end== data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 718800' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H41 N3 Ti' _chemical_formula_weight 503.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_int_tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.143(2) _cell_length_b 25.070(3) _cell_length_c 14.5813(18) _cell_angle_alpha 90.00 _cell_angle_beta 116.658(2) _cell_angle_gamma 90.00 _cell_volume 5600.4(12) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 0.329 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5941 _exptl_absorpt_correction_T_max 0.7464 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004-2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector (Bruker AXS Smart 1000)' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 57812 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 30.03 _reflns_number_total 8193 _reflns_number_gt 6171 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 1997-2003)' _computing_cell_refinement 'SAINT (Bruker AXS, 1997-2006)' _computing_data_reduction 'SAINT (Bruker AXS, 1997-2006)' _computing_structure_solution 'DIRDIF (Beurskens, 1999-2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+11.1074P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8193 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1136 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.08299(12) 0.25978(7) -0.05132(14) 0.0241(3) Uani 1 1 d . . . H1A H 0.1034 0.2839 0.0088 0.029 Uiso 1 1 calc R . . H1B H 0.0184 0.2582 -0.0835 0.029 Uiso 1 1 calc R . . C2 C 0.11415(12) 0.27957(8) -0.12797(16) 0.0307(4) Uani 1 1 d . . . H2A H 0.1538 0.3105 -0.0997 0.037 Uiso 1 1 calc R . . H2B H 0.0639 0.2906 -0.1927 0.037 Uiso 1 1 calc R . . C3 C 0.16253(11) 0.23258(7) -0.14709(13) 0.0217(3) Uani 1 1 d . . . H3A H 0.1310 0.2195 -0.2185 0.026 Uiso 1 1 calc R . . H3B H 0.2226 0.2428 -0.1331 0.026 Uiso 1 1 calc R . . C4 C 0.16317(10) 0.19120(6) -0.07167(12) 0.0173(3) Uani 1 1 d . . . C5 C 0.25322(10) 0.11579(7) -0.07822(13) 0.0201(3) Uani 1 1 d . . . C6 C 0.29597(11) 0.07083(7) -0.02065(14) 0.0234(3) Uani 1 1 d . . . H6 H 0.2893 0.0622 0.0389 0.028 Uiso 1 1 calc R . . C7 C 0.34786(11) 0.03850(7) -0.04801(15) 0.0271(4) Uani 1 1 d . . . C8 C 0.35777(12) 0.05186(8) -0.13501(16) 0.0298(4) Uani 1 1 d . . . H8 H 0.3932 0.0302 -0.1546 0.036 Uiso 1 1 calc R . . C9 C 0.31676(12) 0.09628(8) -0.19356(15) 0.0278(4) Uani 1 1 d . . . C10 C 0.26508(11) 0.12859(7) -0.16473(13) 0.0224(3) Uani 1 1 d . . . H10 H 0.2378 0.1594 -0.2040 0.027 Uiso 1 1 calc R . . C11 C 0.38950(14) -0.01070(8) 0.01432(19) 0.0382(5) Uani 1 1 d . . . H11A H 0.4042 -0.0041 0.0865 0.057 Uiso 1 1 calc R . . H11B H 0.4427 -0.0193 0.0082 0.057 Uiso 1 1 calc R . . H11C H 0.3486 -0.0407 -0.0112 0.057 Uiso 1 1 calc R . . C12 C 0.32493(15) 0.10927(9) -0.29011(17) 0.0375(5) Uani 1 1 d . . . H12A H 0.3643 0.0836 -0.2987 0.056 Uiso 1 1 calc R . . H12B H 0.3485 0.1454 -0.2848 0.056 Uiso 1 1 calc R . . H12C H 0.2673 0.1073 -0.3495 0.056 Uiso 1 1 calc R . . C13 C 0.29979(10) 0.16121(6) 0.28928(12) 0.0176(3) Uani 1 1 d . . . C14 C 0.37816(10) 0.13155(6) 0.33689(13) 0.0196(3) Uani 1 1 d . . . C15 C 0.43412(11) 0.14025(7) 0.44006(13) 0.0240(3) Uani 1 1 d . . . H15 H 0.4867 0.1203 0.4716 0.029 Uiso 1 1 calc R . . C16 C 0.41539(11) 0.17731(7) 0.49854(13) 0.0243(3) Uani 1 1 d . . . C17 C 0.33929(11) 0.20715(7) 0.45047(13) 0.0228(3) Uani 1 1 d . . . H17 H 0.3263 0.2331 0.4891 0.027 Uiso 1 1 calc R . . C18 C 0.28133(10) 0.20011(7) 0.34682(13) 0.0195(3) Uani 1 1 d . . . C19 C 0.39919(11) 0.09037(7) 0.27640(15) 0.0255(4) Uani 1 1 d . . . H19A H 0.4567 0.0749 0.3194 0.038 Uiso 1 1 calc R . . H19B H 0.3996 0.1072 0.2159 0.038 Uiso 1 1 calc R . . H19C H 0.3549 0.0621 0.2544 0.038 Uiso 1 1 calc R . . C20 C 0.47607(13) 0.18437(9) 0.61149(14) 0.0335(4) Uani 1 1 d . . . H20A H 0.4508 0.2102 0.6411 0.050 Uiso 1 1 calc R . . H20B H 0.5327 0.1975 0.6198 0.050 Uiso 1 1 calc R . . H20C H 0.4839 0.1500 0.6467 0.050 Uiso 1 1 calc R . . C21 C 0.19929(11) 0.23286(7) 0.29747(14) 0.0249(3) Uani 1 1 d . . . H21A H 0.2013 0.2615 0.3442 0.037 Uiso 1 1 calc R . . H21B H 0.1486 0.2100 0.2826 0.037 Uiso 1 1 calc R . . H21C H 0.1945 0.2484 0.2335 0.037 Uiso 1 1 calc R . . C22 C 0.01037(10) 0.10541(7) -0.03108(13) 0.0216(3) Uani 1 1 d . . . C23 C 0.06645(11) 0.06188(7) -0.01729(13) 0.0225(3) Uani 1 1 d . . . C24 C 0.11225(10) 0.05100(6) 0.08968(13) 0.0205(3) Uani 1 1 d . . . C25 C 0.08304(10) 0.08736(6) 0.14225(13) 0.0193(3) Uani 1 1 d . . . C26 C 0.02050(10) 0.12168(7) 0.06727(13) 0.0196(3) Uani 1 1 d . . . C27 C -0.04934(12) 0.13073(8) -0.13166(14) 0.0326(4) Uani 1 1 d . . . H27A H -0.0165 0.1389 -0.1702 0.049 Uiso 1 1 calc R . . H27B H -0.0735 0.1637 -0.1190 0.049 Uiso 1 1 calc R . . H27C H -0.0970 0.1061 -0.1714 0.049 Uiso 1 1 calc R . . C28 C 0.07307(14) 0.03058(8) -0.10133(16) 0.0354(4) Uani 1 1 d . . . H28A H 0.0260 0.0042 -0.1285 0.053 Uiso 1 1 calc R . . H28B H 0.1296 0.0123 -0.0739 0.053 Uiso 1 1 calc R . . H28C H 0.0680 0.0548 -0.1565 0.053 Uiso 1 1 calc R . . C29 C 0.17361(12) 0.00518(7) 0.13776(18) 0.0335(4) Uani 1 1 d . . . H29A H 0.1399 -0.0276 0.1298 0.050 Uiso 1 1 calc R . . H29B H 0.2095 0.0124 0.2109 0.050 Uiso 1 1 calc R . . H29C H 0.2114 0.0008 0.1040 0.050 Uiso 1 1 calc R . . C30 C 0.11192(12) 0.08741(8) 0.25571(13) 0.0273(4) Uani 1 1 d . . . H30A H 0.0812 0.0592 0.2730 0.041 Uiso 1 1 calc R . . H30B H 0.0985 0.1221 0.2764 0.041 Uiso 1 1 calc R . . H30C H 0.1750 0.0810 0.2920 0.041 Uiso 1 1 calc R . . C31 C -0.02767(12) 0.16700(8) 0.08579(16) 0.0295(4) Uani 1 1 d . . . H31A H -0.0259 0.1982 0.0462 0.044 Uiso 1 1 calc R . . H31B H -0.0001 0.1759 0.1590 0.044 Uiso 1 1 calc R . . H31C H -0.0885 0.1566 0.0643 0.044 Uiso 1 1 calc R . . N1 N 0.12015(9) 0.20666(5) -0.02019(11) 0.0187(3) Uani 1 1 d . . . N2 N 0.19956(9) 0.14283(6) -0.04480(11) 0.0202(3) Uani 1 1 d . . . N3 N 0.24227(8) 0.15289(5) 0.18745(10) 0.0171(3) Uani 1 1 d . . . Ti Ti 0.156334(17) 0.137421(11) 0.06919(2) 0.01464(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0284(8) 0.0178(7) 0.0252(9) 0.0021(6) 0.0113(7) 0.0025(6) C2 0.0236(8) 0.0347(10) 0.0366(10) 0.0180(8) 0.0159(8) 0.0097(7) C3 0.0252(8) 0.0221(8) 0.0173(7) 0.0003(6) 0.0091(6) -0.0060(6) C4 0.0144(6) 0.0213(7) 0.0139(7) -0.0005(5) 0.0043(5) -0.0027(5) C5 0.0159(7) 0.0240(8) 0.0206(8) -0.0062(6) 0.0084(6) -0.0042(6) C6 0.0196(7) 0.0266(8) 0.0249(8) -0.0037(6) 0.0109(7) -0.0002(6) C7 0.0181(8) 0.0280(9) 0.0339(10) -0.0105(7) 0.0106(7) -0.0013(6) C8 0.0217(8) 0.0331(9) 0.0402(11) -0.0194(8) 0.0190(8) -0.0081(7) C9 0.0253(8) 0.0339(9) 0.0305(9) -0.0171(7) 0.0182(8) -0.0151(7) C10 0.0210(7) 0.0261(8) 0.0219(8) -0.0082(6) 0.0113(6) -0.0084(6) C11 0.0311(10) 0.0326(10) 0.0514(13) -0.0035(9) 0.0190(10) 0.0102(8) C12 0.0448(12) 0.0428(12) 0.0388(11) -0.0183(9) 0.0312(10) -0.0154(9) C13 0.0138(6) 0.0198(7) 0.0177(7) 0.0035(6) 0.0059(6) -0.0020(5) C14 0.0149(7) 0.0192(7) 0.0227(8) 0.0050(6) 0.0066(6) -0.0017(5) C15 0.0151(7) 0.0248(8) 0.0250(8) 0.0086(6) 0.0026(6) -0.0034(6) C16 0.0191(7) 0.0298(9) 0.0182(8) 0.0044(6) 0.0031(6) -0.0079(6) C17 0.0223(8) 0.0262(8) 0.0193(8) -0.0005(6) 0.0088(7) -0.0050(6) C18 0.0162(7) 0.0228(7) 0.0181(7) 0.0029(6) 0.0064(6) -0.0016(6) C19 0.0199(8) 0.0227(8) 0.0315(9) 0.0041(7) 0.0094(7) 0.0029(6) C20 0.0254(9) 0.0451(11) 0.0203(9) 0.0053(8) 0.0016(7) -0.0094(8) C21 0.0222(8) 0.0298(9) 0.0222(8) 0.0005(7) 0.0095(7) 0.0043(6) C22 0.0156(7) 0.0254(8) 0.0195(8) 0.0033(6) 0.0041(6) -0.0029(6) C23 0.0206(7) 0.0225(8) 0.0239(8) -0.0044(6) 0.0095(6) -0.0056(6) C24 0.0164(7) 0.0165(7) 0.0261(8) 0.0029(6) 0.0072(6) -0.0011(5) C25 0.0170(7) 0.0208(7) 0.0200(7) 0.0038(6) 0.0083(6) -0.0024(6) C26 0.0147(7) 0.0220(7) 0.0227(8) 0.0045(6) 0.0087(6) 0.0005(5) C27 0.0240(8) 0.0388(11) 0.0227(9) 0.0080(7) -0.0006(7) -0.0058(7) C28 0.0363(10) 0.0352(10) 0.0349(11) -0.0170(8) 0.0161(9) -0.0104(8) C29 0.0242(9) 0.0203(8) 0.0522(13) 0.0087(8) 0.0139(9) 0.0037(7) C30 0.0264(8) 0.0354(10) 0.0205(8) 0.0080(7) 0.0110(7) -0.0031(7) C31 0.0249(9) 0.0297(9) 0.0401(11) 0.0067(8) 0.0201(8) 0.0068(7) N1 0.0182(6) 0.0199(6) 0.0187(6) 0.0033(5) 0.0087(5) 0.0015(5) N2 0.0205(6) 0.0234(7) 0.0192(6) 0.0013(5) 0.0112(5) 0.0029(5) N3 0.0151(6) 0.0188(6) 0.0171(6) 0.0018(5) 0.0071(5) -0.0007(5) Ti 0.01314(12) 0.01627(12) 0.01437(13) 0.00129(10) 0.00605(10) 0.00066(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.458(2) . ? C1 C2 1.522(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.537(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.508(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N1 1.324(2) . ? C4 N2 1.339(2) . ? C5 C10 1.402(2) . ? C5 N2 1.395(2) . ? C5 C6 1.400(2) . ? C6 C7 1.388(2) . ? C6 H6 0.9500 . ? C7 C8 1.394(3) . ? C7 C11 1.508(3) . ? C8 C9 1.387(3) . ? C8 H8 0.9500 . ? C9 C10 1.397(2) . ? C9 C12 1.512(3) . ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N3 1.381(2) . ? C13 C18 1.412(2) . ? C13 C14 1.415(2) . ? C14 C15 1.391(2) . ? C14 C19 1.503(2) . ? C15 C16 1.393(3) . ? C15 H15 0.9500 . ? C16 C17 1.390(2) . ? C16 C20 1.513(2) . ? C17 C18 1.398(2) . ? C17 H17 0.9500 . ? C18 C21 1.504(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.408(2) . ? C22 C26 1.425(2) . ? C22 C27 1.502(2) . ? C22 Ti 2.4000(16) . ? C23 C24 1.423(2) . ? C23 C28 1.502(3) . ? C23 Ti 2.4099(17) . ? C24 C25 1.419(2) . ? C24 C29 1.502(2) . ? C24 Ti 2.3574(16) . ? C25 C26 1.426(2) . ? C25 C30 1.499(2) . ? C25 Ti 2.3430(16) . ? C26 C31 1.499(2) . ? C26 Ti 2.3495(16) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N1 Ti 2.0907(14) . ? N2 Ti 2.1061(14) . ? N3 Ti 1.7363(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 106.14(14) . . ? N1 C1 H1A 110.5 . . ? C2 C1 H1A 110.5 . . ? N1 C1 H1B 110.5 . . ? C2 C1 H1B 110.5 . . ? H1A C1 H1B 108.7 . . ? C1 C2 C3 106.22(14) . . ? C1 C2 H2A 110.5 . . ? C3 C2 H2A 110.5 . . ? C1 C2 H2B 110.5 . . ? C3 C2 H2B 110.5 . . ? H2A C2 H2B 108.7 . . ? C4 C3 C2 102.88(14) . . ? C4 C3 H3A 111.2 . . ? C2 C3 H3A 111.2 . . ? C4 C3 H3B 111.2 . . ? C2 C3 H3B 111.2 . . ? H3A C3 H3B 109.1 . . ? N1 C4 N2 113.82(14) . . ? N1 C4 C3 112.85(14) . . ? N2 C4 C3 133.31(15) . . ? C10 C5 N2 125.99(16) . . ? C10 C5 C6 118.39(15) . . ? N2 C5 C6 115.57(15) . . ? C7 C6 C5 121.89(17) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C6 C7 C8 118.48(18) . . ? C6 C7 C11 119.70(18) . . ? C8 C7 C11 121.79(17) . . ? C9 C8 C7 121.18(16) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 119.67(17) . . ? C8 C9 C12 120.86(17) . . ? C10 C9 C12 119.44(19) . . ? C9 C10 C5 120.37(17) . . ? C9 C10 H10 119.8 . . ? C5 C10 H10 119.8 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C18 120.07(14) . . ? N3 C13 C14 120.72(15) . . ? C18 C13 C14 119.20(15) . . ? C15 C14 C13 119.36(16) . . ? C15 C14 C19 120.77(15) . . ? C13 C14 C19 119.86(15) . . ? C14 C15 C16 122.02(16) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C17 C16 C15 118.18(16) . . ? C17 C16 C20 121.16(18) . . ? C15 C16 C20 120.66(17) . . ? C16 C17 C18 121.88(17) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C17 C18 C13 119.31(15) . . ? C17 C18 C21 120.44(16) . . ? C13 C18 C21 120.24(15) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C26 108.13(14) . . ? C23 C22 C27 126.13(17) . . ? C26 C22 C27 125.74(16) . . ? C23 C22 Ti 73.36(9) . . ? C26 C22 Ti 70.62(9) . . ? C27 C22 Ti 121.41(12) . . ? C22 C23 C24 108.10(15) . . ? C22 C23 C28 125.82(17) . . ? C24 C23 C28 126.00(17) . . ? C22 C23 Ti 72.60(9) . . ? C24 C23 Ti 70.63(9) . . ? C28 C23 Ti 124.96(12) . . ? C25 C24 C23 108.30(14) . . ? C25 C24 C29 125.60(17) . . ? C23 C24 C29 125.79(17) . . ? C25 C24 Ti 71.88(9) . . ? C23 C24 Ti 74.66(9) . . ? C29 C24 Ti 124.39(11) . . ? C24 C25 C26 107.44(14) . . ? C24 C25 C30 125.09(15) . . ? C26 C25 C30 127.45(16) . . ? C24 C25 Ti 72.98(9) . . ? C26 C25 Ti 72.56(9) . . ? C30 C25 Ti 121.49(11) . . ? C22 C26 C25 108.02(15) . . ? C22 C26 C31 124.77(15) . . ? C25 C26 C31 127.22(16) . . ? C22 C26 Ti 74.49(9) . . ? C25 C26 Ti 72.06(9) . . ? C31 C26 Ti 119.58(12) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C4 N1 C1 111.55(14) . . ? C4 N1 Ti 91.46(10) . . ? C1 N1 Ti 156.69(12) . . ? C4 N2 C5 129.16(15) . . ? C4 N2 Ti 90.37(10) . . ? C5 N2 Ti 139.92(12) . . ? C13 N3 Ti 168.52(12) . . ? N3 Ti N1 108.41(6) . . ? N3 Ti N2 109.10(6) . . ? N1 Ti N2 64.25(5) . . ? N3 Ti C25 93.29(6) . . ? N1 Ti C25 131.19(6) . . ? N2 Ti C25 147.52(6) . . ? N3 Ti C26 116.37(6) . . ? N1 Ti C26 96.71(5) . . ? N2 Ti C26 134.36(6) . . ? C25 Ti C26 35.38(5) . . ? N3 Ti C24 104.88(6) . . ? N1 Ti C24 145.06(6) . . ? N2 Ti C24 113.92(6) . . ? C25 Ti C24 35.14(6) . . ? C26 Ti C24 58.32(6) . . ? N3 Ti C22 150.21(6) . . ? N1 Ti C22 87.78(6) . . ? N2 Ti C22 100.40(6) . . ? C25 Ti C22 58.17(6) . . ? C26 Ti C22 34.89(6) . . ? C24 Ti C22 57.59(6) . . ? N3 Ti C23 138.91(6) . . ? N1 Ti C23 112.65(6) . . ? N2 Ti C23 90.36(6) . . ? C25 Ti C23 57.96(6) . . ? C26 Ti C23 57.60(6) . . ? C24 Ti C23 34.71(6) . . ? C22 Ti C23 34.04(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 5.92(19) . . . . ? C1 C2 C3 C4 -5.49(18) . . . . ? C2 C3 C4 N1 3.31(18) . . . . ? C2 C3 C4 N2 -175.10(17) . . . . ? C10 C5 C6 C7 -1.2(2) . . . . ? N2 C5 C6 C7 176.65(15) . . . . ? C5 C6 C7 C8 0.5(3) . . . . ? C5 C6 C7 C11 -177.54(17) . . . . ? C6 C7 C8 C9 -0.2(3) . . . . ? C11 C7 C8 C9 177.85(17) . . . . ? C7 C8 C9 C10 0.5(3) . . . . ? C7 C8 C9 C12 -177.56(17) . . . . ? C8 C9 C10 C5 -1.2(2) . . . . ? C12 C9 C10 C5 176.91(16) . . . . ? N2 C5 C10 C9 -176.09(15) . . . . ? C6 C5 C10 C9 1.5(2) . . . . ? N3 C13 C14 C15 -178.99(14) . . . . ? C18 C13 C14 C15 1.8(2) . . . . ? N3 C13 C14 C19 -0.2(2) . . . . ? C18 C13 C14 C19 -179.40(15) . . . . ? C13 C14 C15 C16 0.2(2) . . . . ? C19 C14 C15 C16 -178.59(16) . . . . ? C14 C15 C16 C17 -1.7(2) . . . . ? C14 C15 C16 C20 177.78(16) . . . . ? C15 C16 C17 C18 1.2(2) . . . . ? C20 C16 C17 C18 -178.25(16) . . . . ? C16 C17 C18 C13 0.8(2) . . . . ? C16 C17 C18 C21 179.62(16) . . . . ? N3 C13 C18 C17 178.53(14) . . . . ? C14 C13 C18 C17 -2.3(2) . . . . ? N3 C13 C18 C21 -0.3(2) . . . . ? C14 C13 C18 C21 178.87(15) . . . . ? C26 C22 C23 C24 -0.39(18) . . . . ? C27 C22 C23 C24 179.17(16) . . . . ? Ti C22 C23 C24 62.08(11) . . . . ? C26 C22 C23 C28 176.58(17) . . . . ? C27 C22 C23 C28 -3.9(3) . . . . ? Ti C22 C23 C28 -120.95(18) . . . . ? C26 C22 C23 Ti -62.47(11) . . . . ? C27 C22 C23 Ti 117.09(17) . . . . ? C22 C23 C24 C25 1.15(18) . . . . ? C28 C23 C24 C25 -175.81(16) . . . . ? Ti C23 C24 C25 64.50(11) . . . . ? C22 C23 C24 C29 175.02(16) . . . . ? C28 C23 C24 C29 -1.9(3) . . . . ? Ti C23 C24 C29 -121.62(17) . . . . ? C22 C23 C24 Ti -63.35(12) . . . . ? C28 C23 C24 Ti 119.69(17) . . . . ? C23 C24 C25 C26 -1.46(18) . . . . ? C29 C24 C25 C26 -175.35(15) . . . . ? Ti C24 C25 C26 64.87(11) . . . . ? C23 C24 C25 C30 176.76(15) . . . . ? C29 C24 C25 C30 2.9(3) . . . . ? Ti C24 C25 C30 -116.91(16) . . . . ? C23 C24 C25 Ti -66.33(11) . . . . ? C29 C24 C25 Ti 119.78(16) . . . . ? C23 C22 C26 C25 -0.52(18) . . . . ? C27 C22 C26 C25 179.92(16) . . . . ? Ti C22 C26 C25 -64.76(11) . . . . ? C23 C22 C26 C31 179.78(16) . . . . ? C27 C22 C26 C31 0.2(3) . . . . ? Ti C22 C26 C31 115.54(16) . . . . ? C23 C22 C26 Ti 64.25(11) . . . . ? C27 C22 C26 Ti -115.31(17) . . . . ? C24 C25 C26 C22 1.22(18) . . . . ? C30 C25 C26 C22 -176.94(16) . . . . ? Ti C25 C26 C22 66.37(11) . . . . ? C24 C25 C26 C31 -179.09(16) . . . . ? C30 C25 C26 C31 2.7(3) . . . . ? Ti C25 C26 C31 -113.94(17) . . . . ? C24 C25 C26 Ti -65.15(11) . . . . ? C30 C25 C26 Ti 116.68(17) . . . . ? N2 C4 N1 C1 179.17(14) . . . . ? C3 C4 N1 C1 0.44(19) . . . . ? N2 C4 N1 Ti 2.95(14) . . . . ? C3 C4 N1 Ti -175.78(11) . . . . ? C2 C1 N1 C4 -4.08(19) . . . . ? C2 C1 N1 Ti 166.3(2) . . . . ? N1 C4 N2 C5 -175.74(15) . . . . ? C3 C4 N2 C5 2.6(3) . . . . ? N1 C4 N2 Ti -2.93(14) . . . . ? C3 C4 N2 Ti 175.47(16) . . . . ? C10 C5 N2 C4 -15.3(3) . . . . ? C6 C5 N2 C4 167.00(16) . . . . ? C10 C5 N2 Ti 175.86(13) . . . . ? C6 C5 N2 Ti -1.8(2) . . . . ? C18 C13 N3 Ti -68.5(6) . . . . ? C14 C13 N3 Ti 112.3(6) . . . . ? C13 N3 Ti N1 123.6(6) . . . . ? C13 N3 Ti N2 -168.1(6) . . . . ? C13 N3 Ti C25 -12.0(6) . . . . ? C13 N3 Ti C26 16.0(6) . . . . ? C13 N3 Ti C24 -45.7(6) . . . . ? C13 N3 Ti C22 3.6(7) . . . . ? C13 N3 Ti C23 -54.0(6) . . . . ? C4 N1 Ti N3 100.94(10) . . . . ? C1 N1 Ti N3 -70.2(3) . . . . ? C4 N1 Ti N2 -1.90(9) . . . . ? C1 N1 Ti N2 -173.0(3) . . . . ? C4 N1 Ti C25 -147.25(9) . . . . ? C1 N1 Ti C25 41.7(3) . . . . ? C4 N1 Ti C26 -138.36(10) . . . . ? C1 N1 Ti C26 50.5(3) . . . . ? C4 N1 Ti C24 -97.39(13) . . . . ? C1 N1 Ti C24 91.5(3) . . . . ? C4 N1 Ti C22 -104.57(10) . . . . ? C1 N1 Ti C22 84.3(3) . . . . ? C4 N1 Ti C23 -80.74(10) . . . . ? C1 N1 Ti C23 108.2(3) . . . . ? C4 N2 Ti N3 -99.89(10) . . . . ? C5 N2 Ti N3 71.44(18) . . . . ? C4 N2 Ti N1 1.88(9) . . . . ? C5 N2 Ti N1 173.22(19) . . . . ? C4 N2 Ti C25 129.03(11) . . . . ? C5 N2 Ti C25 -59.6(2) . . . . ? C4 N2 Ti C26 75.01(12) . . . . ? C5 N2 Ti C26 -113.65(17) . . . . ? C4 N2 Ti C24 143.30(9) . . . . ? C5 N2 Ti C24 -45.36(18) . . . . ? C4 N2 Ti C22 84.28(10) . . . . ? C5 N2 Ti C22 -104.38(17) . . . . ? C4 N2 Ti C23 117.00(10) . . . . ? C5 N2 Ti C23 -71.66(17) . . . . ? C24 C25 Ti N3 -111.43(10) . . . . ? C26 C25 Ti N3 133.44(10) . . . . ? C30 C25 Ti N3 9.73(14) . . . . ? C24 C25 Ti N1 130.49(10) . . . . ? C26 C25 Ti N1 15.37(13) . . . . ? C30 C25 Ti N1 -108.35(14) . . . . ? C24 C25 Ti N2 23.04(15) . . . . ? C26 C25 Ti N2 -92.08(13) . . . . ? C30 C25 Ti N2 144.20(13) . . . . ? C24 C25 Ti C26 115.13(14) . . . . ? C30 C25 Ti C26 -123.71(18) . . . . ? C26 C25 Ti C24 -115.13(14) . . . . ? C30 C25 Ti C24 121.16(18) . . . . ? C24 C25 Ti C22 77.63(10) . . . . ? C26 C25 Ti C22 -37.49(10) . . . . ? C30 C25 Ti C22 -161.20(16) . . . . ? C24 C25 Ti C23 37.28(9) . . . . ? C26 C25 Ti C23 -77.84(11) . . . . ? C30 C25 Ti C23 158.44(16) . . . . ? C22 C26 Ti N3 -169.30(9) . . . . ? C25 C26 Ti N3 -54.01(11) . . . . ? C31 C26 Ti N3 69.17(15) . . . . ? C22 C26 Ti N1 76.29(10) . . . . ? C25 C26 Ti N1 -168.42(10) . . . . ? C31 C26 Ti N1 -45.24(14) . . . . ? C22 C26 Ti N2 16.08(13) . . . . ? C25 C26 Ti N2 131.37(10) . . . . ? C31 C26 Ti N2 -105.45(14) . . . . ? C22 C26 Ti C25 -115.29(14) . . . . ? C31 C26 Ti C25 123.18(18) . . . . ? C22 C26 Ti C24 -77.52(10) . . . . ? C25 C26 Ti C24 37.76(10) . . . . ? C31 C26 Ti C24 160.94(16) . . . . ? C25 C26 Ti C22 115.29(14) . . . . ? C31 C26 Ti C22 -121.53(17) . . . . ? C22 C26 Ti C23 -36.32(9) . . . . ? C25 C26 Ti C23 78.97(11) . . . . ? C31 C26 Ti C23 -157.86(16) . . . . ? C25 C24 Ti N3 74.07(10) . . . . ? C23 C24 Ti N3 -170.32(10) . . . . ? C29 C24 Ti N3 -47.15(17) . . . . ? C25 C24 Ti N1 -87.94(13) . . . . ? C23 C24 Ti N1 27.67(16) . . . . ? C29 C24 Ti N1 150.84(15) . . . . ? C25 C24 Ti N2 -166.71(9) . . . . ? C23 C24 Ti N2 -51.09(11) . . . . ? C29 C24 Ti N2 72.07(17) . . . . ? C23 C24 Ti C25 115.62(14) . . . . ? C29 C24 Ti C25 -121.2(2) . . . . ? C25 C24 Ti C26 -38.02(9) . . . . ? C23 C24 Ti C26 77.59(11) . . . . ? C29 C24 Ti C26 -159.24(18) . . . . ? C25 C24 Ti C22 -79.44(10) . . . . ? C23 C24 Ti C22 36.18(10) . . . . ? C29 C24 Ti C22 159.35(18) . . . . ? C25 C24 Ti C23 -115.62(14) . . . . ? C29 C24 Ti C23 123.2(2) . . . . ? C23 C22 Ti N3 -97.13(15) . . . . ? C26 C22 Ti N3 19.57(17) . . . . ? C27 C22 Ti N3 140.28(15) . . . . ? C23 C22 Ti N1 138.23(11) . . . . ? C26 C22 Ti N1 -105.07(10) . . . . ? C27 C22 Ti N1 15.64(15) . . . . ? C23 C22 Ti N2 74.91(11) . . . . ? C26 C22 Ti N2 -168.39(9) . . . . ? C27 C22 Ti N2 -47.67(16) . . . . ? C23 C22 Ti C25 -78.66(11) . . . . ? C26 C22 Ti C25 38.03(9) . . . . ? C27 C22 Ti C25 158.75(18) . . . . ? C23 C22 Ti C26 -116.70(14) . . . . ? C27 C22 Ti C26 120.71(19) . . . . ? C23 C22 Ti C24 -36.91(10) . . . . ? C26 C22 Ti C24 79.79(10) . . . . ? C27 C22 Ti C24 -159.49(18) . . . . ? C26 C22 Ti C23 116.70(14) . . . . ? C27 C22 Ti C23 -122.6(2) . . . . ? C22 C23 Ti N3 131.41(11) . . . . ? C24 C23 Ti N3 14.32(15) . . . . ? C28 C23 Ti N3 -106.64(17) . . . . ? C22 C23 Ti N1 -46.16(11) . . . . ? C24 C23 Ti N1 -163.25(9) . . . . ? C28 C23 Ti N1 75.79(17) . . . . ? C22 C23 Ti N2 -108.25(10) . . . . ? C24 C23 Ti N2 134.66(10) . . . . ? C28 C23 Ti N2 13.70(16) . . . . ? C22 C23 Ti C25 79.34(11) . . . . ? C24 C23 Ti C25 -37.75(10) . . . . ? C28 C23 Ti C25 -158.71(18) . . . . ? C22 C23 Ti C26 37.24(10) . . . . ? C24 C23 Ti C26 -79.85(11) . . . . ? C28 C23 Ti C26 159.19(18) . . . . ? C22 C23 Ti C24 117.09(15) . . . . ? C28 C23 Ti C24 -121.0(2) . . . . ? C24 C23 Ti C22 -117.09(15) . . . . ? C28 C23 Ti C22 122.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.501 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.067 _audit_block_code 692 _audit_block_refno ga_kw18 _chemical_absolute_configuration ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' #==end== data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 718801' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H47 N3 Ti' _chemical_formula_weight 545.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0565(4) _cell_length_b 10.2565(5) _cell_length_c 18.9495(10) _cell_angle_alpha 86.2970(10) _cell_angle_beta 84.8290(10) _cell_angle_gamma 79.4270(10) _cell_volume 1531.13(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 0.306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6805 _exptl_absorpt_correction_T_max 0.7464 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37750 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 31.00 _reflns_number_total 9660 _reflns_number_gt 7528 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'DIRDIF (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+0.2630P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9660 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1255 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0121(3) -0.10290(17) 0.38118(9) 0.0313(4) Uani 1 1 d . . . H1A H -0.1257 -0.0517 0.3949 0.038 Uiso 1 1 calc R . . H1B H 0.0492 -0.1276 0.4244 0.038 Uiso 1 1 calc R . . C2 C -0.0268(3) -0.22521(17) 0.34376(10) 0.0353(4) Uani 1 1 d . . . H2A H -0.1472 -0.2338 0.3438 0.042 Uiso 1 1 calc R . . H2B H 0.0345 -0.3056 0.3682 0.042 Uiso 1 1 calc R . . C3 C 0.0497(3) -0.21028(17) 0.26869(10) 0.0360(4) Uani 1 1 d . . . H3A H 0.1438 -0.2847 0.2577 0.043 Uiso 1 1 calc R . . H3B H -0.0364 -0.2057 0.2341 0.043 Uiso 1 1 calc R . . C4 C 0.11297(18) -0.08118(13) 0.26852(7) 0.0176(3) Uani 1 1 d . . . C5 C 0.23063(18) -0.05193(13) 0.14728(7) 0.0168(3) Uani 1 1 d . . . C6 C 0.1998(2) 0.04202(14) 0.09128(8) 0.0211(3) Uani 1 1 d . . . H6 H 0.1468 0.1303 0.1011 0.025 Uiso 1 1 calc R . . C7 C 0.2451(2) 0.00894(15) 0.02136(8) 0.0227(3) Uani 1 1 d . . . C8 C 0.32529(19) -0.12067(15) 0.00782(8) 0.0218(3) Uani 1 1 d . . . H8 H 0.3562 -0.1446 -0.0398 0.026 Uiso 1 1 calc R . . C9 C 0.36062(18) -0.21535(14) 0.06293(8) 0.0193(3) Uani 1 1 d . . . C10 C 0.31334(18) -0.18063(14) 0.13244(8) 0.0184(3) Uani 1 1 d . . . H10 H 0.3374 -0.2448 0.1703 0.022 Uiso 1 1 calc R . . C11 C 0.2066(3) 0.11000(18) -0.03888(9) 0.0352(4) Uani 1 1 d . . . H11A H 0.1035 0.0971 -0.0593 0.053 Uiso 1 1 calc R . . H11B H 0.3015 0.0991 -0.0754 0.053 Uiso 1 1 calc R . . H11C H 0.1895 0.1995 -0.0211 0.053 Uiso 1 1 calc R . . C12 C 0.4521(2) -0.35384(15) 0.04720(9) 0.0263(3) Uani 1 1 d . . . H12A H 0.3802 -0.3983 0.0214 0.039 Uiso 1 1 calc R . . H12B H 0.4775 -0.4043 0.0918 0.039 Uiso 1 1 calc R . . H12C H 0.5580 -0.3488 0.0182 0.039 Uiso 1 1 calc R . . C13 C -0.12450(16) 0.38820(13) 0.27386(7) 0.0141(2) Uani 1 1 d . . . C14 C -0.14319(17) 0.46675(13) 0.20974(7) 0.0160(2) Uani 1 1 d . . . C15 C -0.26279(19) 0.58364(14) 0.20916(8) 0.0206(3) Uani 1 1 d . . . H15 H -0.2757 0.6368 0.1664 0.025 Uiso 1 1 calc R . . C16 C -0.36342(19) 0.62377(14) 0.27003(9) 0.0227(3) Uani 1 1 d . . . H16 H -0.4474 0.7019 0.2683 0.027 Uiso 1 1 calc R . . C17 C -0.34095(18) 0.54947(14) 0.33332(8) 0.0202(3) Uani 1 1 d . . . H17 H -0.4082 0.5788 0.3750 0.024 Uiso 1 1 calc R . . C18 C -0.22182(17) 0.43286(13) 0.33698(7) 0.0162(2) Uani 1 1 d . . . C19 C -0.03900(18) 0.41943(14) 0.14263(7) 0.0182(3) Uani 1 1 d . . . H19 H 0.0623 0.3547 0.1571 0.022 Uiso 1 1 calc R . . C20 C -0.1413(2) 0.34521(17) 0.10020(8) 0.0255(3) Uani 1 1 d . . . H20A H -0.1714 0.2689 0.1290 0.038 Uiso 1 1 calc R . . H20B H -0.0733 0.3141 0.0570 0.038 Uiso 1 1 calc R . . H20C H -0.2448 0.4050 0.0873 0.038 Uiso 1 1 calc R . . C21 C 0.0254(3) 0.53108(18) 0.09703(9) 0.0326(4) Uani 1 1 d . . . H21A H -0.0704 0.5899 0.0767 0.049 Uiso 1 1 calc R . . H21B H 0.1059 0.4930 0.0587 0.049 Uiso 1 1 calc R . . H21C H 0.0818 0.5820 0.1265 0.049 Uiso 1 1 calc R . . C22 C -0.19368(18) 0.35229(15) 0.40612(7) 0.0180(3) Uani 1 1 d . . . H22 H -0.0733 0.3050 0.4025 0.022 Uiso 1 1 calc R . . C23 C -0.3039(3) 0.2461(2) 0.41585(10) 0.0363(4) Uani 1 1 d . . . H23A H -0.4231 0.2883 0.4234 0.054 Uiso 1 1 calc R . . H23B H -0.2716 0.1872 0.4571 0.054 Uiso 1 1 calc R . . H23C H -0.2881 0.1942 0.3733 0.054 Uiso 1 1 calc R . . C24 C -0.2160(2) 0.43633(19) 0.47100(9) 0.0323(4) Uani 1 1 d . . . H24A H -0.1470 0.5060 0.4627 0.048 Uiso 1 1 calc R . . H24B H -0.1798 0.3798 0.5125 0.048 Uiso 1 1 calc R . . H24C H -0.3354 0.4771 0.4795 0.048 Uiso 1 1 calc R . . C25 C 0.31791(17) 0.18223(15) 0.38001(7) 0.0178(3) Uani 1 1 d . . . C26 C 0.30797(17) 0.29541(13) 0.33253(7) 0.0160(2) Uani 1 1 d . . . C27 C 0.39750(17) 0.25408(13) 0.26717(7) 0.0155(2) Uani 1 1 d . . . C28 C 0.46778(17) 0.11657(14) 0.27579(7) 0.0169(3) Uani 1 1 d . . . C29 C 0.41864(17) 0.07236(14) 0.34519(7) 0.0175(3) Uani 1 1 d . . . C30 C 0.2451(2) 0.17797(19) 0.45588(8) 0.0286(3) Uani 1 1 d . . . H30A H 0.3367 0.1689 0.4875 0.043 Uiso 1 1 calc R . . H30B H 0.1866 0.1020 0.4645 0.043 Uiso 1 1 calc R . . H30C H 0.1646 0.2602 0.4650 0.043 Uiso 1 1 calc R . . C31 C 0.22774(19) 0.43528(15) 0.34764(9) 0.0238(3) Uani 1 1 d . . . H31A H 0.1488 0.4355 0.3901 0.036 Uiso 1 1 calc R . . H31B H 0.1661 0.4760 0.3072 0.036 Uiso 1 1 calc R . . H31C H 0.3158 0.4860 0.3555 0.036 Uiso 1 1 calc R . . C32 C 0.4246(2) 0.34340(16) 0.20296(8) 0.0236(3) Uani 1 1 d . . . H32A H 0.5268 0.3810 0.2065 0.035 Uiso 1 1 calc R . . H32B H 0.3266 0.4154 0.2001 0.035 Uiso 1 1 calc R . . H32C H 0.4383 0.2922 0.1603 0.035 Uiso 1 1 calc R . . C33 C 0.5822(2) 0.03642(16) 0.22125(9) 0.0257(3) Uani 1 1 d . . . H33A H 0.6975 0.0543 0.2217 0.039 Uiso 1 1 calc R . . H33B H 0.5414 0.0610 0.1742 0.039 Uiso 1 1 calc R . . H33C H 0.5825 -0.0583 0.2323 0.039 Uiso 1 1 calc R . . C34 C 0.4656(2) -0.06513(17) 0.37792(10) 0.0304(4) Uani 1 1 d . . . H34A H 0.4482 -0.1301 0.3449 0.046 Uiso 1 1 calc R . . H34B H 0.3943 -0.0741 0.4221 0.046 Uiso 1 1 calc R . . H34C H 0.5848 -0.0810 0.3882 0.046 Uiso 1 1 calc R . . N1 N 0.08160(16) -0.02541(11) 0.33073(6) 0.0176(2) Uani 1 1 d . . . N2 N 0.18388(16) -0.01051(11) 0.21676(6) 0.0176(2) Uani 1 1 d . . . N3 N -0.01157(14) 0.26975(11) 0.27517(6) 0.0144(2) Uani 1 1 d . . . Ti Ti 0.16341(3) 0.14533(2) 0.286612(12) 0.01165(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0449(10) 0.0270(8) 0.0245(8) 0.0023(6) 0.0080(7) -0.0198(7) C2 0.0463(11) 0.0214(8) 0.0393(10) -0.0043(7) 0.0142(8) -0.0165(7) C3 0.0611(12) 0.0225(8) 0.0295(9) -0.0050(6) 0.0054(8) -0.0243(8) C4 0.0221(7) 0.0124(6) 0.0184(6) -0.0004(5) -0.0024(5) -0.0028(5) C5 0.0207(6) 0.0146(6) 0.0153(6) -0.0042(5) -0.0003(5) -0.0027(5) C6 0.0285(7) 0.0142(6) 0.0180(6) -0.0019(5) 0.0027(5) 0.0011(5) C7 0.0294(8) 0.0201(7) 0.0164(6) -0.0008(5) 0.0022(5) -0.0008(6) C8 0.0258(7) 0.0228(7) 0.0158(6) -0.0064(5) 0.0015(5) -0.0016(6) C9 0.0204(6) 0.0160(6) 0.0211(7) -0.0076(5) -0.0031(5) 0.0010(5) C10 0.0229(7) 0.0138(6) 0.0181(6) -0.0031(5) -0.0036(5) -0.0004(5) C11 0.0509(11) 0.0283(8) 0.0194(7) 0.0044(6) 0.0056(7) 0.0051(8) C12 0.0292(8) 0.0194(7) 0.0285(8) -0.0108(6) -0.0031(6) 0.0043(6) C13 0.0134(6) 0.0129(5) 0.0169(6) -0.0014(5) -0.0038(4) -0.0033(4) C14 0.0168(6) 0.0141(6) 0.0176(6) 0.0013(5) -0.0042(5) -0.0036(5) C15 0.0234(7) 0.0145(6) 0.0246(7) 0.0025(5) -0.0077(6) -0.0032(5) C16 0.0208(7) 0.0143(6) 0.0326(8) -0.0038(6) -0.0075(6) 0.0015(5) C17 0.0177(6) 0.0192(6) 0.0235(7) -0.0071(5) -0.0015(5) -0.0009(5) C18 0.0153(6) 0.0167(6) 0.0177(6) -0.0034(5) -0.0028(5) -0.0039(5) C19 0.0199(6) 0.0188(6) 0.0159(6) 0.0028(5) -0.0029(5) -0.0034(5) C20 0.0253(7) 0.0292(8) 0.0225(7) -0.0074(6) -0.0032(6) -0.0033(6) C21 0.0437(10) 0.0299(8) 0.0245(8) 0.0076(7) 0.0027(7) -0.0128(7) C22 0.0164(6) 0.0239(7) 0.0143(6) -0.0033(5) -0.0014(5) -0.0044(5) C23 0.0434(10) 0.0431(10) 0.0295(9) 0.0130(8) -0.0149(8) -0.0258(9) C24 0.0369(9) 0.0381(9) 0.0202(7) -0.0109(7) -0.0032(6) 0.0016(7) C25 0.0151(6) 0.0252(7) 0.0133(6) -0.0022(5) -0.0026(5) -0.0029(5) C26 0.0137(6) 0.0165(6) 0.0191(6) -0.0056(5) -0.0026(5) -0.0035(5) C27 0.0147(6) 0.0158(6) 0.0169(6) -0.0009(5) -0.0009(5) -0.0048(5) C28 0.0142(6) 0.0174(6) 0.0183(6) -0.0023(5) 0.0006(5) -0.0012(5) C29 0.0153(6) 0.0187(6) 0.0173(6) 0.0025(5) -0.0020(5) -0.0008(5) C30 0.0253(8) 0.0466(10) 0.0136(6) -0.0010(6) -0.0019(5) -0.0054(7) C31 0.0205(7) 0.0195(7) 0.0332(8) -0.0131(6) -0.0011(6) -0.0049(5) C32 0.0233(7) 0.0250(7) 0.0231(7) 0.0055(6) -0.0007(6) -0.0087(6) C33 0.0222(7) 0.0246(7) 0.0275(8) -0.0064(6) 0.0075(6) 0.0005(6) C34 0.0257(8) 0.0279(8) 0.0330(9) 0.0134(7) -0.0047(6) 0.0037(6) N1 0.0229(6) 0.0138(5) 0.0162(5) 0.0017(4) 0.0011(4) -0.0056(4) N2 0.0262(6) 0.0127(5) 0.0142(5) -0.0020(4) 0.0009(4) -0.0050(4) N3 0.0156(5) 0.0136(5) 0.0143(5) -0.0009(4) -0.0016(4) -0.0027(4) Ti 0.01461(11) 0.00974(10) 0.01052(11) -0.00074(7) -0.00013(8) -0.00226(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.4516(19) . ? C1 C2 1.508(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.508(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.503(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N1 1.3270(18) . ? C4 N2 1.3315(18) . ? C4 Ti 2.4808(14) . ? C5 C6 1.394(2) . ? C5 C10 1.3989(18) . ? C5 N2 1.4071(17) . ? C6 C7 1.389(2) . ? C6 H6 0.9500 . ? C7 C8 1.396(2) . ? C7 C11 1.506(2) . ? C8 C9 1.391(2) . ? C8 H8 0.9500 . ? C9 C10 1.3883(19) . ? C9 C12 1.5101(19) . ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N3 1.3780(16) . ? C13 C14 1.4177(18) . ? C13 C18 1.4230(19) . ? C14 C15 1.3936(19) . ? C14 C19 1.5150(19) . ? C15 C16 1.388(2) . ? C15 H15 0.9500 . ? C16 C17 1.386(2) . ? C16 H16 0.9500 . ? C17 C18 1.3916(19) . ? C17 H17 0.9500 . ? C18 C22 1.515(2) . ? C19 C20 1.528(2) . ? C19 C21 1.528(2) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.520(2) . ? C22 C24 1.525(2) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.417(2) . ? C25 C29 1.4240(19) . ? C25 C30 1.504(2) . ? C25 Ti 2.3413(13) . ? C26 C27 1.4243(18) . ? C26 C31 1.4958(19) . ? C26 Ti 2.3444(13) . ? C27 C28 1.4250(19) . ? C27 C32 1.500(2) . ? C27 Ti 2.3517(13) . ? C28 C29 1.4095(19) . ? C28 C33 1.5014(19) . ? C28 Ti 2.4071(14) . ? C29 C34 1.500(2) . ? C29 Ti 2.4000(14) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? N1 Ti 2.0821(12) . ? N2 Ti 2.1146(11) . ? N3 Ti 1.7384(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 105.81(13) . . ? N1 C1 H1A 110.6 . . ? C2 C1 H1A 110.6 . . ? N1 C1 H1B 110.6 . . ? C2 C1 H1B 110.6 . . ? H1A C1 H1B 108.7 . . ? C1 C2 C3 107.45(13) . . ? C1 C2 H2A 110.2 . . ? C3 C2 H2A 110.2 . . ? C1 C2 H2B 110.2 . . ? C3 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? C4 C3 C2 102.69(13) . . ? C4 C3 H3A 111.2 . . ? C2 C3 H3A 111.2 . . ? C4 C3 H3B 111.2 . . ? C2 C3 H3B 111.2 . . ? H3A C3 H3B 109.1 . . ? N1 C4 N2 115.39(12) . . ? N1 C4 C3 112.76(13) . . ? N2 C4 C3 131.69(13) . . ? N1 C4 Ti 57.06(7) . . ? N2 C4 Ti 58.46(7) . . ? C3 C4 Ti 167.62(12) . . ? C6 C5 C10 119.01(12) . . ? C6 C5 N2 118.00(12) . . ? C10 C5 N2 122.93(13) . . ? C7 C6 C5 121.22(13) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C8 118.70(14) . . ? C6 C7 C11 120.83(14) . . ? C8 C7 C11 120.46(13) . . ? C9 C8 C7 121.09(13) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C10 C9 C8 119.36(13) . . ? C10 C9 C12 120.43(14) . . ? C8 C9 C12 120.20(13) . . ? C9 C10 C5 120.59(13) . . ? C9 C10 H10 119.7 . . ? C5 C10 H10 119.7 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 120.14(12) . . ? N3 C13 C18 120.18(12) . . ? C14 C13 C18 119.68(12) . . ? C15 C14 C13 119.07(13) . . ? C15 C14 C19 121.22(12) . . ? C13 C14 C19 119.65(12) . . ? C16 C15 C14 121.13(13) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C17 C16 C15 119.79(13) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 121.33(13) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C17 C18 C13 118.88(13) . . ? C17 C18 C22 121.81(13) . . ? C13 C18 C22 119.31(12) . . ? C14 C19 C20 109.64(12) . . ? C14 C19 C21 113.33(12) . . ? C20 C19 C21 111.09(13) . . ? C14 C19 H19 107.5 . . ? C20 C19 H19 107.5 . . ? C21 C19 H19 107.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 C23 111.04(12) . . ? C18 C22 C24 113.79(13) . . ? C23 C22 C24 111.12(14) . . ? C18 C22 H22 106.8 . . ? C23 C22 H22 106.8 . . ? C24 C22 H22 106.8 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C29 108.35(12) . . ? C26 C25 C30 126.72(14) . . ? C29 C25 C30 124.83(14) . . ? C26 C25 Ti 72.52(7) . . ? C29 C25 Ti 74.79(8) . . ? C30 C25 Ti 121.60(10) . . ? C25 C26 C27 107.50(12) . . ? C25 C26 C31 127.46(13) . . ? C27 C26 C31 124.96(13) . . ? C25 C26 Ti 72.28(8) . . ? C27 C26 Ti 72.62(7) . . ? C31 C26 Ti 123.14(9) . . ? C26 C27 C28 108.05(12) . . ? C26 C27 C32 125.40(13) . . ? C28 C27 C32 126.36(13) . . ? C26 C27 Ti 72.07(7) . . ? C28 C27 Ti 74.71(8) . . ? C32 C27 Ti 123.00(9) . . ? C29 C28 C27 108.05(12) . . ? C29 C28 C33 126.61(13) . . ? C27 C28 C33 125.25(13) . . ? C29 C28 Ti 72.67(8) . . ? C27 C28 Ti 70.46(7) . . ? C33 C28 Ti 125.16(10) . . ? C28 C29 C25 108.00(12) . . ? C28 C29 C34 126.62(14) . . ? C25 C29 C34 125.37(13) . . ? C28 C29 Ti 73.22(8) . . ? C25 C29 Ti 70.28(8) . . ? C34 C29 Ti 122.97(11) . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C4 N1 C1 111.10(12) . . ? C4 N1 Ti 90.61(8) . . ? C1 N1 Ti 156.06(11) . . ? C4 N2 C5 124.77(12) . . ? C4 N2 Ti 89.09(8) . . ? C5 N2 Ti 146.05(9) . . ? C13 N3 Ti 164.91(10) . . ? N3 Ti N1 109.16(5) . . ? N3 Ti N2 113.32(5) . . ? N1 Ti N2 64.74(5) . . ? N3 Ti C25 112.70(5) . . ? N1 Ti C25 97.55(5) . . ? N2 Ti C25 133.91(5) . . ? N3 Ti C26 91.05(5) . . ? N1 Ti C26 132.14(5) . . ? N2 Ti C26 145.03(5) . . ? C25 Ti C26 35.20(5) . . ? N3 Ti C27 104.71(5) . . ? N1 Ti C27 144.36(5) . . ? N2 Ti C27 111.11(5) . . ? C25 Ti C27 58.45(5) . . ? C26 Ti C27 35.31(5) . . ? N3 Ti C29 146.99(5) . . ? N1 Ti C29 87.29(5) . . ? N2 Ti C29 99.52(5) . . ? C25 Ti C29 34.93(5) . . ? C26 Ti C29 58.07(5) . . ? C27 Ti C29 57.72(5) . . ? N3 Ti C28 139.31(5) . . ? N1 Ti C28 111.28(5) . . ? N2 Ti C28 88.09(5) . . ? C25 Ti C28 57.72(5) . . ? C26 Ti C28 58.04(5) . . ? C27 Ti C28 34.82(5) . . ? C29 Ti C28 34.10(5) . . ? N3 Ti C4 114.03(5) . . ? N1 Ti C4 32.34(5) . . ? N2 Ti C4 32.46(4) . . ? C25 Ti C4 120.27(5) . . ? C26 Ti C4 153.20(5) . . ? C27 Ti C4 135.10(5) . . ? C29 Ti C4 95.32(5) . . ? C28 Ti C4 102.52(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -4.2(2) . . . . ? C1 C2 C3 C4 2.8(2) . . . . ? C2 C3 C4 N1 -0.4(2) . . . . ? C2 C3 C4 N2 -175.61(17) . . . . ? C2 C3 C4 Ti -33.4(6) . . . . ? C10 C5 C6 C7 1.9(2) . . . . ? N2 C5 C6 C7 178.89(14) . . . . ? C5 C6 C7 C8 -1.0(2) . . . . ? C5 C6 C7 C11 178.15(16) . . . . ? C6 C7 C8 C9 -0.4(2) . . . . ? C11 C7 C8 C9 -179.53(16) . . . . ? C7 C8 C9 C10 0.8(2) . . . . ? C7 C8 C9 C12 -178.17(15) . . . . ? C8 C9 C10 C5 0.1(2) . . . . ? C12 C9 C10 C5 179.13(14) . . . . ? C6 C5 C10 C9 -1.5(2) . . . . ? N2 C5 C10 C9 -178.30(13) . . . . ? N3 C13 C14 C15 177.59(12) . . . . ? C18 C13 C14 C15 -2.97(19) . . . . ? N3 C13 C14 C19 0.30(19) . . . . ? C18 C13 C14 C19 179.74(12) . . . . ? C13 C14 C15 C16 -0.1(2) . . . . ? C19 C14 C15 C16 177.11(13) . . . . ? C14 C15 C16 C17 2.4(2) . . . . ? C15 C16 C17 C18 -1.6(2) . . . . ? C16 C17 C18 C13 -1.5(2) . . . . ? C16 C17 C18 C22 178.76(13) . . . . ? N3 C13 C18 C17 -176.80(12) . . . . ? C14 C13 C18 C17 3.76(19) . . . . ? N3 C13 C18 C22 2.97(18) . . . . ? C14 C13 C18 C22 -176.47(12) . . . . ? C15 C14 C19 C20 -82.51(16) . . . . ? C13 C14 C19 C20 94.72(15) . . . . ? C15 C14 C19 C21 42.23(19) . . . . ? C13 C14 C19 C21 -140.54(14) . . . . ? C17 C18 C22 C23 91.97(17) . . . . ? C13 C18 C22 C23 -87.79(17) . . . . ? C17 C18 C22 C24 -34.29(19) . . . . ? C13 C18 C22 C24 145.94(14) . . . . ? C29 C25 C26 C27 2.22(15) . . . . ? C30 C25 C26 C27 178.67(13) . . . . ? Ti C25 C26 C27 -64.56(9) . . . . ? C29 C25 C26 C31 -174.65(13) . . . . ? C30 C25 C26 C31 1.8(2) . . . . ? Ti C25 C26 C31 118.56(14) . . . . ? C29 C25 C26 Ti 66.78(10) . . . . ? C30 C25 C26 Ti -116.77(14) . . . . ? C25 C26 C27 C28 -2.28(15) . . . . ? C31 C26 C27 C28 174.69(13) . . . . ? Ti C26 C27 C28 -66.61(9) . . . . ? C25 C26 C27 C32 -177.48(13) . . . . ? C31 C26 C27 C32 -0.5(2) . . . . ? Ti C26 C27 C32 118.18(13) . . . . ? C25 C26 C27 Ti 64.34(9) . . . . ? C31 C26 C27 Ti -118.69(13) . . . . ? C26 C27 C28 C29 1.48(15) . . . . ? C32 C27 C28 C29 176.62(13) . . . . ? Ti C27 C28 C29 -63.38(10) . . . . ? C26 C27 C28 C33 -175.31(13) . . . . ? C32 C27 C28 C33 -0.2(2) . . . . ? Ti C27 C28 C33 119.83(14) . . . . ? C26 C27 C28 Ti 64.86(9) . . . . ? C32 C27 C28 Ti -119.99(14) . . . . ? C27 C28 C29 C25 -0.10(15) . . . . ? C33 C28 C29 C25 176.62(14) . . . . ? Ti C28 C29 C25 -62.06(9) . . . . ? C27 C28 C29 C34 -179.09(14) . . . . ? C33 C28 C29 C34 -2.4(2) . . . . ? Ti C28 C29 C34 118.96(15) . . . . ? C27 C28 C29 Ti 61.96(9) . . . . ? C33 C28 C29 Ti -121.31(14) . . . . ? C26 C25 C29 C28 -1.32(16) . . . . ? C30 C25 C29 C28 -177.85(13) . . . . ? Ti C25 C29 C28 63.97(10) . . . . ? C26 C25 C29 C34 177.68(14) . . . . ? C30 C25 C29 C34 1.1(2) . . . . ? Ti C25 C29 C34 -117.03(15) . . . . ? C26 C25 C29 Ti -65.29(9) . . . . ? C30 C25 C29 Ti 118.18(14) . . . . ? N2 C4 N1 C1 173.70(14) . . . . ? C3 C4 N1 C1 -2.34(19) . . . . ? Ti C4 N1 C1 169.67(14) . . . . ? N2 C4 N1 Ti 4.02(13) . . . . ? C3 C4 N1 Ti -172.02(13) . . . . ? C2 C1 N1 C4 4.1(2) . . . . ? C2 C1 N1 Ti 157.8(2) . . . . ? N1 C4 N2 C5 178.71(13) . . . . ? C3 C4 N2 C5 -6.2(3) . . . . ? Ti C4 N2 C5 -177.32(16) . . . . ? N1 C4 N2 Ti -3.96(13) . . . . ? C3 C4 N2 Ti 171.15(17) . . . . ? C6 C5 N2 C4 139.56(15) . . . . ? C10 C5 N2 C4 -43.6(2) . . . . ? C6 C5 N2 Ti -35.6(2) . . . . ? C10 C5 N2 Ti 141.22(15) . . . . ? C14 C13 N3 Ti 101.5(4) . . . . ? C18 C13 N3 Ti -77.9(4) . . . . ? C13 N3 Ti N1 134.3(4) . . . . ? C13 N3 Ti N2 -155.7(4) . . . . ? C13 N3 Ti C25 27.0(4) . . . . ? C13 N3 Ti C26 -1.5(4) . . . . ? C13 N3 Ti C27 -34.5(4) . . . . ? C13 N3 Ti C29 18.0(4) . . . . ? C13 N3 Ti C28 -39.3(4) . . . . ? C13 N3 Ti C4 168.7(4) . . . . ? C4 N1 Ti N3 104.89(9) . . . . ? C1 N1 Ti N3 -50.8(3) . . . . ? C4 N1 Ti N2 -2.53(8) . . . . ? C1 N1 Ti N2 -158.2(3) . . . . ? C4 N1 Ti C25 -137.84(9) . . . . ? C1 N1 Ti C25 66.5(3) . . . . ? C4 N1 Ti C26 -145.19(8) . . . . ? C1 N1 Ti C26 59.2(3) . . . . ? C4 N1 Ti C27 -93.99(11) . . . . ? C1 N1 Ti C27 110.4(3) . . . . ? C4 N1 Ti C29 -104.38(9) . . . . ? C1 N1 Ti C29 100.0(3) . . . . ? C4 N1 Ti C28 -79.62(9) . . . . ? C1 N1 Ti C28 124.7(3) . . . . ? C1 N1 Ti C4 -155.7(3) . . . . ? C4 N2 Ti N3 -98.54(9) . . . . ? C5 N2 Ti N3 77.52(18) . . . . ? C4 N2 Ti N1 2.52(8) . . . . ? C5 N2 Ti N1 178.58(19) . . . . ? C4 N2 Ti C25 77.90(10) . . . . ? C5 N2 Ti C25 -106.04(18) . . . . ? C4 N2 Ti C26 130.83(10) . . . . ? C5 N2 Ti C26 -53.1(2) . . . . ? C4 N2 Ti C27 143.88(8) . . . . ? C5 N2 Ti C27 -40.05(19) . . . . ? C4 N2 Ti C29 84.93(9) . . . . ? C5 N2 Ti C29 -99.01(18) . . . . ? C4 N2 Ti C28 117.19(9) . . . . ? C5 N2 Ti C28 -66.75(18) . . . . ? C5 N2 Ti C4 176.1(2) . . . . ? C26 C25 Ti N3 -56.05(9) . . . . ? C29 C25 Ti N3 -171.37(8) . . . . ? C30 C25 Ti N3 66.79(14) . . . . ? C26 C25 Ti N1 -170.53(8) . . . . ? C29 C25 Ti N1 74.15(9) . . . . ? C30 C25 Ti N1 -47.69(13) . . . . ? C26 C25 Ti N2 127.49(8) . . . . ? C29 C25 Ti N2 12.18(11) . . . . ? C30 C25 Ti N2 -109.67(13) . . . . ? C29 C25 Ti C26 -115.32(12) . . . . ? C30 C25 Ti C26 122.84(16) . . . . ? C26 C25 Ti C27 37.74(8) . . . . ? C29 C25 Ti C27 -77.57(9) . . . . ? C30 C25 Ti C27 160.58(14) . . . . ? C26 C25 Ti C29 115.32(12) . . . . ? C30 C25 Ti C29 -121.85(16) . . . . ? C26 C25 Ti C28 79.02(9) . . . . ? C29 C25 Ti C28 -36.29(8) . . . . ? C30 C25 Ti C28 -158.14(15) . . . . ? C26 C25 Ti C4 164.91(8) . . . . ? C29 C25 Ti C4 49.59(10) . . . . ? C30 C25 Ti C4 -72.26(14) . . . . ? C25 C26 Ti N3 130.06(8) . . . . ? C27 C26 Ti N3 -114.43(8) . . . . ? C31 C26 Ti N3 6.41(12) . . . . ? C25 C26 Ti N1 12.70(11) . . . . ? C27 C26 Ti N1 128.22(8) . . . . ? C31 C26 Ti N1 -110.94(12) . . . . ? C25 C26 Ti N2 -94.14(11) . . . . ? C27 C26 Ti N2 21.37(13) . . . . ? C31 C26 Ti N2 142.22(11) . . . . ? C27 C26 Ti C25 115.52(11) . . . . ? C31 C26 Ti C25 -123.64(15) . . . . ? C25 C26 Ti C27 -115.52(11) . . . . ? C31 C26 Ti C27 120.84(16) . . . . ? C25 C26 Ti C29 -37.58(8) . . . . ? C27 C26 Ti C29 77.94(8) . . . . ? C31 C26 Ti C29 -161.22(14) . . . . ? C25 C26 Ti C28 -78.01(9) . . . . ? C27 C26 Ti C28 37.51(8) . . . . ? C31 C26 Ti C28 158.35(14) . . . . ? C25 C26 Ti C4 -29.92(15) . . . . ? C27 C26 Ti C4 85.60(13) . . . . ? C31 C26 Ti C4 -153.56(12) . . . . ? C26 C27 Ti N3 70.25(9) . . . . ? C28 C27 Ti N3 -174.53(8) . . . . ? C32 C27 Ti N3 -50.80(12) . . . . ? C26 C27 Ti N1 -91.33(11) . . . . ? C28 C27 Ti N1 23.89(12) . . . . ? C32 C27 Ti N1 147.62(11) . . . . ? C26 C27 Ti N2 -167.06(8) . . . . ? C28 C27 Ti N2 -51.84(9) . . . . ? C32 C27 Ti N2 71.89(12) . . . . ? C26 C27 Ti C25 -37.62(8) . . . . ? C28 C27 Ti C25 77.60(9) . . . . ? C32 C27 Ti C25 -158.67(13) . . . . ? C28 C27 Ti C26 115.22(12) . . . . ? C32 C27 Ti C26 -121.05(15) . . . . ? C26 C27 Ti C29 -79.03(9) . . . . ? C28 C27 Ti C29 36.19(8) . . . . ? C32 C27 Ti C29 159.92(13) . . . . ? C26 C27 Ti C28 -115.22(12) . . . . ? C32 C27 Ti C28 123.73(15) . . . . ? C26 C27 Ti C4 -140.44(8) . . . . ? C28 C27 Ti C4 -25.22(11) . . . . ? C32 C27 Ti C4 98.52(12) . . . . ? C28 C29 Ti N3 -102.07(11) . . . . ? C25 C29 Ti N3 14.73(14) . . . . ? C34 C29 Ti N3 134.76(13) . . . . ? C28 C29 Ti N1 135.89(9) . . . . ? C25 C29 Ti N1 -107.31(9) . . . . ? C34 C29 Ti N1 12.72(12) . . . . ? C28 C29 Ti N2 72.06(9) . . . . ? C25 C29 Ti N2 -171.14(8) . . . . ? C34 C29 Ti N2 -51.10(13) . . . . ? C28 C29 Ti C25 -116.80(12) . . . . ? C34 C29 Ti C25 120.03(16) . . . . ? C28 C29 Ti C26 -78.93(9) . . . . ? C25 C29 Ti C26 37.87(8) . . . . ? C34 C29 Ti C26 157.91(14) . . . . ? C28 C29 Ti C27 -36.97(8) . . . . ? C25 C29 Ti C27 79.83(9) . . . . ? C34 C29 Ti C27 -160.14(14) . . . . ? C25 C29 Ti C28 116.80(12) . . . . ? C34 C29 Ti C28 -123.17(16) . . . . ? C28 C29 Ti C4 104.53(8) . . . . ? C25 C29 Ti C4 -138.67(8) . . . . ? C34 C29 Ti C4 -18.63(13) . . . . ? C29 C28 Ti N3 125.20(9) . . . . ? C27 C28 Ti N3 8.13(12) . . . . ? C33 C28 Ti N3 -111.82(13) . . . . ? C29 C28 Ti N1 -48.26(9) . . . . ? C27 C28 Ti N1 -165.33(8) . . . . ? C33 C28 Ti N1 74.72(13) . . . . ? C29 C28 Ti N2 -110.15(8) . . . . ? C27 C28 Ti N2 132.78(8) . . . . ? C33 C28 Ti N2 12.84(12) . . . . ? C29 C28 Ti C25 37.19(8) . . . . ? C27 C28 Ti C25 -79.88(9) . . . . ? C33 C28 Ti C25 160.17(14) . . . . ? C29 C28 Ti C26 79.03(9) . . . . ? C27 C28 Ti C26 -38.05(8) . . . . ? C33 C28 Ti C26 -157.99(14) . . . . ? C29 C28 Ti C27 117.07(12) . . . . ? C33 C28 Ti C27 -119.95(16) . . . . ? C27 C28 Ti C29 -117.07(12) . . . . ? C33 C28 Ti C29 122.98(16) . . . . ? C29 C28 Ti C4 -80.87(9) . . . . ? C27 C28 Ti C4 162.06(8) . . . . ? C33 C28 Ti C4 42.11(13) . . . . ? N1 C4 Ti N3 -88.15(9) . . . . ? N2 C4 Ti N3 96.11(9) . . . . ? C3 C4 Ti N3 -51.5(6) . . . . ? N2 C4 Ti N1 -175.73(14) . . . . ? C3 C4 Ti N1 36.7(5) . . . . ? N1 C4 Ti N2 175.73(14) . . . . ? C3 C4 Ti N2 -147.6(6) . . . . ? N1 C4 Ti C25 50.39(10) . . . . ? N2 C4 Ti C25 -125.35(9) . . . . ? C3 C4 Ti C25 87.1(6) . . . . ? N1 C4 Ti C26 69.83(14) . . . . ? N2 C4 Ti C26 -105.90(12) . . . . ? C3 C4 Ti C26 106.5(5) . . . . ? N1 C4 Ti C27 124.56(9) . . . . ? N2 C4 Ti C27 -51.17(11) . . . . ? C3 C4 Ti C27 161.3(5) . . . . ? N1 C4 Ti C29 76.36(9) . . . . ? N2 C4 Ti C29 -99.38(9) . . . . ? C3 C4 Ti C29 113.1(6) . . . . ? N1 C4 Ti C28 110.13(9) . . . . ? N2 C4 Ti C28 -65.60(9) . . . . ? C3 C4 Ti C28 146.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.473 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.069 _chemical_absolute_configuration ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' #==end== data_complex_5 _database_code_depnum_ccdc_archive 'CCDC 718802' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H39 N3 Ti' _chemical_formula_weight 489.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.8833(13) _cell_length_b 9.7449(9) _cell_length_c 20.1013(18) _cell_angle_alpha 90.00 _cell_angle_beta 100.422(2) _cell_angle_gamma 90.00 _cell_volume 2674.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour black _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.342 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6577 _exptl_absorpt_correction_T_max 0.7463 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004-2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector (Bruker AXS Smart 1000)' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 35562 _diffrn_reflns_av_R_equivalents 0.0916 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4724 _reflns_number_gt 3111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 1997-2003)' _computing_cell_refinement 'SAINT (Bruker AXS, 1997-2008)' _computing_data_reduction 'SAINT (Bruker AXS, 1997-2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+8.8688P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4724 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1078 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1490 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0851(3) 0.5834(4) 0.0791(2) 0.0284(10) Uani 1 1 d . . . H1A H 0.0236 0.5328 0.0627 0.034 Uiso 1 1 calc R . . H1B H 0.1088 0.6236 0.0398 0.034 Uiso 1 1 calc R . . C2 C 0.0689(3) 0.6950(5) 0.1291(2) 0.0297(10) Uani 1 1 d . . . H2A H 0.0693 0.7868 0.1080 0.036 Uiso 1 1 calc R . . H2B H 0.0052 0.6818 0.1438 0.036 Uiso 1 1 calc R . . C3 C 0.1529(3) 0.6820(4) 0.18903(19) 0.0190(9) Uani 1 1 d . . . H3A H 0.2009 0.7573 0.1894 0.023 Uiso 1 1 calc R . . H3B H 0.1287 0.6822 0.2324 0.023 Uiso 1 1 calc R . . C4 C 0.1972(3) 0.5450(4) 0.17649(18) 0.0148(8) Uani 1 1 d . . . C5 C 0.3061(3) 0.4820(4) 0.28241(18) 0.0144(8) Uani 1 1 d . . . C6 C 0.3462(3) 0.3651(4) 0.31551(18) 0.0168(8) Uani 1 1 d . . . H6 H 0.3453 0.2819 0.2908 0.020 Uiso 1 1 calc R . . C7 C 0.3877(3) 0.3661(4) 0.38394(19) 0.0196(9) Uani 1 1 d . . . C8 C 0.3868(3) 0.4879(4) 0.41947(19) 0.0217(9) Uani 1 1 d . . . H8 H 0.4128 0.4895 0.4666 0.026 Uiso 1 1 calc R . . C9 C 0.3490(3) 0.6069(4) 0.38782(19) 0.0203(9) Uani 1 1 d . . . C10 C 0.3092(3) 0.6046(4) 0.31844(19) 0.0180(9) Uani 1 1 d . . . H10 H 0.2845 0.6866 0.2961 0.022 Uiso 1 1 calc R . . C11 C 0.4333(3) 0.2392(5) 0.4176(2) 0.0305(11) Uani 1 1 d . . . H11A H 0.3987 0.1583 0.3963 0.046 Uiso 1 1 calc R . . H11B H 0.4287 0.2412 0.4657 0.046 Uiso 1 1 calc R . . H11C H 0.5022 0.2348 0.4130 0.046 Uiso 1 1 calc R . . C12 C 0.3475(4) 0.7392(5) 0.4268(2) 0.0325(11) Uani 1 1 d . . . H12A H 0.3139 0.7242 0.4651 0.049 Uiso 1 1 calc R . . H12B H 0.3128 0.8098 0.3970 0.049 Uiso 1 1 calc R . . H12C H 0.4149 0.7693 0.4436 0.049 Uiso 1 1 calc R . . C13 C 0.0772(3) 0.1028(4) 0.18520(18) 0.0147(8) Uani 1 1 d . . . C14 C 0.0931(3) 0.0210(4) 0.24422(19) 0.0171(8) Uani 1 1 d . . . C15 C 0.0210(3) -0.0694(4) 0.2553(2) 0.0214(9) Uani 1 1 d . . . H15 H 0.0320 -0.1248 0.2948 0.026 Uiso 1 1 calc R . . C16 C -0.0669(3) -0.0817(4) 0.2104(2) 0.0233(9) Uani 1 1 d . . . H16 H -0.1154 -0.1446 0.2190 0.028 Uiso 1 1 calc R . . C17 C -0.0828(3) -0.0003(4) 0.1526(2) 0.0208(9) Uani 1 1 d . . . H17 H -0.1430 -0.0081 0.1217 0.025 Uiso 1 1 calc R . . C18 C -0.0126(3) 0.0920(4) 0.13916(19) 0.0187(9) Uani 1 1 d . . . C19 C -0.0316(3) 0.1812(5) 0.0772(2) 0.0263(10) Uani 1 1 d . . . H19A H 0.0101 0.1515 0.0455 0.039 Uiso 1 1 calc R . . H19B H -0.0168 0.2769 0.0902 0.039 Uiso 1 1 calc R . . H19C H -0.1006 0.1733 0.0556 0.039 Uiso 1 1 calc R . . C20 C 0.1879(3) 0.0335(4) 0.2934(2) 0.0239(9) Uani 1 1 d . . . H20A H 0.1863 -0.0265 0.3323 0.036 Uiso 1 1 calc R . . H20B H 0.1971 0.1288 0.3088 0.036 Uiso 1 1 calc R . . H20C H 0.2422 0.0064 0.2711 0.036 Uiso 1 1 calc R . . C21 C 0.2833(3) 0.1370(4) 0.07652(19) 0.0175(8) Uani 1 1 d . . . C22 C 0.3606(3) 0.1635(4) 0.13138(19) 0.0202(9) Uani 1 1 d . . . C23 C 0.3938(3) 0.2996(4) 0.12523(18) 0.0191(8) Uani 1 1 d . . . C24 C 0.3359(3) 0.3578(4) 0.06721(19) 0.0191(9) Uani 1 1 d . . . C25 C 0.2671(3) 0.2579(4) 0.03709(18) 0.0166(8) Uani 1 1 d . . . C26 C 0.2311(4) 0.0033(4) 0.0617(2) 0.0317(11) Uani 1 1 d . . . H26A H 0.1661 0.0197 0.0346 0.048 Uiso 1 1 calc R . . H26B H 0.2242 -0.0413 0.1043 0.048 Uiso 1 1 calc R . . H26C H 0.2689 -0.0562 0.0366 0.048 Uiso 1 1 calc R . . C27 C 0.4059(3) 0.0610(5) 0.1835(2) 0.0315(11) Uani 1 1 d . . . H27A H 0.3572 -0.0088 0.1892 0.047 Uiso 1 1 calc R . . H27B H 0.4282 0.1079 0.2267 0.047 Uiso 1 1 calc R . . H27C H 0.4618 0.0170 0.1686 0.047 Uiso 1 1 calc R . . C28 C 0.4755(3) 0.3713(5) 0.1715(2) 0.0325(11) Uani 1 1 d . . . H28A H 0.5270 0.3961 0.1462 0.049 Uiso 1 1 calc R . . H28B H 0.5026 0.3099 0.2089 0.049 Uiso 1 1 calc R . . H28C H 0.4502 0.4544 0.1897 0.049 Uiso 1 1 calc R . . C29 C 0.3457(4) 0.5020(4) 0.0423(2) 0.0318(11) Uani 1 1 d . . . H29A H 0.3475 0.5664 0.0800 0.048 Uiso 1 1 calc R . . H29B H 0.2897 0.5233 0.0067 0.048 Uiso 1 1 calc R . . H29C H 0.4064 0.5100 0.0242 0.048 Uiso 1 1 calc R . . C30 C 0.1914(3) 0.2784(5) -0.02577(19) 0.0296(11) Uani 1 1 d . . . H30A H 0.2212 0.2622 -0.0657 0.044 Uiso 1 1 calc R . . H30B H 0.1665 0.3727 -0.0268 0.044 Uiso 1 1 calc R . . H30C H 0.1373 0.2139 -0.0258 0.044 Uiso 1 1 calc R . . N1 N 0.1589(2) 0.4925(3) 0.11712(15) 0.0175(7) Uani 1 1 d . . . N2 N 0.2644(2) 0.4656(3) 0.21391(14) 0.0143(7) Uani 1 1 d . . . N3 N 0.1458(2) 0.1974(3) 0.17266(15) 0.0156(7) Uani 1 1 d . . . Ti Ti 0.22789(5) 0.30538(7) 0.14363(3) 0.01256(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.035(3) 0.027(2) 0.019(2) 0.0026(19) -0.0061(19) 0.013(2) C2 0.034(3) 0.022(2) 0.027(2) -0.003(2) -0.0102(19) 0.010(2) C3 0.023(2) 0.017(2) 0.0154(19) -0.0002(17) 0.0003(16) 0.0040(18) C4 0.017(2) 0.0138(19) 0.0130(19) 0.0007(15) 0.0026(16) -0.0037(16) C5 0.0111(19) 0.020(2) 0.0112(18) -0.0038(16) 0.0007(15) -0.0043(16) C6 0.015(2) 0.019(2) 0.016(2) -0.0024(16) 0.0023(16) 0.0010(16) C7 0.013(2) 0.029(2) 0.015(2) 0.0030(18) 0.0000(16) 0.0024(17) C8 0.016(2) 0.037(3) 0.0105(19) -0.0021(18) 0.0004(16) -0.0031(19) C9 0.020(2) 0.026(2) 0.015(2) -0.0070(17) 0.0031(16) -0.0032(18) C10 0.017(2) 0.023(2) 0.0142(19) -0.0015(17) 0.0017(16) -0.0022(17) C11 0.030(3) 0.041(3) 0.019(2) 0.007(2) -0.0014(19) 0.015(2) C12 0.046(3) 0.029(3) 0.021(2) -0.0072(19) 0.004(2) -0.005(2) C13 0.020(2) 0.0094(18) 0.017(2) -0.0028(15) 0.0094(16) 0.0020(16) C14 0.017(2) 0.0137(19) 0.021(2) -0.0011(16) 0.0049(16) 0.0036(16) C15 0.030(3) 0.015(2) 0.021(2) -0.0018(17) 0.0107(19) 0.0007(18) C16 0.024(2) 0.019(2) 0.029(2) -0.0075(18) 0.0126(19) -0.0062(18) C17 0.018(2) 0.020(2) 0.025(2) -0.0085(18) 0.0060(17) -0.0022(17) C18 0.021(2) 0.017(2) 0.019(2) -0.0052(17) 0.0066(17) 0.0016(17) C19 0.023(2) 0.032(3) 0.021(2) 0.000(2) -0.0022(17) -0.005(2) C20 0.026(2) 0.027(2) 0.019(2) 0.0076(18) 0.0034(18) 0.0019(19) C21 0.021(2) 0.018(2) 0.016(2) -0.0047(16) 0.0084(16) -0.0004(17) C22 0.018(2) 0.026(2) 0.017(2) -0.0021(17) 0.0059(16) 0.0086(17) C23 0.017(2) 0.026(2) 0.0162(19) -0.0072(18) 0.0070(16) -0.0013(18) C24 0.023(2) 0.019(2) 0.019(2) -0.0017(17) 0.0117(17) -0.0040(17) C25 0.021(2) 0.020(2) 0.0086(18) 0.0000(16) 0.0023(16) 0.0016(17) C26 0.042(3) 0.020(2) 0.036(3) -0.007(2) 0.017(2) -0.008(2) C27 0.035(3) 0.034(3) 0.028(2) 0.013(2) 0.013(2) 0.019(2) C28 0.021(2) 0.048(3) 0.028(2) -0.013(2) 0.0044(19) -0.005(2) C29 0.041(3) 0.022(2) 0.036(3) 0.004(2) 0.017(2) -0.007(2) C30 0.030(3) 0.044(3) 0.014(2) 0.0008(19) 0.0011(18) 0.001(2) N1 0.0198(18) 0.0198(18) 0.0110(16) 0.0008(14) -0.0021(13) 0.0026(14) N2 0.0188(17) 0.0136(16) 0.0092(15) 0.0002(13) -0.0012(13) 0.0003(14) N3 0.0179(17) 0.0162(16) 0.0122(15) -0.0034(14) 0.0013(13) 0.0011(14) Ti 0.0150(4) 0.0127(3) 0.0093(3) -0.0009(3) 0.0005(2) 0.0005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.460(5) . ? C1 C2 1.525(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.524(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.510(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N1 1.319(5) . ? C4 N2 1.335(5) . ? C5 C6 1.384(5) . ? C5 C10 1.394(5) . ? C5 N2 1.403(4) . ? C6 C7 1.392(5) . ? C6 H6 0.9500 . ? C7 C8 1.386(6) . ? C7 C11 1.495(6) . ? C8 C9 1.380(6) . ? C8 H8 0.9500 . ? C9 C10 1.404(5) . ? C9 C12 1.510(6) . ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 N3 1.381(5) . ? C13 C14 1.414(5) . ? C13 C18 1.416(5) . ? C14 C15 1.381(6) . ? C14 C20 1.501(5) . ? C15 C16 1.385(6) . ? C15 H15 0.9500 . ? C16 C17 1.391(6) . ? C16 H16 0.9500 . ? C17 C18 1.389(6) . ? C17 H17 0.9500 . ? C18 C19 1.502(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C25 1.415(5) . ? C21 C22 1.416(5) . ? C21 C26 1.494(6) . ? C21 Ti 2.341(4) . ? C22 C23 1.417(6) . ? C22 C27 1.501(6) . ? C22 Ti 2.351(4) . ? C23 C24 1.410(6) . ? C23 C28 1.502(6) . ? C23 Ti 2.399(4) . ? C24 C25 1.421(5) . ? C24 C29 1.505(6) . ? C24 Ti 2.388(4) . ? C25 C30 1.503(5) . ? C25 Ti 2.349(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? N1 Ti 2.084(3) . ? N2 Ti 2.105(3) . ? N3 Ti 1.728(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 105.2(3) . . ? N1 C1 H1A 110.7 . . ? C2 C1 H1A 110.7 . . ? N1 C1 H1B 110.7 . . ? C2 C1 H1B 110.7 . . ? H1A C1 H1B 108.8 . . ? C3 C2 C1 106.1(3) . . ? C3 C2 H2A 110.5 . . ? C1 C2 H2A 110.5 . . ? C3 C2 H2B 110.5 . . ? C1 C2 H2B 110.5 . . ? H2A C2 H2B 108.7 . . ? C4 C3 C2 102.6(3) . . ? C4 C3 H3A 111.2 . . ? C2 C3 H3A 111.2 . . ? C4 C3 H3B 111.2 . . ? C2 C3 H3B 111.2 . . ? H3A C3 H3B 109.2 . . ? N1 C4 N2 114.3(3) . . ? N1 C4 C3 112.6(3) . . ? N2 C4 C3 133.1(3) . . ? C6 C5 C10 118.9(3) . . ? C6 C5 N2 115.9(3) . . ? C10 C5 N2 125.1(3) . . ? C5 C6 C7 121.9(4) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C8 C7 C6 118.3(4) . . ? C8 C7 C11 121.2(3) . . ? C6 C7 C11 120.5(4) . . ? C9 C8 C7 121.3(3) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C9 C10 119.5(4) . . ? C8 C9 C12 121.2(3) . . ? C10 C9 C12 119.3(4) . . ? C5 C10 C9 119.9(4) . . ? C5 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 121.5(3) . . ? N3 C13 C18 119.0(3) . . ? C14 C13 C18 119.5(3) . . ? C15 C14 C13 119.2(4) . . ? C15 C14 C20 121.4(4) . . ? C13 C14 C20 119.4(3) . . ? C14 C15 C16 121.9(4) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C15 C16 C17 118.9(4) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C18 C17 C16 121.4(4) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C13 119.1(4) . . ? C17 C18 C19 120.8(4) . . ? C13 C18 C19 120.0(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C14 C20 H20A 109.5 . . ? C14 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C14 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C25 C21 C22 107.8(3) . . ? C25 C21 C26 126.3(4) . . ? C22 C21 C26 125.9(4) . . ? C25 C21 Ti 72.7(2) . . ? C22 C21 Ti 72.8(2) . . ? C26 C21 Ti 121.9(3) . . ? C21 C22 C23 108.4(3) . . ? C21 C22 C27 125.8(4) . . ? C23 C22 C27 125.6(4) . . ? C21 C22 Ti 72.0(2) . . ? C23 C22 Ti 74.5(2) . . ? C27 C22 Ti 123.8(3) . . ? C24 C23 C22 107.6(3) . . ? C24 C23 C28 125.4(4) . . ? C22 C23 C28 127.0(4) . . ? C24 C23 Ti 72.4(2) . . ? C22 C23 Ti 70.8(2) . . ? C28 C23 Ti 122.1(3) . . ? C23 C24 C25 108.4(3) . . ? C23 C24 C29 125.3(4) . . ? C25 C24 C29 126.3(4) . . ? C23 C24 Ti 73.3(2) . . ? C25 C24 Ti 71.0(2) . . ? C29 C24 Ti 121.2(3) . . ? C21 C25 C24 107.8(3) . . ? C21 C25 C30 126.7(4) . . ? C24 C25 C30 125.5(4) . . ? C21 C25 Ti 72.1(2) . . ? C24 C25 Ti 74.1(2) . . ? C30 C25 Ti 119.9(3) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C4 N1 C1 111.6(3) . . ? C4 N1 Ti 90.9(2) . . ? C1 N1 Ti 155.6(3) . . ? C4 N2 C5 127.6(3) . . ? C4 N2 Ti 89.6(2) . . ? C5 N2 Ti 138.5(3) . . ? C13 N3 Ti 170.6(3) . . ? N3 Ti N1 108.55(14) . . ? N3 Ti N2 108.56(13) . . ? N1 Ti N2 64.29(12) . . ? N3 Ti C21 94.22(14) . . ? N1 Ti C21 130.54(13) . . ? N2 Ti C21 147.38(14) . . ? N3 Ti C25 117.62(14) . . ? N1 Ti C25 96.37(13) . . ? N2 Ti C25 133.68(13) . . ? C21 Ti C25 35.12(13) . . ? N3 Ti C22 104.75(15) . . ? N1 Ti C22 145.12(14) . . ? N2 Ti C22 114.09(13) . . ? C21 Ti C22 35.13(14) . . ? C25 Ti C22 58.25(13) . . ? N3 Ti C24 151.25(14) . . ? N1 Ti C24 87.79(13) . . ? N2 Ti C24 99.78(13) . . ? C21 Ti C24 57.94(13) . . ? C25 Ti C24 34.90(13) . . ? C22 Ti C24 57.55(14) . . ? N3 Ti C23 138.43(15) . . ? N1 Ti C23 113.01(14) . . ? N2 Ti C23 89.96(13) . . ? C21 Ti C23 57.99(13) . . ? C25 Ti C23 57.84(13) . . ? C22 Ti C23 34.70(14) . . ? C24 Ti C23 34.27(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 13.6(5) . . . . ? C1 C2 C3 C4 -12.6(4) . . . . ? C2 C3 C4 N1 7.5(4) . . . . ? C2 C3 C4 N2 -170.1(4) . . . . ? C10 C5 C6 C7 1.3(6) . . . . ? N2 C5 C6 C7 -178.4(3) . . . . ? C5 C6 C7 C8 1.1(6) . . . . ? C5 C6 C7 C11 -178.0(4) . . . . ? C6 C7 C8 C9 -2.2(6) . . . . ? C11 C7 C8 C9 176.9(4) . . . . ? C7 C8 C9 C10 0.9(6) . . . . ? C7 C8 C9 C12 179.6(4) . . . . ? C6 C5 C10 C9 -2.6(6) . . . . ? N2 C5 C10 C9 177.0(4) . . . . ? C8 C9 C10 C5 1.5(6) . . . . ? C12 C9 C10 C5 -177.2(4) . . . . ? N3 C13 C14 C15 178.2(3) . . . . ? C18 C13 C14 C15 0.9(5) . . . . ? N3 C13 C14 C20 -2.0(5) . . . . ? C18 C13 C14 C20 -179.4(3) . . . . ? C13 C14 C15 C16 -0.4(6) . . . . ? C20 C14 C15 C16 179.8(4) . . . . ? C14 C15 C16 C17 -0.1(6) . . . . ? C15 C16 C17 C18 0.2(6) . . . . ? C16 C17 C18 C13 0.3(6) . . . . ? C16 C17 C18 C19 -178.8(4) . . . . ? N3 C13 C18 C17 -178.2(3) . . . . ? C14 C13 C18 C17 -0.8(5) . . . . ? N3 C13 C18 C19 0.9(5) . . . . ? C14 C13 C18 C19 178.3(4) . . . . ? C25 C21 C22 C23 -1.3(4) . . . . ? C26 C21 C22 C23 176.6(4) . . . . ? Ti C21 C22 C23 -66.2(3) . . . . ? C25 C21 C22 C27 -176.1(4) . . . . ? C26 C21 C22 C27 1.8(6) . . . . ? Ti C21 C22 C27 119.1(4) . . . . ? C25 C21 C22 Ti 64.8(3) . . . . ? C26 C21 C22 Ti -117.3(4) . . . . ? C21 C22 C23 C24 1.0(4) . . . . ? C27 C22 C23 C24 175.8(4) . . . . ? Ti C22 C23 C24 -63.5(3) . . . . ? C21 C22 C23 C28 -179.2(4) . . . . ? C27 C22 C23 C28 -4.4(6) . . . . ? Ti C22 C23 C28 116.3(4) . . . . ? C21 C22 C23 Ti 64.6(3) . . . . ? C27 C22 C23 Ti -120.7(4) . . . . ? C22 C23 C24 C25 -0.3(4) . . . . ? C28 C23 C24 C25 179.9(4) . . . . ? Ti C23 C24 C25 -62.8(3) . . . . ? C22 C23 C24 C29 179.3(4) . . . . ? C28 C23 C24 C29 -0.6(6) . . . . ? Ti C23 C24 C29 116.8(4) . . . . ? C22 C23 C24 Ti 62.5(3) . . . . ? C28 C23 C24 Ti -117.4(4) . . . . ? C22 C21 C25 C24 1.1(4) . . . . ? C26 C21 C25 C24 -176.7(4) . . . . ? Ti C21 C25 C24 66.0(3) . . . . ? C22 C21 C25 C30 -179.3(4) . . . . ? C26 C21 C25 C30 2.8(6) . . . . ? Ti C21 C25 C30 -114.4(4) . . . . ? C22 C21 C25 Ti -64.9(3) . . . . ? C26 C21 C25 Ti 117.2(4) . . . . ? C23 C24 C25 C21 -0.5(4) . . . . ? C29 C24 C25 C21 179.9(4) . . . . ? Ti C24 C25 C21 -64.8(3) . . . . ? C23 C24 C25 C30 179.9(4) . . . . ? C29 C24 C25 C30 0.3(6) . . . . ? Ti C24 C25 C30 115.7(4) . . . . ? C23 C24 C25 Ti 64.2(3) . . . . ? C29 C24 C25 Ti -115.3(4) . . . . ? N2 C4 N1 C1 179.2(3) . . . . ? C3 C4 N1 C1 1.2(5) . . . . ? N2 C4 N1 Ti 8.8(3) . . . . ? C3 C4 N1 Ti -169.3(3) . . . . ? C2 C1 N1 C4 -9.4(5) . . . . ? C2 C1 N1 Ti 146.8(6) . . . . ? N1 C4 N2 C5 -168.8(3) . . . . ? C3 C4 N2 C5 8.8(7) . . . . ? N1 C4 N2 Ti -8.7(3) . . . . ? C3 C4 N2 Ti 168.9(4) . . . . ? C6 C5 N2 C4 158.0(4) . . . . ? C10 C5 N2 C4 -21.7(6) . . . . ? C6 C5 N2 Ti 9.0(6) . . . . ? C10 C5 N2 Ti -170.6(3) . . . . ? C14 C13 N3 Ti 135.9(16) . . . . ? C18 C13 N3 Ti -46.7(19) . . . . ? C13 N3 Ti N1 96.1(17) . . . . ? C13 N3 Ti N2 164.4(17) . . . . ? C13 N3 Ti C21 -39.3(17) . . . . ? C13 N3 Ti C25 -11.9(18) . . . . ? C13 N3 Ti C22 -73.4(17) . . . . ? C13 N3 Ti C24 -25.7(19) . . . . ? C13 N3 Ti C23 -83.5(17) . . . . ? C4 N1 Ti N3 96.5(2) . . . . ? C1 N1 Ti N3 -61.5(7) . . . . ? C4 N1 Ti N2 -5.6(2) . . . . ? C1 N1 Ti N2 -163.7(7) . . . . ? C4 N1 Ti C21 -150.6(2) . . . . ? C1 N1 Ti C21 51.4(7) . . . . ? C4 N1 Ti C25 -141.5(2) . . . . ? C1 N1 Ti C25 60.5(7) . . . . ? C4 N1 Ti C22 -101.5(3) . . . . ? C1 N1 Ti C22 100.5(7) . . . . ? C4 N1 Ti C24 -107.6(2) . . . . ? C1 N1 Ti C24 94.4(7) . . . . ? C4 N1 Ti C23 -83.8(2) . . . . ? C1 N1 Ti C23 118.2(7) . . . . ? C4 N2 Ti N3 -96.6(2) . . . . ? C5 N2 Ti N3 59.3(4) . . . . ? C4 N2 Ti N1 5.6(2) . . . . ? C5 N2 Ti N1 161.4(4) . . . . ? C4 N2 Ti C21 131.4(3) . . . . ? C5 N2 Ti C21 -72.7(5) . . . . ? C4 N2 Ti C25 78.8(3) . . . . ? C5 N2 Ti C25 -125.4(4) . . . . ? C4 N2 Ti C22 147.0(2) . . . . ? C5 N2 Ti C22 -57.1(4) . . . . ? C4 N2 Ti C24 88.3(2) . . . . ? C5 N2 Ti C24 -115.8(4) . . . . ? C4 N2 Ti C23 121.3(2) . . . . ? C5 N2 Ti C23 -82.8(4) . . . . ? C25 C21 Ti N3 134.7(2) . . . . ? C22 C21 Ti N3 -109.8(2) . . . . ? C26 C21 Ti N3 12.2(3) . . . . ? C25 C21 Ti N1 15.8(3) . . . . ? C22 C21 Ti N1 131.3(2) . . . . ? C26 C21 Ti N1 -106.7(3) . . . . ? C25 C21 Ti N2 -90.3(3) . . . . ? C22 C21 Ti N2 25.2(4) . . . . ? C26 C21 Ti N2 147.2(3) . . . . ? C22 C21 Ti C25 115.5(3) . . . . ? C26 C21 Ti C25 -122.5(4) . . . . ? C25 C21 Ti C22 -115.5(3) . . . . ? C26 C21 Ti C22 122.0(4) . . . . ? C25 C21 Ti C24 -37.7(2) . . . . ? C22 C21 Ti C24 77.9(2) . . . . ? C26 C21 Ti C24 -160.1(4) . . . . ? C25 C21 Ti C23 -78.3(2) . . . . ? C22 C21 Ti C23 37.2(2) . . . . ? C26 C21 Ti C23 159.2(4) . . . . ? C21 C25 Ti N3 -53.2(3) . . . . ? C24 C25 Ti N3 -168.3(2) . . . . ? C30 C25 Ti N3 69.5(3) . . . . ? C21 C25 Ti N1 -168.0(2) . . . . ? C24 C25 Ti N1 76.8(2) . . . . ? C30 C25 Ti N1 -45.3(3) . . . . ? C21 C25 Ti N2 131.8(2) . . . . ? C24 C25 Ti N2 16.6(3) . . . . ? C30 C25 Ti N2 -105.5(3) . . . . ? C24 C25 Ti C21 -115.2(3) . . . . ? C30 C25 Ti C21 122.7(4) . . . . ? C21 C25 Ti C22 37.6(2) . . . . ? C24 C25 Ti C22 -77.5(2) . . . . ? C30 C25 Ti C22 160.3(4) . . . . ? C21 C25 Ti C24 115.2(3) . . . . ? C30 C25 Ti C24 -122.2(4) . . . . ? C21 C25 Ti C23 78.8(2) . . . . ? C24 C25 Ti C23 -36.4(2) . . . . ? C30 C25 Ti C23 -158.5(4) . . . . ? C21 C22 Ti N3 76.0(2) . . . . ? C23 C22 Ti N3 -168.2(2) . . . . ? C27 C22 Ti N3 -45.5(4) . . . . ? C21 C22 Ti N1 -86.3(3) . . . . ? C23 C22 Ti N1 29.4(3) . . . . ? C27 C22 Ti N1 152.1(3) . . . . ? C21 C22 Ti N2 -165.4(2) . . . . ? C23 C22 Ti N2 -49.7(2) . . . . ? C27 C22 Ti N2 73.1(4) . . . . ? C23 C22 Ti C21 115.8(3) . . . . ? C27 C22 Ti C21 -121.5(5) . . . . ? C21 C22 Ti C25 -37.6(2) . . . . ? C23 C22 Ti C25 78.1(2) . . . . ? C27 C22 Ti C25 -159.1(4) . . . . ? C21 C22 Ti C24 -79.1(2) . . . . ? C23 C22 Ti C24 36.7(2) . . . . ? C27 C22 Ti C24 159.4(4) . . . . ? C21 C22 Ti C23 -115.8(3) . . . . ? C27 C22 Ti C23 122.7(5) . . . . ? C23 C24 Ti N3 -95.0(4) . . . . ? C25 C24 Ti N3 21.8(4) . . . . ? C29 C24 Ti N3 143.5(3) . . . . ? C23 C24 Ti N1 138.7(2) . . . . ? C25 C24 Ti N1 -104.4(2) . . . . ? C29 C24 Ti N1 17.2(3) . . . . ? C23 C24 Ti N2 75.3(2) . . . . ? C25 C24 Ti N2 -167.9(2) . . . . ? C29 C24 Ti N2 -46.3(3) . . . . ? C23 C24 Ti C21 -79.0(2) . . . . ? C25 C24 Ti C21 37.9(2) . . . . ? C29 C24 Ti C21 159.5(4) . . . . ? C23 C24 Ti C25 -116.9(3) . . . . ? C29 C24 Ti C25 121.6(4) . . . . ? C23 C24 Ti C22 -37.1(2) . . . . ? C25 C24 Ti C22 79.7(2) . . . . ? C29 C24 Ti C22 -158.7(4) . . . . ? C25 C24 Ti C23 116.9(3) . . . . ? C29 C24 Ti C23 -121.5(4) . . . . ? C24 C23 Ti N3 133.8(3) . . . . ? C22 C23 Ti N3 17.3(3) . . . . ? C28 C23 Ti N3 -105.0(4) . . . . ? C24 C23 Ti N1 -45.8(3) . . . . ? C22 C23 Ti N1 -162.2(2) . . . . ? C28 C23 Ti N1 75.5(4) . . . . ? C24 C23 Ti N2 -107.6(2) . . . . ? C22 C23 Ti N2 135.9(2) . . . . ? C28 C23 Ti N2 13.6(4) . . . . ? C24 C23 Ti C21 78.8(2) . . . . ? C22 C23 Ti C21 -37.7(2) . . . . ? C28 C23 Ti C21 -160.0(4) . . . . ? C24 C23 Ti C25 37.1(2) . . . . ? C22 C23 Ti C25 -79.4(2) . . . . ? C28 C23 Ti C25 158.3(4) . . . . ? C24 C23 Ti C22 116.5(3) . . . . ? C28 C23 Ti C22 -122.3(4) . . . . ? C22 C23 Ti C24 -116.5(3) . . . . ? C28 C23 Ti C24 121.2(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.455 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.084 _audit_block_code ga_kw7 _audit_block_refno 467 _chemical_absolute_configuration ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' #==end== data_complex_11 _database_code_depnum_ccdc_archive 'CCDC 718803' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H59 N3 Ti' _chemical_formula_weight 677.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5091(19) _cell_length_b 12.983(3) _cell_length_c 17.624(4) _cell_angle_alpha 105.994(4) _cell_angle_beta 96.108(4) _cell_angle_gamma 108.513(4) _cell_volume 1937.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 0.254 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6762 _exptl_absorpt_correction_T_max 0.7464 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) SADABS (Sheldrick & Bruker AXS, 2004-2008) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector (Bruker AXS Smart 1000)' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 45869 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 30.03 _reflns_number_total 11314 _reflns_number_gt 7894 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 1997-2003)' _computing_cell_refinement ; SAINT (Bruker AXS, 1997-2008). Includes estimated systematic errors from Monte Carlo simulations. ; _computing_data_reduction 'SAINT (Bruker AXS, 1997-2008)' _computing_structure_solution 'DIRDIF (Beurskens et al., 1999-2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Bond lengths and angles in solvent molecule (pentane) restrained to sensible value. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+0.3031P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11314 _refine_ls_number_parameters 455 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1588 _refine_ls_wR_factor_gt 0.1461 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.125 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1A C 0.5351(2) 0.34720(19) 0.20248(13) 0.0253(4) Uani 0.653(11) 1 d P A 1 H1A1 H 0.6098 0.4214 0.2041 0.030 Uiso 0.653(11) 1 calc PR A 1 H1A2 H 0.5385 0.2852 0.1559 0.030 Uiso 0.653(11) 1 calc PR A 1 C2A C 0.5678(4) 0.3232(5) 0.2816(3) 0.0271(11) Uani 0.653(11) 1 d P A 1 H2A1 H 0.6283 0.2730 0.2765 0.033 Uiso 0.653(11) 1 calc PR A 1 H2A2 H 0.6241 0.3957 0.3266 0.033 Uiso 0.653(11) 1 calc PR A 1 C3A C 0.4132(2) 0.2637(2) 0.29589(14) 0.0279(5) Uani 0.653(11) 1 d P A 1 H3A1 H 0.4104 0.2874 0.3540 0.034 Uiso 0.653(11) 1 calc PR A 1 H3A2 H 0.3815 0.1790 0.2743 0.034 Uiso 0.653(11) 1 calc PR A 1 C1B C 0.5351(2) 0.34720(19) 0.20248(13) 0.0253(4) Uani 0.347(11) 1 d P A 2 H1B1 H 0.6117 0.4239 0.2341 0.030 Uiso 0.347(11) 1 calc PR A 2 H1B2 H 0.5565 0.3238 0.1479 0.030 Uiso 0.347(11) 1 calc PR A 2 C2B C 0.5410(8) 0.2614(9) 0.2435(6) 0.032(2) Uani 0.347(11) 1 d P A 2 H2B1 H 0.6422 0.2852 0.2784 0.039 Uiso 0.347(11) 1 calc PR A 2 H2B2 H 0.5161 0.1841 0.2038 0.039 Uiso 0.347(11) 1 calc PR A 2 C3B C 0.4132(2) 0.2637(2) 0.29589(14) 0.0279(5) Uani 0.347(11) 1 d P A 2 H3B1 H 0.3549 0.1860 0.2968 0.034 Uiso 0.347(11) 1 calc PR A 2 H3B2 H 0.4573 0.3168 0.3519 0.034 Uiso 0.347(11) 1 calc PR A 2 C4 C 0.3169(2) 0.30747(16) 0.24849(11) 0.0197(4) Uani 1 1 d . . . C5 C 0.0890(2) 0.27139(17) 0.30231(12) 0.0197(4) Uani 1 1 d . . . C6 C 0.0184(2) 0.33644(17) 0.34968(12) 0.0210(4) Uani 1 1 d . A . H6 H 0.0382 0.4136 0.3515 0.025 Uiso 1 1 calc R . . C7 C -0.0802(2) 0.28956(18) 0.39410(12) 0.0234(4) Uani 1 1 d . . . C8 C -0.1083(2) 0.17599(19) 0.39115(13) 0.0278(5) Uani 1 1 d . A . H8 H -0.1758 0.1436 0.4216 0.033 Uiso 1 1 calc R . . C9 C -0.0399(3) 0.10989(19) 0.34480(15) 0.0309(5) Uani 1 1 d . . . C10 C 0.0580(2) 0.15755(18) 0.29994(14) 0.0273(4) Uani 1 1 d . A . H10 H 0.1044 0.1123 0.2673 0.033 Uiso 1 1 calc R . . C11 C -0.1539(3) 0.3610(2) 0.44630(14) 0.0339(5) Uani 1 1 d . A . H11A H -0.0993 0.3890 0.5027 0.051 Uiso 1 1 calc R . . H11B H -0.2598 0.3138 0.4418 0.051 Uiso 1 1 calc R . . H11C H -0.1503 0.4266 0.4283 0.051 Uiso 1 1 calc R . . C12 C -0.0731(3) -0.0134(2) 0.3412(2) 0.0518(8) Uani 1 1 d . A . H12A H -0.1020 -0.0230 0.3913 0.078 Uiso 1 1 calc R . . H12B H 0.0177 -0.0325 0.3349 0.078 Uiso 1 1 calc R . . H12C H -0.1565 -0.0646 0.2952 0.078 Uiso 1 1 calc R . . C13 C 0.5403(2) 0.61884(15) 0.32033(11) 0.0158(3) Uani 1 1 d . A . C14 C 0.5612(2) 0.61919(16) 0.40102(11) 0.0172(4) Uani 1 1 d . . . C15 C 0.7078(2) 0.65480(18) 0.44541(12) 0.0222(4) Uani 1 1 d . . . H15 H 0.7227 0.6555 0.4997 0.027 Uiso 1 1 calc R . . C16 C 0.8325(2) 0.68925(19) 0.41194(13) 0.0253(4) Uani 1 1 d . . . H16 H 0.9321 0.7141 0.4433 0.030 Uiso 1 1 calc R . . C17 C 0.8118(2) 0.68737(18) 0.33254(12) 0.0224(4) Uani 1 1 d . . . H17 H 0.8977 0.7105 0.3096 0.027 Uiso 1 1 calc R . . C18 C 0.6668(2) 0.65207(16) 0.28582(11) 0.0173(4) Uani 1 1 d . . . C19 C 0.6471(2) 0.65253(18) 0.20010(12) 0.0217(4) Uani 1 1 d . . . H19A H 0.7469 0.6830 0.1876 0.033 Uiso 1 1 calc R . . H19B H 0.5891 0.7010 0.1935 0.033 Uiso 1 1 calc R . . H19C H 0.5923 0.5739 0.1633 0.033 Uiso 1 1 calc R . . C20 C 0.4279(2) 0.57920(17) 0.43812(11) 0.0194(4) Uani 1 1 d . . . H20A H 0.4635 0.5759 0.4913 0.029 Uiso 1 1 calc R . . H20B H 0.3591 0.5026 0.4032 0.029 Uiso 1 1 calc R . . H20C H 0.3741 0.6331 0.4440 0.029 Uiso 1 1 calc R . . C21 C 0.1407(2) 0.54751(16) 0.27642(11) 0.0171(3) Uani 1 1 d . . . H21 H 0.0449 0.5414 0.2898 0.021 Uiso 1 1 calc R A . C22 C 0.2826(2) 0.62712(16) 0.29971(10) 0.0151(3) Uani 1 1 d . A . C23 C 0.3235(2) 0.75317(16) 0.33740(11) 0.0165(3) Uani 1 1 d . . . C24 C 0.2336(2) 0.79252(17) 0.38722(12) 0.0194(4) Uani 1 1 d . A . H24 H 0.1498 0.7384 0.3972 0.023 Uiso 1 1 calc R . . C25 C 0.2642(2) 0.90836(17) 0.42211(12) 0.0233(4) Uani 1 1 d . . . H25 H 0.2015 0.9327 0.4559 0.028 Uiso 1 1 calc R A . C26 C 0.3857(2) 0.99029(17) 0.40863(12) 0.0227(4) Uani 1 1 d . A . C27 C 0.4761(2) 0.95139(17) 0.35975(13) 0.0241(4) Uani 1 1 d . . . H27 H 0.5600 1.0057 0.3500 0.029 Uiso 1 1 calc R A . C28 C 0.4463(2) 0.83471(17) 0.32489(12) 0.0203(4) Uani 1 1 d . A . H28 H 0.5106 0.8104 0.2922 0.024 Uiso 1 1 calc R . . C29 C 0.4185(3) 1.11691(17) 0.44785(14) 0.0295(5) Uani 1 1 d . . . H29A H 0.3288 1.1344 0.4323 0.044 Uiso 1 1 calc R A . H29B H 0.5043 1.1618 0.4299 0.044 Uiso 1 1 calc R . . H29C H 0.4435 1.1367 0.5067 0.044 Uiso 1 1 calc R . . C30 C 0.0908(2) 0.29898(16) 0.07271(11) 0.0194(4) Uani 1 1 d . . . C31 C -0.0132(2) 0.34754(18) 0.10394(12) 0.0222(4) Uani 1 1 d . A . C32 C 0.0384(3) 0.46488(19) 0.10855(12) 0.0257(4) Uani 1 1 d . . . C33 C 0.1757(3) 0.48952(18) 0.08068(12) 0.0251(4) Uani 1 1 d . A . C34 C 0.2076(2) 0.38678(18) 0.05781(11) 0.0214(4) Uani 1 1 d . A . C35 C 0.0805(3) 0.17718(17) 0.05749(14) 0.0283(5) Uani 1 1 d . A . H35A H 0.0213 0.1300 0.0028 0.042 Uiso 1 1 calc R . . H35B H 0.0306 0.1474 0.0970 0.042 Uiso 1 1 calc R . . H35C H 0.1828 0.1745 0.0627 0.042 Uiso 1 1 calc R . . C36 C -0.1526(2) 0.2866(2) 0.12950(14) 0.0341(5) Uani 1 1 d . . . H36A H -0.2411 0.2589 0.0852 0.051 Uiso 1 1 calc R A . H36B H -0.1672 0.3398 0.1769 0.051 Uiso 1 1 calc R . . H36C H -0.1408 0.2211 0.1432 0.051 Uiso 1 1 calc R . . C37 C -0.0452(3) 0.5463(2) 0.12894(15) 0.0414(6) Uani 1 1 d . A . H37A H -0.0939 0.5516 0.0790 0.062 Uiso 1 1 calc R . . H37B H 0.0266 0.6225 0.1628 0.062 Uiso 1 1 calc R . . H37C H -0.1226 0.5177 0.1583 0.062 Uiso 1 1 calc R . . C38 C 0.2652(3) 0.6044(2) 0.07477(15) 0.0385(6) Uani 1 1 d . . . H38A H 0.3571 0.6010 0.0555 0.058 Uiso 1 1 calc R A . H38B H 0.2935 0.6633 0.1281 0.058 Uiso 1 1 calc R . . H38C H 0.2033 0.6237 0.0368 0.058 Uiso 1 1 calc R . . C39 C 0.3372(3) 0.3707(2) 0.02099(13) 0.0297(5) Uani 1 1 d . . . H39A H 0.3043 0.3403 -0.0380 0.045 Uiso 1 1 calc R A . H39B H 0.3707 0.3164 0.0401 0.045 Uiso 1 1 calc R . . H39C H 0.4215 0.4448 0.0368 0.045 Uiso 1 1 calc R . . C71 C 0.1772(6) 0.8998(4) 0.1648(3) 0.1007(17) Uani 1 1 d D . . H71A H 0.1788 0.8278 0.1717 0.151 Uiso 1 1 calc R . . H71B H 0.0750 0.8879 0.1378 0.151 Uiso 1 1 calc R . . H71C H 0.2053 0.9594 0.2178 0.151 Uiso 1 1 calc R . . C72 C 0.2891(5) 0.9372(5) 0.1140(3) 0.121(2) Uani 1 1 d D . . H72A H 0.2464 0.8877 0.0569 0.145 Uiso 1 1 calc R . . H72B H 0.3033 1.0172 0.1169 0.145 Uiso 1 1 calc R . . C73 C 0.4408(5) 0.9310(4) 0.1405(2) 0.0882(14) Uani 1 1 d D . . H73A H 0.4843 0.9839 0.1966 0.106 Uiso 1 1 calc R . . H73B H 0.4238 0.8521 0.1415 0.106 Uiso 1 1 calc R . . C74 C 0.5556(5) 0.9589(6) 0.0915(3) 0.149(3) Uani 1 1 d D . . H74A H 0.5708 1.0367 0.0887 0.179 Uiso 1 1 calc R . . H74B H 0.5145 0.9040 0.0358 0.179 Uiso 1 1 calc R . . C75 C 0.7081(5) 0.9557(3) 0.1216(3) 0.0840(13) Uani 1 1 d D . . H75A H 0.7534 1.0131 0.1755 0.126 Uiso 1 1 calc R . . H75B H 0.7749 0.9730 0.0845 0.126 Uiso 1 1 calc R . . H75C H 0.6953 0.8791 0.1246 0.126 Uiso 1 1 calc R . . N1 N 0.38217(18) 0.35106(14) 0.19692(10) 0.0195(3) Uani 1 1 d . A . N2 N 0.18424(18) 0.32017(14) 0.25547(10) 0.0186(3) Uani 1 1 d . A . N3 N 0.39327(17) 0.58146(13) 0.27295(9) 0.0161(3) Uani 1 1 d . . . Ti Ti 0.22649(4) 0.44587(3) 0.198812(19) 0.01491(9) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.0219(10) 0.0316(11) 0.0294(11) 0.0115(9) 0.0111(8) 0.0158(9) C2A 0.0225(17) 0.032(2) 0.031(2) 0.0101(19) 0.0019(14) 0.0167(16) C3A 0.0269(11) 0.0347(12) 0.0314(11) 0.0187(10) 0.0065(9) 0.0165(9) C1B 0.0219(10) 0.0316(11) 0.0294(11) 0.0115(9) 0.0111(8) 0.0158(9) C2B 0.026(3) 0.038(5) 0.044(5) 0.022(5) 0.011(3) 0.019(3) C3B 0.0269(11) 0.0347(12) 0.0314(11) 0.0187(10) 0.0065(9) 0.0165(9) C4 0.0240(10) 0.0192(9) 0.0172(9) 0.0052(7) 0.0049(7) 0.0100(8) C5 0.0174(9) 0.0217(9) 0.0193(9) 0.0089(7) 0.0042(7) 0.0041(7) C6 0.0216(9) 0.0191(9) 0.0198(9) 0.0065(7) 0.0068(7) 0.0031(7) C7 0.0185(9) 0.0287(10) 0.0181(9) 0.0060(8) 0.0040(7) 0.0033(8) C8 0.0204(10) 0.0326(11) 0.0289(11) 0.0171(9) 0.0057(8) 0.0012(9) C9 0.0251(11) 0.0281(11) 0.0427(13) 0.0203(10) 0.0078(9) 0.0062(9) C10 0.0268(11) 0.0236(10) 0.0359(12) 0.0141(9) 0.0114(9) 0.0097(9) C11 0.0321(12) 0.0338(12) 0.0305(12) 0.0073(10) 0.0177(10) 0.0044(10) C12 0.0485(17) 0.0361(14) 0.087(2) 0.0409(16) 0.0291(16) 0.0150(13) C13 0.0139(8) 0.0174(8) 0.0171(8) 0.0055(7) 0.0038(6) 0.0071(7) C14 0.0168(9) 0.0184(9) 0.0189(9) 0.0066(7) 0.0059(7) 0.0085(7) C15 0.0210(9) 0.0289(10) 0.0185(9) 0.0073(8) 0.0038(7) 0.0118(8) C16 0.0158(9) 0.0354(12) 0.0250(10) 0.0092(9) 0.0023(7) 0.0109(8) C17 0.0151(9) 0.0273(10) 0.0264(10) 0.0091(8) 0.0077(7) 0.0085(8) C18 0.0164(8) 0.0192(9) 0.0178(8) 0.0061(7) 0.0053(7) 0.0080(7) C19 0.0196(9) 0.0295(10) 0.0207(9) 0.0113(8) 0.0096(7) 0.0108(8) C20 0.0202(9) 0.0240(9) 0.0180(9) 0.0093(8) 0.0073(7) 0.0100(8) C21 0.0146(8) 0.0194(9) 0.0177(8) 0.0057(7) 0.0047(7) 0.0064(7) C22 0.0156(8) 0.0189(8) 0.0129(8) 0.0060(7) 0.0041(6) 0.0080(7) C23 0.0166(8) 0.0184(9) 0.0151(8) 0.0057(7) 0.0015(7) 0.0074(7) C24 0.0176(9) 0.0204(9) 0.0203(9) 0.0060(7) 0.0053(7) 0.0072(7) C25 0.0249(10) 0.0232(10) 0.0234(10) 0.0049(8) 0.0051(8) 0.0133(8) C26 0.0267(10) 0.0192(9) 0.0206(9) 0.0060(7) -0.0025(8) 0.0092(8) C27 0.0211(10) 0.0203(9) 0.0292(10) 0.0107(8) 0.0035(8) 0.0036(8) C28 0.0189(9) 0.0200(9) 0.0223(9) 0.0079(7) 0.0056(7) 0.0065(7) C29 0.0398(13) 0.0167(9) 0.0291(11) 0.0054(8) 0.0005(9) 0.0104(9) C30 0.0187(9) 0.0192(9) 0.0162(8) 0.0025(7) 0.0013(7) 0.0053(7) C31 0.0171(9) 0.0297(10) 0.0180(9) 0.0049(8) 0.0010(7) 0.0093(8) C32 0.0320(11) 0.0291(11) 0.0157(9) 0.0028(8) -0.0029(8) 0.0172(9) C33 0.0339(11) 0.0247(10) 0.0165(9) 0.0093(8) 0.0015(8) 0.0094(9) C34 0.0222(9) 0.0256(10) 0.0151(8) 0.0062(7) 0.0036(7) 0.0072(8) C35 0.0298(11) 0.0196(10) 0.0292(11) 0.0013(8) 0.0038(9) 0.0071(9) C36 0.0181(10) 0.0476(14) 0.0298(11) 0.0054(10) 0.0052(9) 0.0093(10) C37 0.0554(16) 0.0482(15) 0.0263(12) 0.0041(11) -0.0053(11) 0.0378(13) C38 0.0537(16) 0.0275(12) 0.0282(12) 0.0149(10) -0.0046(11) 0.0060(11) C39 0.0280(11) 0.0392(12) 0.0194(10) 0.0079(9) 0.0115(8) 0.0082(10) C71 0.157(5) 0.100(3) 0.066(3) 0.007(2) 0.020(3) 0.092(4) C72 0.080(3) 0.159(6) 0.089(4) 0.023(4) -0.020(3) 0.025(3) C73 0.142(4) 0.060(2) 0.063(2) 0.028(2) 0.028(3) 0.028(3) C74 0.110(4) 0.163(6) 0.135(5) 0.095(5) -0.022(4) -0.028(4) C75 0.095(3) 0.057(2) 0.087(3) 0.019(2) 0.032(3) 0.012(2) N1 0.0201(8) 0.0223(8) 0.0205(8) 0.0078(7) 0.0084(6) 0.0117(7) N2 0.0199(8) 0.0205(8) 0.0192(8) 0.0085(6) 0.0077(6) 0.0094(6) N3 0.0141(7) 0.0191(8) 0.0155(7) 0.0048(6) 0.0041(6) 0.0069(6) Ti 0.01537(16) 0.01637(16) 0.01414(16) 0.00536(12) 0.00420(11) 0.00663(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1A N1 1.465(2) . ? C1A C2A 1.533(4) . ? C1A H1A1 0.9900 . ? C1A H1A2 0.9900 . ? C2A C3A 1.512(4) . ? C2A H2A1 0.9900 . ? C2A H2A2 0.9900 . ? C3A C4 1.513(3) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C2B H2B1 0.9900 . ? C2B H2B2 0.9900 . ? C4 N1 1.308(2) . ? C4 N2 1.337(2) . ? C4 Ti 2.534(2) . ? C5 C6 1.397(3) . ? C5 C10 1.400(3) . ? C5 N2 1.409(2) . ? C6 C7 1.385(3) . ? C6 H6 0.9500 . ? C7 C8 1.397(3) . ? C7 C11 1.509(3) . ? C8 C9 1.382(3) . ? C8 H8 0.9500 . ? C9 C10 1.391(3) . ? C9 C12 1.511(3) . ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.405(2) . ? C13 N3 1.409(2) . ? C13 C14 1.413(3) . ? C14 C15 1.389(3) . ? C14 C20 1.500(3) . ? C15 C16 1.382(3) . ? C15 H15 0.9500 . ? C16 C17 1.384(3) . ? C16 H16 0.9500 . ? C17 C18 1.392(3) . ? C17 H17 0.9500 . ? C18 C19 1.504(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.350(3) . ? C21 Ti 2.0506(19) . ? C21 H21 0.9500 . ? C22 N3 1.424(2) . ? C22 C23 1.487(3) . ? C23 C28 1.390(3) . ? C23 C24 1.398(3) . ? C24 C25 1.378(3) . ? C24 H24 0.9500 . ? C25 C26 1.393(3) . ? C25 H25 0.9500 . ? C26 C27 1.389(3) . ? C26 C29 1.510(3) . ? C27 C28 1.389(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.413(3) . ? C30 C34 1.423(3) . ? C30 C35 1.498(3) . ? C30 Ti 2.3943(19) . ? C31 C32 1.420(3) . ? C31 C36 1.499(3) . ? C31 Ti 2.405(2) . ? C32 C33 1.416(3) . ? C32 C37 1.504(3) . ? C32 Ti 2.384(2) . ? C33 C34 1.421(3) . ? C33 C38 1.502(3) . ? C33 Ti 2.345(2) . ? C34 C39 1.498(3) . ? C34 Ti 2.359(2) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C71 C72 1.511(4) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.503(4) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.480(4) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.508(4) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? N1 Ti 2.2029(16) . ? N2 Ti 2.0950(16) . ? N3 Ti 1.9595(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1A C2A 104.50(19) . . ? N1 C1A H1A1 110.9 . . ? C2A C1A H1A1 110.9 . . ? N1 C1A H1A2 110.9 . . ? C2A C1A H1A2 110.9 . . ? H1A1 C1A H1A2 108.9 . . ? C3A C2A C1A 104.8(2) . . ? C3A C2A H2A1 110.8 . . ? C1A C2A H2A1 110.8 . . ? C3A C2A H2A2 110.8 . . ? C1A C2A H2A2 110.8 . . ? H2A1 C2A H2A2 108.9 . . ? C2A C3A C4 100.45(19) . . ? C2A C3A H3A1 111.7 . . ? C4 C3A H3A1 111.7 . . ? C2A C3A H3A2 111.7 . . ? C4 C3A H3A2 111.7 . . ? H3A1 C3A H3A2 109.5 . . ? H2B1 C2B H2B2 109.2 . . ? N1 C4 N2 114.13(17) . . ? N1 C4 C3A 113.98(17) . . ? N2 C4 C3A 131.49(18) . . ? N1 C4 Ti 60.34(10) . . ? N2 C4 Ti 55.68(9) . . ? C3A C4 Ti 160.16(15) . . ? C6 C5 C10 119.01(18) . . ? C6 C5 N2 119.29(17) . . ? C10 C5 N2 121.64(18) . . ? C7 C6 C5 120.68(19) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 119.18(19) . . ? C6 C7 C11 120.39(19) . . ? C8 C7 C11 120.42(18) . . ? C9 C8 C7 121.24(19) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 119.1(2) . . ? C8 C9 C12 120.7(2) . . ? C10 C9 C12 120.2(2) . . ? C9 C10 C5 120.8(2) . . ? C9 C10 H10 119.6 . . ? C5 C10 H10 119.6 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 N3 119.41(16) . . ? C18 C13 C14 119.90(16) . . ? N3 C13 C14 120.65(16) . . ? C15 C14 C13 119.00(17) . . ? C15 C14 C20 120.03(17) . . ? C13 C14 C20 120.96(16) . . ? C16 C15 C14 121.16(18) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 119.78(19) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C18 120.94(18) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C17 C18 C13 119.20(17) . . ? C17 C18 C19 120.02(17) . . ? C13 C18 C19 120.77(16) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C14 C20 H20A 109.5 . . ? C14 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C14 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 Ti 86.40(12) . . ? C22 C21 H21 136.8 . . ? Ti C21 H21 136.8 . . ? C21 C22 N3 112.84(16) . . ? C21 C22 C23 125.76(17) . . ? N3 C22 C23 120.70(15) . . ? C28 C23 C24 117.86(17) . . ? C28 C23 C22 123.29(17) . . ? C24 C23 C22 118.85(16) . . ? C25 C24 C23 121.24(18) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 C25 C26 121.05(19) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C27 C26 C25 117.81(18) . . ? C27 C26 C29 121.79(19) . . ? C25 C26 C29 120.39(19) . . ? C28 C27 C26 121.36(18) . . ? C28 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? C27 C28 C23 120.67(18) . . ? C27 C28 H28 119.7 . . ? C23 C28 H28 119.7 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C34 107.60(18) . . ? C31 C30 C35 126.55(18) . . ? C34 C30 C35 125.86(18) . . ? C31 C30 Ti 73.29(11) . . ? C34 C30 Ti 71.21(11) . . ? C35 C30 Ti 121.26(13) . . ? C30 C31 C32 108.45(18) . . ? C30 C31 C36 125.9(2) . . ? C32 C31 C36 125.6(2) . . ? C30 C31 Ti 72.46(11) . . ? C32 C31 Ti 71.93(11) . . ? C36 C31 Ti 120.63(14) . . ? C33 C32 C31 107.94(18) . . ? C33 C32 C37 124.7(2) . . ? C31 C32 C37 126.9(2) . . ? C33 C32 Ti 71.08(11) . . ? C31 C32 Ti 73.57(11) . . ? C37 C32 Ti 126.76(14) . . ? C32 C33 C34 107.81(18) . . ? C32 C33 C38 124.5(2) . . ? C34 C33 C38 127.7(2) . . ? C32 C33 Ti 74.07(11) . . ? C34 C33 Ti 72.94(11) . . ? C38 C33 Ti 120.38(14) . . ? C33 C34 C30 108.19(18) . . ? C33 C34 C39 126.56(19) . . ? C30 C34 C39 125.20(19) . . ? C33 C34 Ti 71.89(11) . . ? C30 C34 Ti 73.95(11) . . ? C39 C34 Ti 122.00(14) . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C72 C71 H71A 109.5 . . ? C72 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C72 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C73 C72 C71 112.9(4) . . ? C73 C72 H72A 109.0 . . ? C71 C72 H72A 109.0 . . ? C73 C72 H72B 109.0 . . ? C71 C72 H72B 109.0 . . ? H72A C72 H72B 107.8 . . ? C74 C73 C72 117.2(4) . . ? C74 C73 H73A 108.0 . . ? C72 C73 H73A 108.0 . . ? C74 C73 H73B 108.0 . . ? C72 C73 H73B 108.0 . . ? H73A C73 H73B 107.2 . . ? C73 C74 C75 115.6(4) . . ? C73 C74 H74A 108.4 . . ? C75 C74 H74A 108.4 . . ? C73 C74 H74B 108.4 . . ? C75 C74 H74B 108.4 . . ? H74A C74 H74B 107.4 . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C4 N1 C1A 109.51(16) . . ? C4 N1 Ti 88.59(12) . . ? C1A N1 Ti 151.13(14) . . ? C4 N2 C5 123.51(16) . . ? C4 N2 Ti 92.51(11) . . ? C5 N2 Ti 142.70(13) . . ? C13 N3 C22 122.11(15) . . ? C13 N3 Ti 143.59(13) . . ? C22 N3 Ti 88.05(10) . . ? N3 Ti C21 70.34(7) . . ? N3 Ti N2 106.54(7) . . ? C21 Ti N2 94.24(7) . . ? N3 Ti N1 87.50(7) . . ? C21 Ti N1 142.00(7) . . ? N2 Ti N1 62.15(6) . . ? N3 Ti C33 106.17(7) . . ? C21 Ti C33 101.08(8) . . ? N2 Ti C33 146.95(7) . . ? N1 Ti C33 114.87(7) . . ? N3 Ti C34 122.30(7) . . ? C21 Ti C34 134.41(7) . . ? N2 Ti C34 118.29(7) . . ? N1 Ti C34 83.46(7) . . ? C33 Ti C34 35.17(7) . . ? N3 Ti C32 120.99(7) . . ? C21 Ti C32 77.83(7) . . ? N2 Ti C32 124.51(7) . . ? N1 Ti C32 139.73(7) . . ? C33 Ti C32 34.85(8) . . ? C34 Ti C32 57.83(7) . . ? N3 Ti C30 156.64(7) . . ? C21 Ti C30 126.71(7) . . ? N2 Ti C30 89.23(7) . . ? N1 Ti C30 84.81(7) . . ? C33 Ti C30 58.16(7) . . ? C34 Ti C30 34.84(7) . . ? C32 Ti C30 57.52(7) . . ? N3 Ti C31 154.67(7) . . ? C21 Ti C31 92.47(7) . . ? N2 Ti C31 92.78(7) . . ? N1 Ti C31 116.46(7) . . ? C33 Ti C31 57.74(7) . . ? C34 Ti C31 57.42(7) . . ? C32 Ti C31 34.50(7) . . ? C30 Ti C31 34.25(7) . . ? N3 Ti C4 93.19(7) . . ? C21 Ti C4 117.40(7) . . ? N2 Ti C4 31.81(6) . . ? N1 Ti C4 31.07(6) . . ? C33 Ti C4 141.00(7) . . ? C34 Ti C4 105.99(7) . . ? C32 Ti C4 145.81(7) . . ? C30 Ti C4 91.52(7) . . ? C31 Ti C4 111.52(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1A C2A C3A 24.7(4) . . . . ? C1A C2A C3A C4 -24.3(3) . . . . ? C2A C3A C4 N1 17.1(3) . . . . ? C2A C3A C4 N2 -155.1(3) . . . . ? C2A C3A C4 Ti -51.6(5) . . . . ? C10 C5 C6 C7 0.4(3) . . . . ? N2 C5 C6 C7 177.63(18) . . . . ? C5 C6 C7 C8 0.1(3) . . . . ? C5 C6 C7 C11 178.91(19) . . . . ? C6 C7 C8 C9 -0.1(3) . . . . ? C11 C7 C8 C9 -178.9(2) . . . . ? C7 C8 C9 C10 -0.4(3) . . . . ? C7 C8 C9 C12 -179.1(2) . . . . ? C8 C9 C10 C5 0.9(3) . . . . ? C12 C9 C10 C5 179.6(2) . . . . ? C6 C5 C10 C9 -0.9(3) . . . . ? N2 C5 C10 C9 -178.1(2) . . . . ? C18 C13 C14 C15 1.2(3) . . . . ? N3 C13 C14 C15 178.93(17) . . . . ? C18 C13 C14 C20 -177.30(17) . . . . ? N3 C13 C14 C20 0.4(3) . . . . ? C13 C14 C15 C16 -0.2(3) . . . . ? C20 C14 C15 C16 178.33(19) . . . . ? C14 C15 C16 C17 -0.7(3) . . . . ? C15 C16 C17 C18 0.5(3) . . . . ? C16 C17 C18 C13 0.5(3) . . . . ? C16 C17 C18 C19 179.01(19) . . . . ? N3 C13 C18 C17 -179.08(17) . . . . ? C14 C13 C18 C17 -1.4(3) . . . . ? N3 C13 C18 C19 2.4(3) . . . . ? C14 C13 C18 C19 -179.89(17) . . . . ? Ti C21 C22 N3 -13.83(14) . . . . ? Ti C21 C22 C23 156.59(16) . . . . ? C21 C22 C23 C28 -146.9(2) . . . . ? N3 C22 C23 C28 22.8(3) . . . . ? C21 C22 C23 C24 32.3(3) . . . . ? N3 C22 C23 C24 -157.94(16) . . . . ? C28 C23 C24 C25 0.8(3) . . . . ? C22 C23 C24 C25 -178.45(18) . . . . ? C23 C24 C25 C26 0.2(3) . . . . ? C24 C25 C26 C27 -0.8(3) . . . . ? C24 C25 C26 C29 -179.53(19) . . . . ? C25 C26 C27 C28 0.4(3) . . . . ? C29 C26 C27 C28 179.05(19) . . . . ? C26 C27 C28 C23 0.7(3) . . . . ? C24 C23 C28 C27 -1.3(3) . . . . ? C22 C23 C28 C27 177.96(18) . . . . ? C34 C30 C31 C32 0.0(2) . . . . ? C35 C30 C31 C32 -179.77(19) . . . . ? Ti C30 C31 C32 63.36(14) . . . . ? C34 C30 C31 C36 -178.91(19) . . . . ? C35 C30 C31 C36 1.3(3) . . . . ? Ti C30 C31 C36 -115.5(2) . . . . ? C34 C30 C31 Ti -63.38(13) . . . . ? C35 C30 C31 Ti 116.9(2) . . . . ? C30 C31 C32 C33 -0.5(2) . . . . ? C36 C31 C32 C33 178.39(19) . . . . ? Ti C31 C32 C33 63.21(14) . . . . ? C30 C31 C32 C37 172.32(19) . . . . ? C36 C31 C32 C37 -8.8(3) . . . . ? Ti C31 C32 C37 -124.0(2) . . . . ? C30 C31 C32 Ti -63.70(14) . . . . ? C36 C31 C32 Ti 115.2(2) . . . . ? C31 C32 C33 C34 0.8(2) . . . . ? C37 C32 C33 C34 -172.19(19) . . . . ? Ti C32 C33 C34 65.66(13) . . . . ? C31 C32 C33 C38 178.93(19) . . . . ? C37 C32 C33 C38 5.9(3) . . . . ? Ti C32 C33 C38 -116.2(2) . . . . ? C31 C32 C33 Ti -64.84(14) . . . . ? C37 C32 C33 Ti 122.2(2) . . . . ? C32 C33 C34 C30 -0.8(2) . . . . ? C38 C33 C34 C30 -178.9(2) . . . . ? Ti C33 C34 C30 65.57(13) . . . . ? C32 C33 C34 C39 176.74(19) . . . . ? C38 C33 C34 C39 -1.3(3) . . . . ? Ti C33 C34 C39 -116.9(2) . . . . ? C32 C33 C34 Ti -66.41(14) . . . . ? C38 C33 C34 Ti 115.6(2) . . . . ? C31 C30 C34 C33 0.5(2) . . . . ? C35 C30 C34 C33 -179.72(18) . . . . ? Ti C30 C34 C33 -64.22(13) . . . . ? C31 C30 C34 C39 -177.08(18) . . . . ? C35 C30 C34 C39 2.7(3) . . . . ? Ti C30 C34 C39 118.16(19) . . . . ? C31 C30 C34 Ti 64.75(13) . . . . ? C35 C30 C34 Ti -115.50(19) . . . . ? C71 C72 C73 C74 176.3(5) . . . . ? C72 C73 C74 C75 177.9(5) . . . . ? N2 C4 N1 C1A 171.98(17) . . . . ? C3A C4 N1 C1A -1.7(2) . . . . ? Ti C4 N1 C1A 157.01(17) . . . . ? N2 C4 N1 Ti 14.97(17) . . . . ? C3A C4 N1 Ti -158.66(16) . . . . ? C2A C1A N1 C4 -14.6(3) . . . . ? C2A C1A N1 Ti 111.5(3) . . . . ? N1 C4 N2 C5 174.48(17) . . . . ? C3A C4 N2 C5 -13.3(3) . . . . ? Ti C4 N2 C5 -169.8(2) . . . . ? N1 C4 N2 Ti -15.77(18) . . . . ? C3A C4 N2 Ti 156.5(2) . . . . ? C6 C5 N2 C4 138.2(2) . . . . ? C10 C5 N2 C4 -44.6(3) . . . . ? C6 C5 N2 Ti -24.8(3) . . . . ? C10 C5 N2 Ti 152.41(18) . . . . ? C18 C13 N3 C22 -129.64(18) . . . . ? C14 C13 N3 C22 52.7(2) . . . . ? C18 C13 N3 Ti 88.8(2) . . . . ? C14 C13 N3 Ti -88.9(2) . . . . ? C21 C22 N3 C13 -143.87(17) . . . . ? C23 C22 N3 C13 45.2(2) . . . . ? C21 C22 N3 Ti 14.46(15) . . . . ? C23 C22 N3 Ti -156.50(14) . . . . ? C13 N3 Ti C21 138.9(2) . . . . ? C22 N3 Ti C21 -9.26(10) . . . . ? C13 N3 Ti N2 50.3(2) . . . . ? C22 N3 Ti N2 -97.87(10) . . . . ? C13 N3 Ti N1 -9.6(2) . . . . ? C22 N3 Ti N1 -157.81(10) . . . . ? C13 N3 Ti C33 -124.8(2) . . . . ? C22 N3 Ti C33 86.99(11) . . . . ? C13 N3 Ti C34 -90.3(2) . . . . ? C22 N3 Ti C34 121.54(10) . . . . ? C13 N3 Ti C32 -159.45(19) . . . . ? C22 N3 Ti C32 52.34(12) . . . . ? C13 N3 Ti C30 -80.4(3) . . . . ? C22 N3 Ti C30 131.42(16) . . . . ? C13 N3 Ti C31 -171.43(18) . . . . ? C22 N3 Ti C31 40.36(19) . . . . ? C13 N3 Ti C4 20.9(2) . . . . ? C22 N3 Ti C4 -127.26(10) . . . . ? C22 C21 Ti N3 9.79(10) . . . . ? C22 C21 Ti N2 115.85(11) . . . . ? C22 C21 Ti N1 67.61(16) . . . . ? C22 C21 Ti C33 -93.59(12) . . . . ? C22 C21 Ti C34 -106.60(13) . . . . ? C22 C21 Ti C32 -119.73(12) . . . . ? C22 C21 Ti C30 -151.95(11) . . . . ? C22 C21 Ti C31 -151.18(12) . . . . ? C22 C21 Ti C4 92.98(12) . . . . ? C4 N2 Ti N3 -68.38(12) . . . . ? C5 N2 Ti N3 97.5(2) . . . . ? C4 N2 Ti C21 -139.12(12) . . . . ? C5 N2 Ti C21 26.7(2) . . . . ? C4 N2 Ti N1 9.59(11) . . . . ? C5 N2 Ti N1 175.4(2) . . . . ? C4 N2 Ti C33 103.05(16) . . . . ? C5 N2 Ti C33 -91.1(2) . . . . ? C4 N2 Ti C34 74.08(13) . . . . ? C5 N2 Ti C34 -120.1(2) . . . . ? C4 N2 Ti C32 142.75(12) . . . . ? C5 N2 Ti C32 -51.4(2) . . . . ? C4 N2 Ti C30 94.13(12) . . . . ? C5 N2 Ti C30 -100.0(2) . . . . ? C4 N2 Ti C31 128.20(12) . . . . ? C5 N2 Ti C31 -66.0(2) . . . . ? C5 N2 Ti C4 165.8(3) . . . . ? C4 N1 Ti N3 100.41(12) . . . . ? C1A N1 Ti N3 -29.9(3) . . . . ? C4 N1 Ti C21 47.48(17) . . . . ? C1A N1 Ti C21 -82.8(3) . . . . ? C4 N1 Ti N2 -9.80(11) . . . . ? C1A N1 Ti N2 -140.1(3) . . . . ? C4 N1 Ti C33 -152.92(12) . . . . ? C1A N1 Ti C33 76.8(3) . . . . ? C4 N1 Ti C34 -136.67(12) . . . . ? C1A N1 Ti C34 93.0(3) . . . . ? C4 N1 Ti C32 -121.37(14) . . . . ? C1A N1 Ti C32 108.3(3) . . . . ? C4 N1 Ti C30 -101.67(12) . . . . ? C1A N1 Ti C30 128.0(3) . . . . ? C4 N1 Ti C31 -88.16(13) . . . . ? C1A N1 Ti C31 141.5(3) . . . . ? C1A N1 Ti C4 -130.3(3) . . . . ? C32 C33 Ti N3 -121.46(12) . . . . ? C34 C33 Ti N3 123.68(12) . . . . ? C38 C33 Ti N3 -0.5(2) . . . . ? C32 C33 Ti C21 -48.92(13) . . . . ? C34 C33 Ti C21 -163.78(12) . . . . ? C38 C33 Ti C21 72.1(2) . . . . ? C32 C33 Ti N2 67.10(18) . . . . ? C34 C33 Ti N2 -47.76(19) . . . . ? C38 C33 Ti N2 -171.91(16) . . . . ? C32 C33 Ti N1 143.71(12) . . . . ? C34 C33 Ti N1 28.85(14) . . . . ? C38 C33 Ti N1 -95.30(19) . . . . ? C32 C33 Ti C34 114.86(18) . . . . ? C38 C33 Ti C34 -124.2(2) . . . . ? C34 C33 Ti C32 -114.86(18) . . . . ? C38 C33 Ti C32 121.0(2) . . . . ? C32 C33 Ti C30 77.61(13) . . . . ? C34 C33 Ti C30 -37.24(11) . . . . ? C38 C33 Ti C30 -161.4(2) . . . . ? C32 C33 Ti C31 36.96(12) . . . . ? C34 C33 Ti C31 -77.89(13) . . . . ? C38 C33 Ti C31 158.0(2) . . . . ? C32 C33 Ti C4 121.79(14) . . . . ? C34 C33 Ti C4 6.93(18) . . . . ? C38 C33 Ti C4 -117.23(19) . . . . ? C33 C34 Ti N3 -71.01(14) . . . . ? C30 C34 Ti N3 173.16(11) . . . . ? C39 C34 Ti N3 51.31(19) . . . . ? C33 C34 Ti C21 22.56(17) . . . . ? C30 C34 Ti C21 -93.27(14) . . . . ? C39 C34 Ti C21 144.89(16) . . . . ? C33 C34 Ti N2 152.71(12) . . . . ? C30 C34 Ti N2 36.87(14) . . . . ? C39 C34 Ti N2 -84.97(18) . . . . ? C33 C34 Ti N1 -153.86(13) . . . . ? C30 C34 Ti N1 90.31(12) . . . . ? C39 C34 Ti N1 -31.53(17) . . . . ? C30 C34 Ti C33 -115.83(18) . . . . ? C39 C34 Ti C33 122.3(2) . . . . ? C33 C34 Ti C32 37.77(12) . . . . ? C30 C34 Ti C32 -78.06(13) . . . . ? C39 C34 Ti C32 160.1(2) . . . . ? C33 C34 Ti C30 115.83(17) . . . . ? C39 C34 Ti C30 -121.8(2) . . . . ? C33 C34 Ti C31 78.88(13) . . . . ? C30 C34 Ti C31 -36.95(11) . . . . ? C39 C34 Ti C31 -158.8(2) . . . . ? C33 C34 Ti C4 -175.47(12) . . . . ? C30 C34 Ti C4 68.70(12) . . . . ? C39 C34 Ti C4 -53.15(18) . . . . ? C33 C32 Ti N3 72.88(14) . . . . ? C31 C32 Ti N3 -170.98(11) . . . . ? C37 C32 Ti N3 -46.8(2) . . . . ? C33 C32 Ti C21 130.82(13) . . . . ? C31 C32 Ti C21 -113.05(13) . . . . ? C37 C32 Ti C21 11.1(2) . . . . ? C33 C32 Ti N2 -142.43(12) . . . . ? C31 C32 Ti N2 -26.29(15) . . . . ? C37 C32 Ti N2 97.9(2) . . . . ? C33 C32 Ti N1 -56.18(17) . . . . ? C31 C32 Ti N1 59.96(17) . . . . ? C37 C32 Ti N1 -175.90(18) . . . . ? C31 C32 Ti C33 116.14(17) . . . . ? C37 C32 Ti C33 -119.7(3) . . . . ? C33 C32 Ti C34 -38.13(12) . . . . ? C31 C32 Ti C34 78.00(13) . . . . ? C37 C32 Ti C34 -157.9(2) . . . . ? C33 C32 Ti C30 -79.63(13) . . . . ? C31 C32 Ti C30 36.51(11) . . . . ? C37 C32 Ti C30 160.7(2) . . . . ? C33 C32 Ti C31 -116.14(17) . . . . ? C37 C32 Ti C31 124.1(3) . . . . ? C33 C32 Ti C4 -107.83(16) . . . . ? C31 C32 Ti C4 8.31(19) . . . . ? C37 C32 Ti C4 132.5(2) . . . . ? C31 C30 Ti N3 -130.53(17) . . . . ? C34 C30 Ti N3 -14.7(2) . . . . ? C35 C30 Ti N3 106.4(2) . . . . ? C31 C30 Ti C21 1.37(15) . . . . ? C34 C30 Ti C21 117.19(13) . . . . ? C35 C30 Ti C21 -121.66(16) . . . . ? C31 C30 Ti N2 96.08(12) . . . . ? C34 C30 Ti N2 -148.10(12) . . . . ? C35 C30 Ti N2 -26.95(16) . . . . ? C31 C30 Ti N1 158.18(12) . . . . ? C34 C30 Ti N1 -86.00(12) . . . . ? C35 C30 Ti N1 35.15(16) . . . . ? C31 C30 Ti C33 -78.21(13) . . . . ? C34 C30 Ti C33 37.61(12) . . . . ? C35 C30 Ti C33 158.76(19) . . . . ? C31 C30 Ti C34 -115.82(17) . . . . ? C35 C30 Ti C34 121.1(2) . . . . ? C31 C30 Ti C32 -36.79(12) . . . . ? C34 C30 Ti C32 79.03(13) . . . . ? C35 C30 Ti C32 -159.82(19) . . . . ? C34 C30 Ti C31 115.82(17) . . . . ? C35 C30 Ti C31 -123.0(2) . . . . ? C31 C30 Ti C4 127.81(12) . . . . ? C34 C30 Ti C4 -116.37(12) . . . . ? C35 C30 Ti C4 4.78(16) . . . . ? C30 C31 Ti N3 135.21(16) . . . . ? C32 C31 Ti N3 18.3(2) . . . . ? C36 C31 Ti N3 -102.9(2) . . . . ? C30 C31 Ti C21 -178.90(12) . . . . ? C32 C31 Ti C21 64.20(13) . . . . ? C36 C31 Ti C21 -57.01(18) . . . . ? C30 C31 Ti N2 -84.54(12) . . . . ? C32 C31 Ti N2 158.57(12) . . . . ? C36 C31 Ti N2 37.36(18) . . . . ? C30 C31 Ti N1 -24.42(13) . . . . ? C32 C31 Ti N1 -141.32(12) . . . . ? C36 C31 Ti N1 97.47(17) . . . . ? C30 C31 Ti C33 79.55(13) . . . . ? C32 C31 Ti C33 -37.34(12) . . . . ? C36 C31 Ti C33 -158.6(2) . . . . ? C30 C31 Ti C34 37.61(11) . . . . ? C32 C31 Ti C34 -79.29(13) . . . . ? C36 C31 Ti C34 159.5(2) . . . . ? C30 C31 Ti C32 116.89(17) . . . . ? C36 C31 Ti C32 -121.2(2) . . . . ? C32 C31 Ti C30 -116.89(17) . . . . ? C36 C31 Ti C30 121.9(2) . . . . ? C30 C31 Ti C4 -58.10(13) . . . . ? C32 C31 Ti C4 -174.99(12) . . . . ? C36 C31 Ti C4 63.80(18) . . . . ? N1 C4 Ti N3 -79.78(12) . . . . ? N2 C4 Ti N3 116.81(12) . . . . ? C3A C4 Ti N3 -1.3(4) . . . . ? N1 C4 Ti C21 -149.26(12) . . . . ? N2 C4 Ti C21 47.32(14) . . . . ? C3A C4 Ti C21 -70.8(4) . . . . ? N1 C4 Ti N2 163.42(19) . . . . ? C3A C4 Ti N2 -118.1(5) . . . . ? N2 C4 Ti N1 -163.42(19) . . . . ? C3A C4 Ti N1 78.4(4) . . . . ? N1 C4 Ti C33 41.02(17) . . . . ? N2 C4 Ti C33 -122.40(14) . . . . ? C3A C4 Ti C33 119.5(4) . . . . ? N1 C4 Ti C34 45.16(13) . . . . ? N2 C4 Ti C34 -118.25(12) . . . . ? C3A C4 Ti C34 123.6(4) . . . . ? N1 C4 Ti C32 100.83(16) . . . . ? N2 C4 Ti C32 -62.58(17) . . . . ? C3A C4 Ti C32 179.3(4) . . . . ? N1 C4 Ti C30 77.33(12) . . . . ? N2 C4 Ti C30 -86.09(12) . . . . ? C3A C4 Ti C30 155.8(4) . . . . ? N1 C4 Ti C31 105.88(12) . . . . ? N2 C4 Ti C31 -57.54(13) . . . . ? C3A C4 Ti C31 -175.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.991 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.073 _audit_block_code ga_kw16 _audit_block_refno 625 _chemical_absolute_configuration . _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'