# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2279 data_[1] _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetra(t-butylamine)bis(t-butylimido)dichloro-di-\m- chloroditatanium(IV) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H62 Cl4 N6 Ti2' _chemical_formula_weight 672.40 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.6191(2) _cell_length_b 10.4143(2) _cell_length_c 14.51000(10) _cell_angle_alpha 90.00 _cell_angle_beta 117.7330(10) _cell_angle_gamma 90.00 _cell_volume 1821.59(5) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 6397 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.754 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.7945 _exptl_absorpt_correction_T_max 0.9633 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'Area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10950 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 28.16 _reflns_number_total 4027 _reflns_number_gt 3148 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-97 Sheldrick, (1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+1.4423P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4027 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.40644(3) 0.89387(3) 0.04685(3) 0.01869(10) Uani 1 d . . . Cl1 Cl 0.57393(4) 0.77229(5) 0.15384(4) 0.02747(13) Uani 1 d . . . Cl2 Cl 0.50861(4) 1.09865(5) 0.09662(4) 0.02340(12) Uani 1 d . . . C1 C 0.33427(19) 0.9085(2) 0.22272(17) 0.0278(5) Uani 1 d . . . N1 N 0.35110(14) 0.89733(17) 0.13002(13) 0.0218(4) Uani 1 d . . . C2 C 0.3982(2) 1.0272(3) 0.28388(19) 0.0403(6) Uani 1 d . . . H2A H 0.4760 1.0183 0.3020 0.060 Uiso 1 calc R . . H2B H 0.3908 1.0350 0.3470 0.060 Uiso 1 calc R . . H2C H 0.3682 1.1033 0.2414 0.060 Uiso 1 calc R . . C3 C 0.3808(2) 0.7867(3) 0.2882(2) 0.0408(6) Uani 1 d . . . H3A H 0.3369 0.7131 0.2503 0.061 Uiso 1 calc R . . H3B H 0.3778 0.7954 0.3534 0.061 Uiso 1 calc R . . H3C H 0.4572 0.7744 0.3024 0.061 Uiso 1 calc R . . C4 C 0.2103(2) 0.9212(3) 0.1916(2) 0.0405(6) Uani 1 d . . . H4A H 0.1709 0.8465 0.1516 0.061 Uiso 1 calc R . . H4B H 0.1808 0.9979 0.1498 0.061 Uiso 1 calc R . . H4C H 0.2011 0.9273 0.2539 0.061 Uiso 1 calc R . . N2 N 0.33669(16) 0.71371(16) -0.04891(14) 0.0253(4) Uani 1 d . . . H2D H 0.2821 0.7425 -0.1108 0.030 Uiso 1 calc R . . H2E H 0.3918 0.6854 -0.0626 0.030 Uiso 1 calc R . . C5 C 0.28957(18) 0.5928(2) -0.02697(16) 0.0242(5) Uani 1 d . . . C6 C 0.1909(2) 0.6310(3) -0.0105(2) 0.0441(7) Uani 1 d . . . H6A H 0.2156 0.6876 0.0492 0.066 Uiso 1 calc R . . H6B H 0.1578 0.5546 0.0017 0.066 Uiso 1 calc R . . H6C H 0.1363 0.6750 -0.0720 0.066 Uiso 1 calc R . . C7 C 0.3790(2) 0.5290(2) 0.06990(19) 0.0422(7) Uani 1 d . . . H7A H 0.4425 0.5095 0.0591 0.063 Uiso 1 calc R . . H7B H 0.3502 0.4502 0.0837 0.063 Uiso 1 calc R . . H7C H 0.4015 0.5866 0.1288 0.063 Uiso 1 calc R . . C8 C 0.2512(2) 0.5026(2) -0.12067(19) 0.0351(6) Uani 1 d . . . H8A H 0.3147 0.4756 -0.1291 0.053 Uiso 1 calc R . . H8B H 0.1988 0.5471 -0.1830 0.053 Uiso 1 calc R . . H8C H 0.2157 0.4278 -0.1093 0.053 Uiso 1 calc R . . N3 N 0.27863(14) 1.00350(17) -0.09215(13) 0.0233(4) Uani 1 d . . . H3D H 0.3179 1.0636 -0.1068 0.028 Uiso 1 calc R . . H3E H 0.2535 0.9467 -0.1460 0.028 Uiso 1 calc R . . C9 C 0.17675(18) 1.0725(2) -0.10259(17) 0.0248(5) Uani 1 d . . . C10 C 0.0970(2) 0.9718(3) -0.0999(2) 0.0408(6) Uani 1 d . . . H10A H 0.1330 0.9237 -0.0353 0.061 Uiso 1 calc R . . H10B H 0.0757 0.9136 -0.1583 0.061 Uiso 1 calc R . . H10C H 0.0314 1.0138 -0.1043 0.061 Uiso 1 calc R . . C11 C 0.1224(2) 1.1448(2) -0.20688(18) 0.0354(6) Uani 1 d . . . H11A H 0.1005 1.0840 -0.2637 0.053 Uiso 1 calc R . . H11B H 0.1750 1.2057 -0.2096 0.053 Uiso 1 calc R . . H11C H 0.0575 1.1905 -0.2132 0.053 Uiso 1 calc R . . C12 C 0.2127(2) 1.1678(2) -0.01303(19) 0.0353(6) Uani 1 d . . . H12A H 0.2459 1.1218 0.0526 0.053 Uiso 1 calc R . . H12B H 0.1486 1.2154 -0.0194 0.053 Uiso 1 calc R . . H12C H 0.2666 1.2270 -0.0153 0.053 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.01782(19) 0.01891(18) 0.02102(18) -0.00071(15) 0.01045(15) -0.00133(15) Cl1 0.0220(3) 0.0270(3) 0.0316(3) 0.0019(2) 0.0109(2) 0.0014(2) Cl2 0.0247(3) 0.0225(3) 0.0262(3) -0.0050(2) 0.0146(2) -0.0049(2) C1 0.0294(12) 0.0334(12) 0.0269(11) 0.0025(10) 0.0184(10) 0.0036(10) N1 0.0207(9) 0.0231(9) 0.0229(9) 0.0013(7) 0.0113(8) 0.0010(8) C2 0.0491(16) 0.0437(15) 0.0332(13) -0.0089(11) 0.0234(13) -0.0030(13) C3 0.0487(16) 0.0451(15) 0.0339(13) 0.0133(12) 0.0237(13) 0.0079(13) C4 0.0365(14) 0.0549(17) 0.0419(14) 0.0042(12) 0.0281(12) 0.0046(13) N2 0.0309(10) 0.0199(9) 0.0260(9) 0.0004(7) 0.0142(8) -0.0035(8) C5 0.0264(12) 0.0194(10) 0.0254(11) 0.0008(8) 0.0109(9) -0.0051(9) C6 0.0386(15) 0.0418(15) 0.0611(18) -0.0124(13) 0.0310(14) -0.0141(12) C7 0.0454(16) 0.0318(14) 0.0343(13) 0.0090(11) 0.0058(12) -0.0047(12) C8 0.0459(15) 0.0219(11) 0.0328(13) -0.0031(9) 0.0144(11) -0.0073(11) N3 0.0207(9) 0.0241(9) 0.0260(9) 0.0000(7) 0.0116(8) 0.0002(8) C9 0.0210(11) 0.0240(11) 0.0278(11) 0.0025(9) 0.0100(9) 0.0047(9) C10 0.0245(13) 0.0432(15) 0.0547(17) 0.0103(13) 0.0184(13) -0.0018(11) C11 0.0334(14) 0.0359(13) 0.0315(12) 0.0063(10) 0.0104(11) 0.0079(11) C12 0.0447(15) 0.0271(12) 0.0352(13) 0.0006(10) 0.0196(12) 0.0106(11) _geom_special_details ; ? ; 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 Ti N1 1.6947(17) . y Ti N2 2.2638(17) . y Ti N3 2.2657(17) . y Ti Cl1 2.4332(6) . y Ti Cl2 2.4639(6) . y Ti Cl2 2.8142(6) 3_675 y Cl2 Ti 2.8142(6) 3_675 ? C1 N1 1.471(3) . y C1 C2 1.534(3) . ? C1 C3 1.535(3) . ? C1 C4 1.537(3) . ? N2 C5 1.513(3) . y C5 C7 1.519(3) . ? C5 C6 1.524(3) . ? C5 C8 1.531(3) . ? N3 C9 1.506(3) . y C9 C10 1.524(3) . ? C9 C12 1.524(3) . ? C9 C11 1.537(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 Ti N2 104.83(8) . . y N1 Ti N3 102.19(7) . . y N2 Ti N3 86.69(7) . . y N1 Ti Cl1 98.75(6) . . y N2 Ti Cl1 87.79(5) . . y N3 Ti Cl1 159.06(5) . . y N1 Ti Cl2 98.66(6) . . y N2 Ti Cl2 156.31(5) . . y N3 Ti Cl2 85.41(5) . . y Cl1 Ti Cl2 91.69(2) . . y N1 Ti Cl2 176.65(6) . 3_675 ? N2 Ti Cl2 76.61(5) . 3_675 ? N3 Ti Cl2 74.79(4) . 3_675 ? Cl1 Ti Cl2 84.28(2) . 3_675 ? Cl2 Ti Cl2 79.770(19) . 3_675 ? Ti Cl2 Ti 100.230(19) . 3_675 y N1 C1 C2 107.76(18) . . ? N1 C1 C3 107.82(18) . . ? C2 C1 C3 110.4(2) . . ? N1 C1 C4 110.84(18) . . ? C2 C1 C4 110.5(2) . . ? C3 C1 C4 109.5(2) . . ? C1 N1 Ti 164.43(16) . . ? C5 N2 Ti 131.20(13) . . ? N2 C5 C7 108.81(18) . . ? N2 C5 C6 107.88(18) . . ? C7 C5 C6 110.8(2) . . ? N2 C5 C8 109.09(17) . . ? C7 C5 C8 110.4(2) . . ? C6 C5 C8 109.7(2) . . ? C9 N3 Ti 128.32(13) . . ? N3 C9 C10 107.69(18) . . ? N3 C9 C12 108.02(18) . . ? C10 C9 C12 112.1(2) . . ? N3 C9 C11 109.38(18) . . ? C10 C9 C11 109.9(2) . . ? C12 C9 C11 109.65(19) . . ? _diffrn_measured_fraction_theta_max 0.856 _diffrn_reflns_theta_full 28.16 _diffrn_measured_fraction_theta_full 0.856 _refine_diff_density_max 0.351 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.064 #===END data_[3] _audit_creation_method SHELXL-97 _chemical_name_systematic ; dichloro-di-\m-chlorobis(2-methylphenylimido)tetrakis- pyridinedititanium(IV) dichloromethane solvate ; _chemical_name_common ? _chemical_formula_moiety 'C34 H32 Cl4 N6 Ti2, C H2 Cl2' _chemical_formula_sum 'C18 H18 Cl4 N3 Ti' _chemical_formula_weight 466.05 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'p 21/c' 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 9.90300(9) _cell_length_b 15.9595(2) _cell_length_c 13.57730(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.1590(10) _cell_angle_gamma 90.00 _cell_volume 2105.32(3) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 0.921 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.8230 _exptl_absorpt_correction_T_max 0.8372 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'Area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12936 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.11 _reflns_number_total 4717 _reflns_number_gt 3929 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-97 Sheldrick, (1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+1.7746P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4717 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0948 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 1.338 _refine_ls_shift/su_mean 0.016 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.45440(4) 0.00987(2) 0.13664(3) 0.02395(10) Uani 1 d . . . Cl1 Cl 0.63050(6) -0.00937(3) 0.28109(4) 0.03165(13) Uani 1 d . . . Cl2 Cl 0.33631(5) 0.02125(3) -0.03914(3) 0.02702(12) Uani 1 d . . . N1 N 0.32170(18) 0.02968(11) 0.19740(13) 0.0283(4) Uani 1 d . . . C11 C 0.2300(2) 0.04234(12) 0.26111(16) 0.0281(4) Uani 1 d . . . C12 C 0.0902(2) 0.06124(14) 0.22413(17) 0.0345(5) Uani 1 d . . . C13 C 0.0030(3) 0.07033(17) 0.2927(2) 0.0455(6) Uani 1 d . . . H13A H -0.0906 0.0821 0.2689 0.055 Uiso 1 calc R . . C14 C 0.0508(3) 0.06247(18) 0.3948(2) 0.0504(7) Uani 1 d . . . H14A H -0.0103 0.0687 0.4394 0.061 Uiso 1 calc R . . C15 C 0.1875(3) 0.04558(17) 0.43140(19) 0.0472(6) Uani 1 d . . . H15A H 0.2196 0.0408 0.5010 0.057 Uiso 1 calc R . . C16 C 0.2785(3) 0.03555(14) 0.36628(17) 0.0369(5) Uani 1 d . . . C17 C 0.0365(3) 0.07127(19) 0.11379(19) 0.0488(6) Uani 1 d . . . H17A H -0.0612 0.0590 0.0989 0.073 Uiso 1 calc R . . H17B H 0.0845 0.0329 0.0770 0.073 Uiso 1 calc R . . H17C H 0.0516 0.1284 0.0940 0.073 Uiso 1 calc R . . N2 N 0.40750(19) -0.12671(11) 0.12219(12) 0.0286(4) Uani 1 d . . . C22 C 0.2752(2) -0.15192(14) 0.10559(16) 0.0349(5) Uani 1 d . . . H22A H 0.2057 -0.1110 0.0976 0.042 Uiso 1 calc R . . C23 C 0.2375(3) -0.23550(16) 0.09979(19) 0.0440(6) Uani 1 d . . . H23A H 0.1441 -0.2508 0.0877 0.053 Uiso 1 calc R . . C24 C 0.3384(3) -0.29603(15) 0.11193(18) 0.0476(7) Uani 1 d . . . H24A H 0.3152 -0.3532 0.1087 0.057 Uiso 1 calc R . . C25 C 0.4743(3) -0.27105(15) 0.12901(17) 0.0428(6) Uani 1 d . . . H25A H 0.5453 -0.3110 0.1379 0.051 Uiso 1 calc R . . C26 C 0.5045(3) -0.18628(14) 0.13283(16) 0.0342(5) Uani 1 d . . . H26A H 0.5973 -0.1698 0.1434 0.041 Uiso 1 calc R . . N3 N 0.50433(19) 0.14475(11) 0.12543(12) 0.0284(4) Uani 1 d . . . C32 C 0.4015(3) 0.20113(14) 0.11345(17) 0.0348(5) Uani 1 d . . . H32A H 0.3104 0.1815 0.1047 0.042 Uiso 1 calc R . . C33 C 0.4236(3) 0.28643(15) 0.11348(19) 0.0440(6) Uani 1 d . . . H33A H 0.3491 0.3240 0.1045 0.053 Uiso 1 calc R . . C34 C 0.5564(3) 0.31563(15) 0.12681(19) 0.0472(7) Uani 1 d . . . H34A H 0.5742 0.3735 0.1286 0.057 Uiso 1 calc R . . C35 C 0.6627(3) 0.25918(16) 0.13743(18) 0.0423(6) Uani 1 d . . . H35A H 0.7542 0.2778 0.1452 0.051 Uiso 1 calc R . . C36 C 0.6333(2) 0.17436(14) 0.13653(16) 0.0329(5) Uani 1 d . . . H36A H 0.7065 0.1359 0.1440 0.039 Uiso 1 calc R . . C1 C 0.0780(4) 0.1395(2) 0.7607(3) 0.0720(10) Uani 1 d . . . H1A H 0.1526 0.0983 0.7686 0.086 Uiso 1 calc R . . H1B H -0.0051 0.1109 0.7724 0.086 Uiso 1 calc R . . Cl3 Cl 0.04841(12) 0.17929(9) 0.63844(9) 0.0999(4) Uani 1 d . . . Cl4 Cl 0.12213(11) 0.21930(7) 0.84997(10) 0.0945(3) Uani 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 Ti 0.02831(19) 0.02115(18) 0.02253(17) -0.00027(13) 0.00528(14) 0.00065(14) Cl1 0.0371(3) 0.0300(3) 0.0256(2) 0.00185(19) 0.0007(2) 0.0001(2) Cl2 0.0284(2) 0.0281(2) 0.0241(2) 0.00004(18) 0.00414(18) 0.00221(18) N1 0.0321(9) 0.0267(9) 0.0264(8) -0.0014(7) 0.0061(7) 0.0006(7) C11 0.0336(11) 0.0204(9) 0.0322(10) -0.0027(8) 0.0111(9) -0.0027(8) C12 0.0355(12) 0.0318(11) 0.0370(12) -0.0022(9) 0.0087(10) -0.0027(9) C13 0.0392(13) 0.0463(14) 0.0552(16) -0.0015(12) 0.0199(12) 0.0001(11) C14 0.0586(17) 0.0514(16) 0.0496(15) 0.0008(12) 0.0312(13) 0.0006(13) C15 0.0684(18) 0.0446(14) 0.0320(12) 0.0015(10) 0.0178(12) -0.0038(13) C16 0.0516(14) 0.0302(11) 0.0305(11) -0.0007(9) 0.0121(10) -0.0020(10) C17 0.0420(14) 0.0595(17) 0.0429(14) -0.0036(12) 0.0032(11) 0.0004(12) N2 0.0370(10) 0.0246(8) 0.0246(8) 0.0024(7) 0.0068(7) -0.0002(7) C22 0.0396(12) 0.0323(11) 0.0328(11) 0.0024(9) 0.0074(9) -0.0052(9) C23 0.0543(15) 0.0389(13) 0.0392(13) 0.0002(10) 0.0104(11) -0.0167(11) C24 0.083(2) 0.0264(11) 0.0350(12) -0.0006(9) 0.0153(13) -0.0102(12) C25 0.0701(18) 0.0276(11) 0.0306(11) 0.0026(9) 0.0094(11) 0.0117(11) C26 0.0431(13) 0.0301(11) 0.0291(10) 0.0018(9) 0.0061(9) 0.0047(9) N3 0.0361(10) 0.0240(8) 0.0250(8) -0.0026(7) 0.0053(7) -0.0013(7) C32 0.0417(13) 0.0274(11) 0.0362(12) -0.0016(9) 0.0094(10) 0.0045(9) C33 0.0655(17) 0.0270(11) 0.0414(13) -0.0008(10) 0.0150(12) 0.0088(11) C34 0.082(2) 0.0241(11) 0.0395(13) -0.0046(9) 0.0203(13) -0.0088(12) C35 0.0546(15) 0.0391(13) 0.0352(12) -0.0049(10) 0.0138(11) -0.0185(11) C36 0.0393(12) 0.0311(11) 0.0281(10) -0.0017(8) 0.0061(9) -0.0030(9) C1 0.062(2) 0.0449(17) 0.112(3) 0.0072(18) 0.025(2) 0.0077(14) Cl3 0.0778(7) 0.1209(10) 0.1028(8) 0.0148(7) 0.0218(6) 0.0170(6) Cl4 0.0777(6) 0.0767(6) 0.1293(9) -0.0241(6) 0.0209(6) 0.0234(5) _geom_special_details ; ? ; 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 Ti N1 1.7109(18) . y Ti N3 2.2204(17) . y Ti N2 2.2294(17) . y Ti Cl1 2.3788(6) . y Ti Cl2 2.4528(6) . y Ti Cl2 2.7123(6) 3_655 y Cl2 Ti 2.7123(6) 3_655 ? N1 C11 1.385(3) . y C11 C12 1.411(3) . ? C11 C16 1.420(3) . ? C12 C13 1.395(3) . ? C12 C17 1.498(3) . ? C13 C14 1.380(4) . ? C14 C15 1.376(4) . ? C15 C16 1.388(3) . ? N2 C26 1.339(3) . ? N2 C22 1.347(3) . ? C22 C23 1.383(3) . ? C23 C24 1.377(4) . ? C24 C25 1.379(4) . ? C25 C26 1.384(3) . ? N3 C36 1.342(3) . ? N3 C32 1.345(3) . ? C32 C33 1.379(3) . ? C33 C34 1.374(4) . ? C34 C35 1.372(4) . ? C35 C36 1.384(3) . ? C1 Cl3 1.749(4) . ? C1 Cl4 1.754(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ti N3 93.21(7) . . y N1 Ti N2 93.25(8) . . y N3 Ti N2 170.82(6) . . y N1 Ti Cl1 97.77(6) . . y N3 Ti Cl1 92.53(5) . . y N2 Ti Cl1 93.05(5) . . y N1 Ti Cl2 100.92(6) . . y N3 Ti Cl2 86.11(5) . . y N2 Ti Cl2 86.26(5) . . y Cl1 Ti Cl2 161.30(2) . . y N1 Ti Cl2 179.63(6) . 3_655 ? N3 Ti Cl2 86.72(5) . 3_655 ? N2 Ti Cl2 86.78(5) . 3_655 ? Cl1 Ti Cl2 82.60(2) . 3_655 ? Cl2 Ti Cl2 78.710(19) . 3_655 ? Ti Cl2 Ti 101.291(19) . 3_655 ? C11 N1 Ti 170.35(16) . . y N1 C11 C12 121.72(19) . . ? N1 C11 C16 118.9(2) . . ? C12 C11 C16 119.4(2) . . ? C13 C12 C11 118.4(2) . . ? C13 C12 C17 120.7(2) . . ? C11 C12 C17 120.8(2) . . ? C14 C13 C12 121.7(2) . . ? C15 C14 C13 120.1(2) . . ? C14 C15 C16 120.5(2) . . ? C15 C16 C11 119.8(2) . . ? C26 N2 C22 117.4(2) . . ? C26 N2 Ti 123.49(15) . . ? C22 N2 Ti 119.09(15) . . ? N2 C22 C23 122.7(2) . . ? C24 C23 C22 119.2(2) . . ? C23 C24 C25 118.6(2) . . ? C24 C25 C26 119.1(2) . . ? N2 C26 C25 123.0(2) . . ? C36 N3 C32 117.36(19) . . ? C36 N3 Ti 123.59(15) . . ? C32 N3 Ti 118.90(15) . . ? N3 C32 C33 123.0(2) . . ? C34 C33 C32 118.9(2) . . ? C35 C34 C33 119.1(2) . . ? C34 C35 C36 119.0(2) . . ? N3 C36 C35 122.7(2) . . ? Cl3 C1 Cl4 111.46(19) . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 28.11 _diffrn_measured_fraction_theta_full 0.889 _refine_diff_density_max 0.750 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.058 #===END data_[4] _audit_creation_method SHELXL-97 _chemical_name_systematic ; dichloro-di-\m-chloro(2-t-butylphenylimido)tetrakis- pyridinedititanium(IV) bis(dichloromethane) solvate ; _chemical_name_common ? _chemical_formula_moiety 'C40 H46 Cl4 N6 Ti2, 2(C H2 Cl2)' _chemical_formula_sum 'C22 H27 Cl6 N3 Ti' _chemical_formula_weight 594.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.042 _cell_length_b 10.73410(10) _cell_length_c 16.4281(2) _cell_angle_alpha 77.0130(10) _cell_angle_beta 77.1400(9) _cell_angle_gamma 84.5900(10) _cell_volume 1345.67(2) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 5528 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description Prism _exptl_crystal_colour Brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.930 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.7189 _exptl_absorpt_correction_T_max 0.8008 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'Area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13769 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 28.59 _reflns_number_total 6103 _reflns_number_gt 5181 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-97 Sheldrick, (1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0983P)^2^+1.0795P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6103 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1548 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.003 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti -0.01183(5) 0.64514(4) 0.40019(3) 0.02184(14) Uani 1 d . . . Cl1 Cl -0.26178(8) 0.77633(6) 0.39435(4) 0.03260(17) Uani 1 d . . . Cl2 Cl 0.18876(7) 0.47462(6) 0.44840(4) 0.02547(15) Uani 1 d . . . N1 N 0.1234(3) 0.7087(2) 0.30768(13) 0.0253(4) Uani 1 d . . . C1 C 0.2609(3) 0.7377(3) 0.24061(16) 0.0267(5) Uani 1 d . . . C2 C 0.2574(3) 0.8353(3) 0.16745(16) 0.0282(5) Uani 1 d . . . C3 C 0.4058(4) 0.8487(3) 0.10479(18) 0.0365(6) Uani 1 d . . . H3 H 0.4061 0.9117 0.0547 0.044 Uiso 1 calc R . . C4 C 0.5513(4) 0.7746(4) 0.1124(2) 0.0452(8) Uani 1 d . . . H4 H 0.6485 0.7867 0.0679 0.054 Uiso 1 calc R . . C5 C 0.5557(4) 0.6833(4) 0.1844(2) 0.0489(8) Uani 1 d . . . H5 H 0.6566 0.6337 0.1909 0.059 Uiso 1 calc R . . C6 C 0.4099(4) 0.6644(3) 0.2479(2) 0.0395(7) Uani 1 d . . . H6 H 0.4120 0.6003 0.2972 0.047 Uiso 1 calc R . . C7 C 0.0997(3) 0.9217(3) 0.15669(17) 0.0311(6) Uani 1 d . . . C8 C 0.1314(5) 1.0246(4) 0.0747(2) 0.0486(8) Uani 1 d . . . H8A H 0.0297 1.0802 0.0719 0.073 Uiso 1 calc R . . H8B H 0.1587 0.9843 0.0258 0.073 Uiso 1 calc R . . H8C H 0.2261 1.0745 0.0744 0.073 Uiso 1 calc R . . C9 C -0.0452(4) 0.8420(3) 0.1543(2) 0.0394(7) Uani 1 d . . . H9A H -0.1440 0.8978 0.1444 0.059 Uiso 1 calc R . . H9B H -0.0748 0.7817 0.2084 0.059 Uiso 1 calc R . . H9C H -0.0092 0.7955 0.1086 0.059 Uiso 1 calc R . . C10 C 0.0465(4) 0.9915(3) 0.23019(19) 0.0369(6) Uani 1 d . . . H10A H -0.0537 1.0470 0.2225 0.055 Uiso 1 calc R . . H10B H 0.1391 1.0424 0.2313 0.055 Uiso 1 calc R . . H10C H 0.0201 0.9295 0.2837 0.055 Uiso 1 calc R . . N2 N -0.1165(3) 0.5087(2) 0.34515(14) 0.0280(4) Uani 1 d . . . C21 C -0.2783(4) 0.4741(3) 0.36976(19) 0.0336(6) Uani 1 d . . . H21 H -0.3489 0.5047 0.4156 0.040 Uiso 1 calc R . . C22 C -0.3459(4) 0.3964(3) 0.3313(2) 0.0410(7) Uani 1 d . . . H22 H -0.4601 0.3734 0.3508 0.049 Uiso 1 calc R . . C23 C -0.2447(5) 0.3530(3) 0.2643(2) 0.0505(8) Uani 1 d . . . H23 H -0.2888 0.3010 0.2358 0.061 Uiso 1 calc R . . C24 C -0.0783(5) 0.3859(4) 0.2390(2) 0.0527(9) Uani 1 d . . . H24 H -0.0055 0.3558 0.1935 0.063 Uiso 1 calc R . . C25 C -0.0196(4) 0.4632(3) 0.2809(2) 0.0401(7) Uani 1 d . . . H25 H 0.0952 0.4852 0.2633 0.048 Uiso 1 calc R . . N3 N 0.0773(3) 0.7601(2) 0.47505(14) 0.0266(4) Uani 1 d . . . C31 C 0.2418(3) 0.7873(3) 0.45807(18) 0.0328(6) Uani 1 d . . . H31 H 0.3172 0.7555 0.4140 0.039 Uiso 1 calc R . . C32 C 0.3048(4) 0.8591(3) 0.5020(2) 0.0391(6) Uani 1 d . . . H32 H 0.4216 0.8755 0.4887 0.047 Uiso 1 calc R . . C33 C 0.1964(4) 0.9070(3) 0.5656(2) 0.0401(7) Uani 1 d . . . H33 H 0.2364 0.9577 0.5964 0.048 Uiso 1 calc R . . C34 C 0.0274(4) 0.8790(3) 0.5833(2) 0.0404(7) Uani 1 d . . . H34 H -0.0505 0.9102 0.6268 0.049 Uiso 1 calc R . . C35 C -0.0263(4) 0.8062(3) 0.53763(19) 0.0335(6) Uani 1 d . . . H35 H -0.1422 0.7874 0.5508 0.040 Uiso 1 calc R . . C50 C 0.7174(13) 0.4379(8) -0.0649(6) 0.142(3) Uani 1 d . . . H50A H 0.6120 0.3911 -0.0439 0.170 Uiso 1 calc R . . H50B H 0.7847 0.4026 -0.1127 0.170 Uiso 1 calc R . . Cl3 Cl 0.6633(4) 0.5941(2) -0.1031(3) 0.224(2) Uani 1 d . . . Cl4 Cl 0.8241(7) 0.4087(6) 0.0107(3) 0.261(2) Uani 1 d . . . C51 C -0.4687(5) 1.0164(4) 0.2454(2) 0.0509(8) Uani 1 d . . . H51A H -0.5495 0.9562 0.2415 0.061 Uiso 1 calc R . . H51B H -0.3698 0.9667 0.2635 0.061 Uiso 1 calc R . . Cl5 Cl -0.40245(15) 1.11431(10) 0.14535(7) 0.0650(3) Uani 1 d . . . Cl6 Cl -0.56514(14) 1.10486(12) 0.32081(8) 0.0682(3) Uani 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 Ti 0.0183(2) 0.0236(2) 0.0212(2) -0.00129(16) -0.00124(15) -0.00365(15) Cl1 0.0241(3) 0.0319(3) 0.0387(3) -0.0032(3) -0.0056(2) 0.0020(2) Cl2 0.0195(3) 0.0281(3) 0.0244(3) -0.0008(2) 0.0003(2) -0.0019(2) N1 0.0215(9) 0.0288(11) 0.0235(10) -0.0009(8) -0.0035(8) -0.0043(8) C1 0.0225(11) 0.0313(13) 0.0242(11) -0.0012(10) -0.0024(9) -0.0078(9) C2 0.0265(12) 0.0337(13) 0.0238(11) -0.0022(10) -0.0050(9) -0.0092(10) C3 0.0341(14) 0.0453(17) 0.0253(12) 0.0015(11) -0.0002(11) -0.0132(12) C4 0.0290(14) 0.062(2) 0.0364(15) -0.0013(14) 0.0054(12) -0.0115(13) C5 0.0241(13) 0.061(2) 0.0483(18) 0.0027(16) 0.0053(13) 0.0001(13) C6 0.0281(13) 0.0442(17) 0.0359(15) 0.0059(12) 0.0009(11) -0.0022(12) C7 0.0296(12) 0.0339(14) 0.0278(12) 0.0023(10) -0.0088(10) -0.0057(10) C8 0.0499(18) 0.0515(19) 0.0357(16) 0.0133(14) -0.0119(14) -0.0052(15) C9 0.0309(14) 0.0501(18) 0.0403(15) -0.0062(13) -0.0155(12) -0.0065(12) C10 0.0394(15) 0.0326(14) 0.0378(15) -0.0035(12) -0.0093(12) -0.0032(11) N2 0.0270(10) 0.0294(11) 0.0278(10) -0.0047(8) -0.0060(8) -0.0052(8) C21 0.0294(13) 0.0341(14) 0.0370(14) -0.0021(11) -0.0096(11) -0.0065(11) C22 0.0385(15) 0.0364(15) 0.0503(17) -0.0028(13) -0.0167(14) -0.0102(12) C23 0.062(2) 0.0446(18) 0.054(2) -0.0140(15) -0.0226(17) -0.0167(16) C24 0.060(2) 0.055(2) 0.0487(19) -0.0265(17) -0.0024(16) -0.0116(17) C25 0.0390(15) 0.0447(17) 0.0378(15) -0.0141(13) -0.0026(12) -0.0073(13) N3 0.0244(10) 0.0258(10) 0.0277(10) -0.0027(8) -0.0028(8) -0.0053(8) C31 0.0255(12) 0.0359(14) 0.0362(14) -0.0053(11) -0.0051(11) -0.0061(10) C32 0.0325(14) 0.0385(16) 0.0482(17) -0.0080(13) -0.0103(12) -0.0093(12) C33 0.0446(16) 0.0337(15) 0.0487(17) -0.0133(13) -0.0187(14) -0.0033(12) C34 0.0411(16) 0.0404(16) 0.0441(16) -0.0198(13) -0.0080(13) 0.0005(13) C35 0.0290(13) 0.0343(14) 0.0375(14) -0.0107(11) -0.0033(11) -0.0035(11) C50 0.176(9) 0.108(6) 0.132(7) -0.038(5) 0.007(6) -0.028(6) Cl3 0.167(2) 0.1037(16) 0.302(4) -0.013(2) 0.117(3) 0.0164(16) Cl4 0.268(5) 0.342(6) 0.217(4) -0.068(4) -0.101(4) -0.090(4) C51 0.0471(18) 0.0444(18) 0.064(2) -0.0064(16) -0.0191(17) -0.0077(15) Cl5 0.0780(7) 0.0570(6) 0.0581(6) -0.0053(4) -0.0175(5) -0.0022(5) Cl6 0.0532(5) 0.0786(7) 0.0728(7) -0.0238(6) 0.0014(5) -0.0181(5) _geom_special_details ; ? ; 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 Ti N1 1.702(2) . y Ti N3 2.189(2) . y Ti N2 2.200(2) . y Ti Cl1 2.3502(7) . y Ti Cl2 2.4373(7) . y Ti Cl2 2.6825(7) 2_566 y Cl2 Ti 2.6826(7) 2_566 ? N1 C1 1.379(3) . y C1 C6 1.383(4) . ? C1 C2 1.410(3) . ? C2 C3 1.387(4) . ? C2 C7 1.518(4) . ? C3 C4 1.365(5) . ? C4 C5 1.362(5) . ? C5 C6 1.382(4) . ? C7 C9 1.522(4) . ? C7 C10 1.522(4) . ? C7 C8 1.526(4) . ? N2 C25 1.324(4) . ? N2 C21 1.335(3) . ? C21 C22 1.365(4) . ? C22 C23 1.361(5) . ? C23 C24 1.365(5) . ? C24 C25 1.364(5) . ? N3 C35 1.328(4) . ? N3 C31 1.336(3) . ? C31 C32 1.364(4) . ? C32 C33 1.367(5) . ? C33 C34 1.372(4) . ? C34 C35 1.353(4) . ? C50 Cl4 1.620(10) . ? C50 Cl3 1.705(9) . ? C51 Cl6 1.732(4) . ? C51 Cl5 1.740(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ti N3 93.89(9) . . y N1 Ti N2 94.87(9) . . y N3 Ti N2 170.64(8) . . y N1 Ti Cl1 103.05(8) . . y N3 Ti Cl1 91.80(6) . . y N2 Ti Cl1 89.44(6) . . y N1 Ti Cl2 95.39(7) . . y N3 Ti Cl2 87.68(6) . . y N2 Ti Cl2 88.21(6) . . y Cl1 Ti Cl2 161.54(3) . . y N1 Ti Cl2 172.32(7) . 2_566 ? N3 Ti Cl2 84.70(6) . 2_566 ? N2 Ti Cl2 86.18(6) . 2_566 ? Cl1 Ti Cl2 84.56(2) . 2_566 ? Cl2 Ti Cl2 77.02(2) . 2_566 ? Ti Cl2 Ti 102.98(2) . 2_566 y C1 N1 Ti 165.91(19) . . ? N1 C1 C6 116.2(2) . . ? N1 C1 C2 124.3(2) . . ? C6 C1 C2 119.6(2) . . ? C3 C2 C1 116.7(3) . . ? C3 C2 C7 121.1(2) . . ? C1 C2 C7 122.2(2) . . ? C4 C3 C2 123.1(3) . . ? C5 C4 C3 120.0(3) . . ? C4 C5 C6 119.1(3) . . ? C5 C6 C1 121.6(3) . . ? C2 C7 C9 109.6(2) . . ? C2 C7 C10 110.1(2) . . ? C9 C7 C10 109.8(2) . . ? C2 C7 C8 112.2(2) . . ? C9 C7 C8 108.4(2) . . ? C10 C7 C8 106.6(3) . . ? C25 N2 C21 117.2(3) . . ? C25 N2 Ti 119.45(19) . . ? C21 N2 Ti 123.24(19) . . ? N2 C21 C22 123.0(3) . . ? C23 C22 C21 118.7(3) . . ? C22 C23 C24 119.1(3) . . ? C25 C24 C23 118.8(3) . . ? N2 C25 C24 123.2(3) . . ? C35 N3 C31 117.3(2) . . ? C35 N3 Ti 122.74(18) . . ? C31 N3 Ti 119.92(18) . . ? N3 C31 C32 122.7(3) . . ? C31 C32 C33 119.3(3) . . ? C32 C33 C34 118.1(3) . . ? C35 C34 C33 119.5(3) . . ? N3 C35 C34 123.1(3) . . ? Cl4 C50 Cl3 117.1(6) . . ? Cl6 C51 Cl5 111.6(2) . . ? _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 28.59 _diffrn_measured_fraction_theta_full 0.887 _refine_diff_density_max 0.992 _refine_diff_density_min -1.210 _refine_diff_density_rms 0.101 #===END data_[5] _audit_creation_method SHELXL-97 _chemical_name_systematic ; dichloro-di-\m-chloro(2-phenylphenylimido)tetrakis- pyridinedititanium(IV) ; _chemical_name_common ? _chemical_formula_moiety 'C44 H38 Cl4 N6 Ti2' _chemical_formula_sum 'C22 H19 Cl2 N3 Ti' _chemical_formula_weight 444.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.1087(4) _cell_length_b 17.1958(6) _cell_length_c 12.4949(5) _cell_angle_alpha 90.00 _cell_angle_beta 111.420(1) _cell_angle_gamma 90.00 _cell_volume 2021.97(13) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 6880 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description Prism _exptl_crystal_colour Brown _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.8122 _exptl_absorpt_correction_T_max 0.8962 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'Area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12622 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 28.26 _reflns_number_total 4557 _reflns_number_gt 3588 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-97 Sheldrick, (1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+1.4688P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4557 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.110 _refine_ls_shift/su_mean 0.021 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.15355(4) 0.04794(2) 0.13394(3) 0.02076(11) Uani 1 d . . . Cl1 Cl 0.12670(6) 0.09936(3) 0.30304(5) 0.02894(14) Uani 1 d . . . Cl2 Cl 0.12320(6) -0.01164(3) -0.05165(5) 0.02496(13) Uani 1 d . . . N1 N 0.3351(2) 0.05670(11) 0.17762(16) 0.0237(4) Uani 1 d . . . N2 N 0.1641(2) -0.06879(11) 0.20991(16) 0.0259(4) Uani 1 d . . . N3 N 0.0784(2) 0.16399(11) 0.05284(16) 0.0254(4) Uani 1 d . . . C1 C 0.4797(2) 0.04816(13) 0.23409(19) 0.0240(5) Uani 1 d . . . C2 C 0.5287(3) 0.00626(15) 0.3382(2) 0.0305(5) Uani 1 d . . . H2A H 0.4625 -0.0172 0.3648 0.037 Uiso 1 calc R . . C3 C 0.6724(3) -0.00108(16) 0.4022(2) 0.0380(6) Uani 1 d . . . H3A H 0.7030 -0.0294 0.4714 0.046 Uiso 1 calc R . . C4 C 0.7710(3) 0.03358(17) 0.3637(2) 0.0399(7) Uani 1 d . . . H4A H 0.8687 0.0296 0.4075 0.048 Uiso 1 calc R . . C5 C 0.7254(3) 0.07382(16) 0.2610(2) 0.0339(6) Uani 1 d . . . H5A H 0.7933 0.0962 0.2353 0.041 Uiso 1 calc R . . C6 C 0.5814(2) 0.08223(14) 0.1942(2) 0.0262(5) Uani 1 d . . . C7 C 0.5378(2) 0.12548(14) 0.0830(2) 0.0276(5) Uani 1 d . . . C8 C 0.5964(3) 0.19846(15) 0.0782(2) 0.0351(6) Uani 1 d . . . H8A H 0.6632 0.2200 0.1453 0.042 Uiso 1 calc R . . C9 C 0.5572(3) 0.23934(17) -0.0241(3) 0.0437(7) Uani 1 d . . . H9A H 0.5957 0.2889 -0.0255 0.052 Uiso 1 calc R . . C10 C 0.4617(3) 0.20761(19) -0.1241(3) 0.0457(7) Uani 1 d . . . H10A H 0.4356 0.2354 -0.1935 0.055 Uiso 1 calc R . . C11 C 0.4046(3) 0.13479(18) -0.1217(2) 0.0397(6) Uani 1 d . . . H11A H 0.3410 0.1126 -0.1897 0.048 Uiso 1 calc R . . C12 C 0.4418(3) 0.09451(15) -0.0182(2) 0.0306(5) Uani 1 d . . . H12A H 0.4012 0.0455 -0.0168 0.037 Uiso 1 calc R . . C13 C 0.0834(3) -0.08856(16) 0.2711(2) 0.0330(6) Uani 1 d . . . H13A H 0.0311 -0.0495 0.2904 0.040 Uiso 1 calc R . . C14 C 0.0746(3) -0.16329(16) 0.3062(2) 0.0406(7) Uani 1 d . . . H14A H 0.0186 -0.1747 0.3500 0.049 Uiso 1 calc R . . C15 C 0.1489(3) -0.22169(16) 0.2768(2) 0.0418(7) Uani 1 d . . . H15A H 0.1408 -0.2737 0.2968 0.050 Uiso 1 calc R . . C16 C 0.2350(3) -0.20179(15) 0.2174(2) 0.0360(6) Uani 1 d . . . H16A H 0.2894 -0.2399 0.1984 0.043 Uiso 1 calc R . . C17 C 0.2405(3) -0.12542(15) 0.1861(2) 0.0298(5) Uani 1 d . . . H17A H 0.3005 -0.1124 0.1464 0.036 Uiso 1 calc R . . C18 C 0.1435(3) 0.20032(15) -0.0094(2) 0.0327(6) Uani 1 d . . . H18A H 0.2120 0.1728 -0.0287 0.039 Uiso 1 calc R . . C19 C 0.1144(3) 0.27640(16) -0.0464(2) 0.0415(7) Uani 1 d . . . H19A H 0.1620 0.2998 -0.0900 0.050 Uiso 1 calc R . . C20 C 0.0144(3) 0.31732(16) -0.0182(2) 0.0437(7) Uani 1 d . . . H20A H -0.0058 0.3694 -0.0409 0.052 Uiso 1 calc R . . C21 C -0.0551(3) 0.28084(15) 0.0436(2) 0.0375(6) Uani 1 d . . . H21A H -0.1243 0.3075 0.0632 0.045 Uiso 1 calc R . . C22 C -0.0223(3) 0.20467(14) 0.0765(2) 0.0294(5) Uani 1 d . . . H22A H -0.0720 0.1798 0.1173 0.035 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0185(2) 0.0200(2) 0.0252(2) 0.00057(16) 0.00962(16) -0.00018(16) Cl1 0.0334(3) 0.0273(3) 0.0283(3) -0.0032(2) 0.0139(2) -0.0006(2) Cl2 0.0204(3) 0.0282(3) 0.0287(3) -0.0034(2) 0.0119(2) -0.0017(2) N1 0.0200(9) 0.0248(10) 0.0278(9) 0.0011(8) 0.0104(8) -0.0006(8) N2 0.0241(10) 0.0243(10) 0.0298(10) 0.0015(8) 0.0102(8) 0.0010(8) N3 0.0231(10) 0.0236(10) 0.0292(10) 0.0007(8) 0.0091(8) -0.0006(8) C1 0.0206(11) 0.0247(12) 0.0277(11) -0.0033(9) 0.0100(9) 0.0013(9) C2 0.0286(13) 0.0321(14) 0.0302(12) 0.0004(11) 0.0101(10) 0.0017(10) C3 0.0378(15) 0.0427(16) 0.0286(13) 0.0019(12) 0.0062(11) 0.0075(12) C4 0.0216(13) 0.0509(17) 0.0406(15) -0.0023(13) 0.0033(11) 0.0093(12) C5 0.0215(12) 0.0433(16) 0.0387(14) -0.0059(12) 0.0131(11) 0.0004(11) C6 0.0219(11) 0.0270(12) 0.0301(12) -0.0051(10) 0.0102(10) -0.0002(9) C7 0.0216(12) 0.0304(13) 0.0358(13) 0.0001(10) 0.0165(10) 0.0041(10) C8 0.0300(13) 0.0343(14) 0.0479(15) -0.0023(12) 0.0226(12) -0.0014(11) C9 0.0472(17) 0.0364(16) 0.0603(19) 0.0076(14) 0.0347(15) 0.0024(13) C10 0.0480(17) 0.0569(19) 0.0436(16) 0.0171(15) 0.0303(14) 0.0150(15) C11 0.0347(14) 0.0551(18) 0.0346(14) 0.0025(13) 0.0188(12) 0.0078(13) C12 0.0241(12) 0.0357(14) 0.0352(13) -0.0014(11) 0.0146(10) 0.0017(10) C13 0.0332(14) 0.0331(14) 0.0365(13) 0.0037(11) 0.0172(11) 0.0000(11) C14 0.0439(16) 0.0381(16) 0.0427(15) 0.0080(12) 0.0191(13) -0.0080(13) C15 0.0441(16) 0.0263(14) 0.0428(15) 0.0101(12) 0.0014(13) -0.0047(12) C16 0.0359(14) 0.0266(13) 0.0381(14) 0.0019(11) 0.0049(12) 0.0075(11) C17 0.0271(12) 0.0308(13) 0.0302(12) 0.0024(10) 0.0088(10) 0.0046(10) C18 0.0309(13) 0.0344(14) 0.0336(13) 0.0044(11) 0.0127(11) -0.0021(11) C19 0.0467(17) 0.0374(16) 0.0389(15) 0.0105(12) 0.0138(13) -0.0084(13) C20 0.0530(18) 0.0246(14) 0.0437(16) 0.0083(12) 0.0059(14) 0.0034(13) C21 0.0393(15) 0.0280(14) 0.0407(14) 0.0002(11) 0.0094(12) 0.0094(11) C22 0.0254(12) 0.0284(13) 0.0350(13) -0.0010(11) 0.0117(10) 0.0000(10) _geom_special_details ; ? ; 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 Ti N1 1.7194(19) . y Ti N2 2.206(2) . y Ti N3 2.2415(19) . y Ti Cl1 2.3956(7) . y Ti Cl2 2.4498(7) . y Ti Cl2 2.6781(7) 3 y Cl2 Ti 2.6781(7) 3 ? N1 C1 1.380(3) . y N2 C17 1.342(3) . ? N2 C13 1.349(3) . ? N3 C18 1.343(3) . ? N3 C22 1.353(3) . ? C1 C2 1.409(3) . ? C1 C6 1.421(3) . ? C2 C3 1.384(4) . ? C3 C4 1.390(4) . ? C4 C5 1.380(4) . ? C5 C6 1.396(3) . ? C6 C7 1.494(3) . ? C7 C12 1.389(3) . ? C7 C8 1.398(3) . ? C8 C9 1.383(4) . ? C9 C10 1.382(4) . ? C10 C11 1.383(4) . ? C11 C12 1.392(4) . ? C13 C14 1.371(4) . ? C14 C15 1.382(4) . ? C15 C16 1.377(4) . ? C16 C17 1.377(4) . ? C18 C19 1.383(4) . ? C19 C20 1.379(4) . ? C20 C21 1.371(4) . ? C21 C22 1.377(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 Ti N2 93.73(8) . . y N1 Ti N3 102.23(8) . . y N2 Ti N3 163.65(7) . . y N1 Ti Cl1 98.00(7) . . y N2 Ti Cl1 87.68(5) . . y N3 Ti Cl1 86.63(5) . . y N1 Ti Cl2 95.01(7) . . y N2 Ti Cl2 89.80(5) . . y N3 Ti Cl2 92.28(5) . . y Cl1 Ti Cl2 166.88(3) . . y N1 Ti Cl2 170.54(7) . 3 ? N2 Ti Cl2 80.36(5) . 3 ? N3 Ti Cl2 84.24(5) . 3 ? Cl1 Ti Cl2 89.18(2) . 3 ? Cl2 Ti Cl2 77.70(2) . 3 ? Ti Cl2 Ti 102.30(2) . 3 ? C1 N1 Ti 164.11(17) . . y C17 N2 C13 117.3(2) . . ? C17 N2 Ti 120.40(16) . . ? C13 N2 Ti 121.94(16) . . ? C18 N3 C22 116.9(2) . . ? C18 N3 Ti 121.27(16) . . ? C22 N3 Ti 121.28(16) . . ? N1 C1 C2 118.4(2) . . ? N1 C1 C6 122.9(2) . . ? C2 C1 C6 118.6(2) . . ? C3 C2 C1 121.4(2) . . ? C2 C3 C4 119.7(2) . . ? C5 C4 C3 119.9(2) . . ? C4 C5 C6 122.0(2) . . ? C5 C6 C1 118.5(2) . . ? C5 C6 C7 119.8(2) . . ? C1 C6 C7 121.7(2) . . ? C12 C7 C8 118.1(2) . . ? C12 C7 C6 121.8(2) . . ? C8 C7 C6 120.1(2) . . ? C9 C8 C7 120.9(3) . . ? C10 C9 C8 120.3(3) . . ? C9 C10 C11 119.8(3) . . ? C10 C11 C12 119.8(3) . . ? C7 C12 C11 121.1(3) . . ? N2 C13 C14 122.7(3) . . ? C13 C14 C15 119.4(3) . . ? C16 C15 C14 118.3(2) . . ? C15 C16 C17 119.3(3) . . ? N2 C17 C16 122.9(2) . . ? N3 C18 C19 123.0(3) . . ? C20 C19 C18 118.9(3) . . ? C21 C20 C19 119.0(3) . . ? C20 C21 C22 119.1(3) . . ? N3 C22 C21 123.0(2) . . ? _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.881 _refine_diff_density_max 0.350 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.069 #===END data_[6] _audit_creation_method SHELXL-97 _chemical_name_systematic ; dichloro(2-t-butylphenylimido)(N,N,N',N'-tetramethylethylenediamine)- titanium(IV) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H29 Cl2 N3 Ti' _chemical_formula_weight 382.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 15.1800(4) _cell_length_b 7.5428(2) _cell_length_c 17.0488(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.7150(10) _cell_angle_gamma 90.00 _cell_volume 1951.93(9) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 4105 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description Tablet _exptl_crystal_colour Orange _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.713 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.8093 _exptl_absorpt_correction_T_max 0.9652 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'Area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11970 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0698 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 28.22 _reflns_number_total 4337 _reflns_number_gt 2941 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-97 Sheldrick, (1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+1.2176P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0013(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4337 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0974 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.66539(3) 0.59172(6) 0.18671(3) 0.02230(14) Uani 1 d . . . Cl1 Cl 0.55862(5) 0.36906(9) 0.16876(5) 0.0347(2) Uani 1 d . . . Cl2 Cl 0.68497(5) 0.54626(10) 0.32038(4) 0.0374(2) Uani 1 d . . . N1 N 0.75688(14) 0.5047(3) 0.14303(12) 0.0247(5) Uani 1 d . . . N2 N 0.72101(15) 0.8651(3) 0.20405(13) 0.0286(5) Uani 1 d . . . N3 N 0.58552(15) 0.7578(3) 0.09784(13) 0.0283(5) Uani 1 d . . . C1 C 0.83486(17) 0.4051(3) 0.13983(16) 0.0240(6) Uani 1 d . . . C2 C 0.87116(17) 0.3362(4) 0.06951(16) 0.0289(7) Uani 1 d . . . C3 C 0.94609(19) 0.2302(4) 0.07723(18) 0.0366(7) Uani 1 d . . . H3A H 0.9697 0.1789 0.0318 0.044 Uiso 1 calc R . . C4 C 0.98747(19) 0.1968(4) 0.14900(19) 0.0382(8) Uani 1 d . . . H4A H 1.0381 0.1252 0.1515 0.046 Uiso 1 calc R . . C5 C 0.95375(18) 0.2694(4) 0.21612(18) 0.0338(7) Uani 1 d . . . H5A H 0.9820 0.2503 0.2648 0.041 Uiso 1 calc R . . C6 C 0.87794(18) 0.3709(4) 0.21154(16) 0.0279(6) Uani 1 d . . . H6A H 0.8546 0.4183 0.2578 0.034 Uiso 1 calc R . . C7 C 0.83185(19) 0.3803(4) -0.01150(16) 0.0356(7) Uani 1 d . . . C8 C 0.8855(2) 0.3011(6) -0.07915(19) 0.0617(11) Uani 1 d . . . H8A H 0.8872 0.1730 -0.0741 0.093 Uiso 1 calc R . . H8B H 0.9451 0.3477 -0.0771 0.093 Uiso 1 calc R . . H8C H 0.8580 0.3327 -0.1289 0.093 Uiso 1 calc R . . C9 C 0.7378(2) 0.3053(4) -0.01929(18) 0.0385(8) Uani 1 d . . . H9A H 0.7031 0.3444 0.0249 0.058 Uiso 1 calc R . . H9B H 0.7401 0.1768 -0.0199 0.058 Uiso 1 calc R . . H9C H 0.7108 0.3474 -0.0677 0.058 Uiso 1 calc R . . C10 C 0.8323(2) 0.5830(4) -0.02224(18) 0.0450(8) Uani 1 d . . . H10A H 0.8014 0.6382 0.0208 0.067 Uiso 1 calc R . . H10B H 0.8033 0.6132 -0.0714 0.067 Uiso 1 calc R . . H10C H 0.8927 0.6252 -0.0228 0.067 Uiso 1 calc R . . C11 C 0.7107(2) 0.9550(4) 0.12672(18) 0.0424(8) Uani 1 d . . . H11A H 0.7484 0.8973 0.0881 0.051 Uiso 1 calc R . . H11B H 0.7290 1.0792 0.1314 0.051 Uiso 1 calc R . . C12 C 0.6161(2) 0.9456(4) 0.0999(2) 0.0468(9) Uani 1 d . . . H12A H 0.5793 1.0140 0.1358 0.056 Uiso 1 calc R . . H12B H 0.6102 0.9978 0.0475 0.056 Uiso 1 calc R . . C13 C 0.81655(19) 0.8578(4) 0.2243(2) 0.0413(8) Uani 1 d . . . H13A H 0.8393 0.9773 0.2297 0.062 Uiso 1 calc R . . H13B H 0.8478 0.7968 0.1829 0.062 Uiso 1 calc R . . H13C H 0.8248 0.7944 0.2733 0.062 Uiso 1 calc R . . C14 C 0.6760(2) 0.9698(4) 0.26577(18) 0.0409(8) Uani 1 d . . . H14A H 0.6967 1.0914 0.2645 0.061 Uiso 1 calc R . . H14B H 0.6890 0.9188 0.3168 0.061 Uiso 1 calc R . . H14C H 0.6129 0.9675 0.2562 0.061 Uiso 1 calc R . . C15 C 0.48928(19) 0.7575(4) 0.11464(19) 0.0407(8) Uani 1 d . . . H15A H 0.4592 0.8382 0.0791 0.061 Uiso 1 calc R . . H15B H 0.4801 0.7952 0.1683 0.061 Uiso 1 calc R . . H15C H 0.4660 0.6387 0.1075 0.061 Uiso 1 calc R . . C16 C 0.5962(2) 0.6854(4) 0.01739(16) 0.0363(7) Uani 1 d . . . H16A H 0.5580 0.7493 -0.0188 0.055 Uiso 1 calc R . . H16B H 0.5806 0.5607 0.0170 0.055 Uiso 1 calc R . . H16C H 0.6570 0.6989 0.0015 0.055 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0246(3) 0.0181(2) 0.0242(3) 0.0003(2) -0.00130(19) -0.0009(2) Cl1 0.0330(4) 0.0230(4) 0.0479(5) -0.0021(3) -0.0019(3) -0.0060(3) Cl2 0.0449(5) 0.0406(5) 0.0267(4) 0.0049(3) 0.0005(3) -0.0038(3) N1 0.0264(13) 0.0236(12) 0.0241(12) 0.0000(10) -0.0020(10) -0.0026(10) N2 0.0325(13) 0.0221(12) 0.0311(13) -0.0003(10) -0.0065(11) -0.0037(10) N3 0.0341(13) 0.0209(12) 0.0297(13) -0.0027(10) -0.0071(11) 0.0012(10) C1 0.0224(13) 0.0216(14) 0.0280(15) 0.0009(12) -0.0006(11) -0.0030(12) C2 0.0242(15) 0.0332(17) 0.0291(16) -0.0012(13) 0.0004(12) -0.0043(12) C3 0.0278(16) 0.0441(19) 0.0381(19) -0.0050(15) 0.0051(14) 0.0044(14) C4 0.0233(15) 0.0402(19) 0.051(2) 0.0043(16) 0.0008(14) 0.0064(14) C5 0.0260(15) 0.0418(19) 0.0335(17) 0.0078(14) -0.0055(13) -0.0033(14) C6 0.0306(15) 0.0276(16) 0.0255(15) 0.0001(12) -0.0009(12) -0.0028(12) C7 0.0327(16) 0.052(2) 0.0222(15) -0.0047(14) 0.0035(12) 0.0017(15) C8 0.053(2) 0.102(3) 0.0303(19) -0.009(2) 0.0047(17) 0.015(2) C9 0.0387(18) 0.0445(19) 0.0322(17) -0.0028(15) -0.0062(14) -0.0025(15) C10 0.0377(18) 0.062(2) 0.0350(18) 0.0159(17) 0.0007(14) -0.0089(17) C11 0.063(2) 0.0240(16) 0.0394(19) 0.0086(14) -0.0105(17) -0.0153(15) C12 0.070(2) 0.0217(17) 0.048(2) 0.0049(15) -0.0259(18) 0.0000(15) C13 0.0303(16) 0.0373(18) 0.056(2) -0.0044(16) -0.0072(15) -0.0103(14) C14 0.048(2) 0.0314(18) 0.044(2) -0.0129(15) -0.0052(16) 0.0033(15) C15 0.0345(17) 0.044(2) 0.043(2) -0.0008(15) -0.0027(15) 0.0155(15) C16 0.0391(18) 0.0409(19) 0.0288(17) -0.0004(14) -0.0057(13) 0.0031(14) _geom_special_details ; ? ; 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 Ti N1 1.715(2) . y Ti N2 2.247(2) . y Ti N3 2.300(2) . y Ti Cl2 2.3200(9) . y Ti Cl1 2.3514(8) . y N1 C1 1.404(3) . y N2 C13 1.487(4) . ? N2 C14 1.489(4) . ? N2 C11 1.489(4) . y N3 C16 1.487(3) . ? N3 C12 1.491(4) . y N3 C15 1.492(4) . ? C1 C6 1.403(4) . ? C1 C2 1.424(4) . ? C2 C3 1.396(4) . ? C2 C7 1.534(4) . ? C3 C4 1.391(4) . ? C4 C5 1.373(4) . ? C5 C6 1.383(4) . ? C7 C10 1.540(4) . ? C7 C9 1.540(4) . ? C7 C8 1.541(4) . ? C11 C12 1.503(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ti N2 95.95(10) . . y N1 Ti N3 110.22(9) . . y N2 Ti N3 77.33(8) . . y N1 Ti Cl2 105.99(8) . . y N2 Ti Cl2 87.88(6) . . y N3 Ti Cl2 141.96(6) . . y N1 Ti Cl1 103.34(8) . . y N2 Ti Cl1 158.45(6) . . y N3 Ti Cl1 86.94(6) . . y Cl2 Ti Cl1 95.85(3) . . y C1 N1 Ti 155.48(19) . . y C13 N2 C14 108.1(2) . . ? C13 N2 C11 108.3(2) . . ? C14 N2 C11 109.9(2) . . ? C13 N2 Ti 111.10(17) . . ? C14 N2 Ti 113.88(18) . . ? C11 N2 Ti 105.45(16) . . ? C16 N3 C12 109.5(2) . . ? C16 N3 C15 107.1(2) . . ? C12 N3 C15 107.6(2) . . ? C16 N3 Ti 110.16(17) . . ? C12 N3 Ti 109.90(17) . . ? C15 N3 Ti 112.44(18) . . ? C6 C1 N1 116.7(2) . . ? C6 C1 C2 119.1(2) . . ? N1 C1 C2 124.3(2) . . ? C3 C2 C1 117.0(3) . . ? C3 C2 C7 121.1(3) . . ? C1 C2 C7 121.9(2) . . ? C4 C3 C2 123.0(3) . . ? C5 C4 C3 119.5(3) . . ? C4 C5 C6 119.5(3) . . ? C5 C6 C1 122.0(3) . . ? C2 C7 C10 108.6(2) . . ? C2 C7 C9 110.4(2) . . ? C10 C7 C9 111.1(3) . . ? C2 C7 C8 112.7(3) . . ? C10 C7 C8 107.0(3) . . ? C9 C7 C8 106.9(3) . . ? N2 C11 C12 109.7(3) . . ? N3 C12 C11 110.4(2) . . ? _diffrn_measured_fraction_theta_max 0.839 _diffrn_reflns_theta_full 28.22 _diffrn_measured_fraction_theta_full 0.839 _refine_diff_density_max 0.355 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.074 #===END data_[7] _audit_creation_method SHELXL-97 _chemical_name_systematic ; dichloro-di-\m-chloro(2-phenylphenylimido)bis(N,N,N',N'- tetraethylenediamine)dititanium(IV) ; _chemical_name_common ? _chemical_formula_moiety 'C18 H25 Cl2 N3 Ti' _chemical_formula_sum 'C18 H25 Cl2 N3 Ti' _chemical_formula_weight 402.21 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7374(5) _cell_length_b 10.4470(7) _cell_length_c 12.5090(9) _cell_angle_alpha 75.8640(10) _cell_angle_beta 80.6930(10) _cell_angle_gamma 77.2650(10) _cell_volume 950.15(11) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 4048 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description Tablet _exptl_crystal_colour Brown _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 420 _exptl_absorpt_coefficient_mu 0.736 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_min 0.8489 _exptl_absorpt_correction_T_max 0.9711 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'Area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7248 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.41 _reflns_number_total 3830 _reflns_number_gt 2966 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-97 Sheldrick, (1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+0.2647P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3830 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1124 _refine_ls_wR_factor_gt 0.1000 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.005 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti -0.00174(6) 0.67141(5) 0.38205(4) 0.01982(14) Uani 1 d . . . Cl1 Cl -0.22090(10) 0.79574(7) 0.49241(6) 0.03245(19) Uani 1 d . . . Cl2 Cl -0.11566(9) 0.46328(6) 0.42134(5) 0.02501(17) Uani 1 d . . . N1 N -0.0916(3) 0.7293(2) 0.25839(17) 0.0207(5) Uani 1 d . . . N2 N 0.1785(3) 0.8265(2) 0.3649(2) 0.0280(5) Uani 1 d . . . N3 N 0.2680(3) 0.5765(2) 0.29747(19) 0.0262(5) Uani 1 d . . . C1 C -0.1718(3) 0.7418(3) 0.1636(2) 0.0220(6) Uani 1 d . . . C2 C -0.2425(3) 0.8683(3) 0.0981(2) 0.0229(6) Uani 1 d . . . C3 C -0.3052(4) 0.8709(3) -0.0010(2) 0.0289(6) Uani 1 d . . . H3A H -0.3481 0.9545 -0.0462 0.035 Uiso 1 calc R . . C4 C -0.3063(4) 0.7540(3) -0.0353(2) 0.0336(7) Uani 1 d . . . H4A H -0.3490 0.7589 -0.1027 0.040 Uiso 1 calc R . . C5 C -0.2440(4) 0.6307(3) 0.0307(2) 0.0311(7) Uani 1 d . . . H5A H -0.2469 0.5511 0.0093 0.037 Uiso 1 calc R . . C6 C -0.1772(4) 0.6245(3) 0.1290(2) 0.0255(6) Uani 1 d . . . H6A H -0.1346 0.5401 0.1731 0.031 Uiso 1 calc R . . C7 C -0.2530(3) 0.9974(3) 0.1312(2) 0.0230(6) Uani 1 d . . . C8 C -0.3320(4) 1.0180(3) 0.2357(2) 0.0260(6) Uani 1 d . . . H8A H -0.3752 0.9475 0.2879 0.031 Uiso 1 calc R . . C9 C -0.3477(4) 1.1406(3) 0.2636(3) 0.0309(7) Uani 1 d . . . H9A H -0.4065 1.1544 0.3329 0.037 Uiso 1 calc R . . C10 C -0.2765(4) 1.2431(3) 0.1891(3) 0.0376(8) Uani 1 d . . . H10A H -0.2834 1.3255 0.2089 0.045 Uiso 1 calc R . . C11 C -0.1959(4) 1.2240(3) 0.0863(3) 0.0391(8) Uani 1 d . . . H11A H -0.1466 1.2931 0.0361 0.047 Uiso 1 calc R . . C12 C -0.1874(4) 1.1036(3) 0.0566(2) 0.0303(7) Uani 1 d . . . H12A H -0.1365 1.0930 -0.0149 0.036 Uiso 1 calc R . . C13 C 0.3493(4) 0.7910(3) 0.2946(3) 0.0382(8) Uani 1 d . . . H13A H 0.4443 0.7484 0.3422 0.046 Uiso 1 calc R . . H13B H 0.3824 0.8730 0.2462 0.046 Uiso 1 calc R . . C14 C 0.3316(4) 0.6970(3) 0.2253(2) 0.0339(7) Uani 1 d . . . H14A H 0.2468 0.7431 0.1715 0.041 Uiso 1 calc R . . H14B H 0.4473 0.6692 0.1841 0.041 Uiso 1 calc R . . C15 C 0.2184(5) 0.8418(3) 0.4731(3) 0.0412(8) Uani 1 d . . . H15A H 0.2942 0.9080 0.4601 0.062 Uiso 1 calc R . . H15B H 0.2791 0.7562 0.5128 0.062 Uiso 1 calc R . . H15C H 0.1080 0.8713 0.5169 0.062 Uiso 1 calc R . . C16 C 0.0835(4) 0.9599(3) 0.3087(3) 0.0368(7) Uani 1 d . . . H16A H 0.1568 1.0268 0.3006 0.055 Uiso 1 calc R . . H16B H -0.0287 0.9850 0.3527 0.055 Uiso 1 calc R . . H16C H 0.0604 0.9551 0.2359 0.055 Uiso 1 calc R . . C17 C 0.2463(4) 0.4898(3) 0.2245(3) 0.0374(8) Uani 1 d . . . H17A H 0.3626 0.4525 0.1909 0.056 Uiso 1 calc R . . H17B H 0.1740 0.5430 0.1667 0.056 Uiso 1 calc R . . H17C H 0.1882 0.4174 0.2681 0.056 Uiso 1 calc R . . C18 C 0.4094(4) 0.4985(3) 0.3682(3) 0.0352(7) Uani 1 d . . . H18A H 0.5142 0.4649 0.3217 0.053 Uiso 1 calc R . . H18B H 0.3661 0.4234 0.4197 0.053 Uiso 1 calc R . . H18C H 0.4402 0.5562 0.4094 0.053 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0190(3) 0.0194(3) 0.0217(3) -0.00518(19) -0.00307(18) -0.00384(19) Cl1 0.0352(4) 0.0281(4) 0.0317(4) -0.0108(3) 0.0013(3) 0.0001(3) Cl2 0.0284(4) 0.0238(3) 0.0251(3) -0.0037(3) -0.0068(3) -0.0088(3) N1 0.0227(11) 0.0169(11) 0.0232(11) -0.0057(9) -0.0032(9) -0.0034(9) N2 0.0275(13) 0.0258(12) 0.0334(13) -0.0043(10) -0.0093(10) -0.0085(10) N3 0.0208(12) 0.0317(13) 0.0259(12) -0.0078(10) -0.0026(9) -0.0032(10) C1 0.0179(13) 0.0265(14) 0.0235(13) -0.0073(11) -0.0017(10) -0.0067(11) C2 0.0182(13) 0.0250(14) 0.0247(13) -0.0055(11) -0.0015(10) -0.0034(11) C3 0.0295(16) 0.0300(15) 0.0254(14) -0.0040(12) -0.0101(12) 0.0008(12) C4 0.0328(16) 0.0421(18) 0.0302(16) -0.0150(14) -0.0123(12) -0.0018(14) C5 0.0285(16) 0.0339(16) 0.0364(16) -0.0159(13) -0.0056(12) -0.0069(13) C6 0.0246(14) 0.0232(14) 0.0305(15) -0.0068(12) -0.0058(11) -0.0053(11) C7 0.0204(13) 0.0226(13) 0.0263(14) -0.0060(11) -0.0043(11) -0.0024(11) C8 0.0234(14) 0.0266(14) 0.0285(15) -0.0045(12) -0.0044(11) -0.0068(11) C9 0.0274(15) 0.0316(16) 0.0345(16) -0.0123(13) -0.0043(12) -0.0015(12) C10 0.0379(18) 0.0236(15) 0.053(2) -0.0150(14) -0.0062(15) -0.0017(13) C11 0.0387(18) 0.0213(15) 0.051(2) 0.0006(14) 0.0021(15) -0.0067(13) C12 0.0297(15) 0.0234(14) 0.0326(16) -0.0039(12) 0.0002(12) 0.0008(12) C13 0.0261(16) 0.0384(18) 0.0491(19) -0.0008(15) -0.0053(14) -0.0132(14) C14 0.0253(15) 0.0429(18) 0.0290(15) -0.0011(13) 0.0016(12) -0.0082(13) C15 0.053(2) 0.0356(17) 0.0430(19) -0.0084(15) -0.0187(16) -0.0169(16) C16 0.0397(18) 0.0280(16) 0.0457(19) -0.0022(14) -0.0145(14) -0.0119(14) C17 0.0265(16) 0.049(2) 0.0425(18) -0.0276(16) -0.0008(13) -0.0018(14) C18 0.0237(15) 0.0423(18) 0.0365(17) -0.0072(14) -0.0054(12) -0.0001(13) _geom_special_details ; ? ; 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 Ti N1 1.717(2) . y Ti N3 2.312(2) . y Ti N2 2.312(2) . y Ti Cl1 2.3699(8) . y Ti Cl2 2.4350(8) . y Ti Cl2 2.7060(8) 2_566 y Cl2 Ti 2.7061(8) 2_566 ? N1 C1 1.390(3) . y N2 C13 1.491(4) . ? N2 C15 1.489(4) . ? N2 C16 1.488(4) . ? N3 C14 1.489(4) . ? N3 C17 1.484(4) . ? N3 C18 1.487(4) . ? C1 C6 1.408(4) . ? C1 C2 1.419(4) . ? C2 C3 1.396(4) . ? C2 C7 1.486(4) . ? C3 C4 1.392(4) . ? C4 C5 1.382(4) . ? C5 C6 1.390(4) . ? C7 C8 1.397(4) . ? C7 C12 1.396(4) . ? C8 C9 1.383(4) . ? C9 C10 1.388(4) . ? C10 C11 1.377(4) . ? C11 C12 1.381(4) . ? C13 C14 1.500(5) . ? 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 Ti N3 92.44(9) . . y N1 Ti N2 100.01(9) . . y N3 Ti N2 75.99(9) . . y N1 Ti Cl1 98.68(8) . . y N3 Ti Cl1 162.79(7) . . y N2 Ti Cl1 89.11(6) . . y N1 Ti Cl2 92.55(7) . . y N3 Ti Cl2 92.56(6) . . y N2 Ti Cl2 163.26(6) . . y Cl1 Ti Cl2 99.97(3) . . y N1 Ti Cl2 168.90(8) . 2_566 ? N3 Ti Cl2 87.38(6) . 2_566 ? N2 Ti Cl2 90.72(6) . 2_566 ? Cl1 Ti Cl2 84.20(3) . 2_566 ? Cl2 Ti Cl2 76.38(3) . 2_566 ? Ti Cl2 Ti 103.62(3) . 2_566 y C1 N1 Ti 164.99(19) . . y C13 N2 C15 109.2(2) . . ? C13 N2 C16 108.0(2) . . ? C15 N2 C16 107.0(2) . . ? C13 N2 Ti 110.68(18) . . ? C15 N2 Ti 113.66(18) . . ? C16 N2 Ti 108.05(17) . . ? C14 N3 C17 107.7(2) . . ? C14 N3 C18 108.7(2) . . ? C17 N3 C18 106.9(2) . . ? C14 N3 Ti 101.91(17) . . ? C17 N3 Ti 112.45(17) . . ? C18 N3 Ti 118.66(17) . . ? N1 C1 C6 118.6(2) . . ? N1 C1 C2 122.7(2) . . ? C6 C1 C2 118.6(2) . . ? C3 C2 C1 118.4(3) . . ? C3 C2 C7 118.9(2) . . ? C1 C2 C7 122.7(2) . . ? C4 C3 C2 122.2(3) . . ? C5 C4 C3 119.3(3) . . ? C4 C5 C6 120.0(3) . . ? C1 C6 C5 121.4(3) . . ? C8 C7 C12 117.9(3) . . ? C8 C7 C2 121.6(2) . . ? C12 C7 C2 120.5(2) . . ? C9 C8 C7 121.0(3) . . ? C8 C9 C10 119.9(3) . . ? C11 C10 C9 119.9(3) . . ? C10 C11 C12 120.2(3) . . ? C11 C12 C7 121.1(3) . . ? N2 C13 C14 110.8(2) . . ? N3 C14 C13 110.0(2) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.526 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.076 #===END