Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _audit_creation_date 22-07-02 _audit_creation_method CRYSTALS _journal_coden_Cambridge 186 loop_ _publ_author_name 'Philip Mountford' 'Catherine L. Boyd' 'Stuart R. Dubberley' 'Aldo E. Guiducci' 'Ben R. Tyrrell' _publ_contact_author_name 'Dr Philip Mountford' _publ_contact_author_address ; University of Oxford Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UNITED KINGDOM ; _publ_contact_author_phone '+44 1865 272679' _contact_author_fax '+44 1865 272690' _publ_contact_author_email Philip.Mountford@chem.ox.ac.uk _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Titanium imido complexes of pendant arm functionalised benzamidinate ligands ; _publ_contact_letter ; These are the CIF format data (5 compounds) for the paper Titanium imido complexes of pendant arm functionalised benzamidinate ligands C. L. Boyd, A. E. Guiducci, S. R. Dubberley, B. R. Tyrrell and P. Mountford ; data_Compound_1 _database_code_CSD 190460 _chemical_name_systematic ; [Ti(N-t-Bu){Me3SiNC(Ph)NCH2CH2NMe2}Cl] ; _publ_section_exptl_refinement ; No special details of the structure solution or refinement ; _cell_length_a 11.7460(3) _cell_length_b 9.9836(3) _cell_length_c 20.1557(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.265(1) _cell_angle_gamma 90.00 _cell_volume 2363.6 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International_Tables_Vol_IV_Table_2.2B' 'Ti ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C18 H33 Cl1 N4 Si1 Ti1 ' _chemical_formula_moiety ' C18 H33 Cl1 N4 Si1 Ti1 ' _chemical_formula_weight 416.93 _cell_measurement_reflns_used 3916 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 26.022 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.17 _exptl_crystal_density_method none _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.53 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.853 _exptl_absorpt_correction_T_max 0.948 _diffrn_reflns_av_sigmaI/netI 0.088 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_measurement_device-type 'Nonius KappaCCD' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method CCD _diffrn_ambient_temperature 150 _diffrn_reflns_number 7790 _reflns_number_total 4570 _diffrn_reflns_av_R_equivalents 0.02 _reflns_number_observed 3204 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 26.01 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.27 _refine_diff_density_max 0.22 _refine_ls_number_reflns 3204 _refine_ls_number_parameters 227 _refine_ls_R_factor_obs 0.0329 _refine_ls_wR_factor_obs 0.0366 _refine_ls_goodness_of_fit_obs 1.0513 _refine_ls_shift/esd_max 0.0065 _refine_ls_structure_factor_coef F _refine_ls_hydrogen_treatment 'riding model' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens geometric _refine_ls_matrix_type full _refine_ls_weighting_scheme 'Chebychev polynomial' _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack none _refine_ls_extinction_coef 250.7(352) _refine_ls_extinction_method CCD ; Larson 1970 Crystallographic Computing eq 22 ; _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SIR92 (Altomare, et al, 1994)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_molecular_graphics 'CAMERON (Watkin, Prout and Pearce, 1996)' _computing_publication_material ; CRYSTALS Issue 10 (Watkin et al, 1996) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Ti1 0.19382(3) 0.04096(4) 0.37302(2) 0.0207 1.0000 Uani N1 0.2414(1) -0.1004(2) 0.40978(9) 0.0265 1.0000 Uani N2 0.2395(1) 0.0673(2) 0.27193(8) 0.0237 1.0000 Uani N3 0.3350(1) 0.1630(2) 0.35389(8) 0.0220 1.0000 Uani N4 0.1942(2) 0.1994(2) 0.45226(9) 0.0294 1.0000 Uani Si1 0.20134(6) 0.00462(6) 0.19469(3) 0.0321 1.0000 Uani Cl1 -0.00287(4) 0.03041(6) 0.36162(3) 0.0392 1.0000 Uani C1 0.2724(2) -0.2269(2) 0.4406(1) 0.0335 1.0000 Uani C2 0.3813(3) -0.2069(3) 0.4804(2) 0.0689 1.0000 Uani C3 0.1743(2) -0.2704(3) 0.4856(1) 0.0507 1.0000 Uani C4 0.2904(3) -0.3321(3) 0.3870(2) 0.0583 1.0000 Uani C5 0.3057(2) 0.1700(2) 0.2904(1) 0.0208 1.0000 Uani C6 0.3412(2) 0.2828(2) 0.2468(1) 0.0228 1.0000 Uani C7 0.2616(2) 0.3637(2) 0.2149(1) 0.0293 1.0000 Uani C8 0.2972(2) 0.4679(2) 0.1749(1) 0.0338 1.0000 Uani C9 0.4122(2) 0.4900(2) 0.1656(1) 0.0362 1.0000 Uani C10 0.4923(2) 0.4103(2) 0.1970(1) 0.0352 1.0000 Uani C11 0.4567(2) 0.3076(2) 0.2383(1) 0.0289 1.0000 Uani C12 0.3686(2) 0.2751(2) 0.3953(1) 0.0292 1.0000 Uani C13 0.3136(2) 0.2445(2) 0.4622(1) 0.0342 1.0000 Uani C14 0.1231(2) 0.3132(2) 0.4297(1) 0.0399 1.0000 Uani C15 0.1478(2) 0.1474(3) 0.5156(1) 0.0443 1.0000 Uani C16 0.3177(3) 0.0346(3) 0.1340(1) 0.0510 1.0000 Uani C17 0.0650(2) 0.0782(3) 0.1646(1) 0.0491 1.0000 Uani C18 0.1817(3) -0.1780(3) 0.2069(2) 0.0573 1.0000 Uani H21 0.4030 -0.2899 0.5010 0.0888 1.0000 Uiso H22 0.3683 -0.1406 0.5140 0.0888 1.0000 Uiso H23 0.4411 -0.1773 0.4516 0.0888 1.0000 Uiso H31 0.1925 -0.3541 0.5065 0.0687 1.0000 Uiso H32 0.1625 -0.2032 0.5189 0.0687 1.0000 Uiso H33 0.1061 -0.2804 0.4596 0.0687 1.0000 Uiso H41 0.3109 -0.4160 0.4070 0.0703 1.0000 Uiso H42 0.3504 -0.3032 0.3581 0.0703 1.0000 Uiso H43 0.2215 -0.3430 0.3618 0.0703 1.0000 Uiso H71 0.1818 0.3466 0.2207 0.0387 1.0000 Uiso H81 0.2421 0.5251 0.1539 0.0453 1.0000 Uiso H91 0.4368 0.5609 0.1369 0.0479 1.0000 Uiso H101 0.5721 0.4261 0.1904 0.0466 1.0000 Uiso H111 0.5119 0.2532 0.2610 0.0383 1.0000 Uiso H121 0.4500 0.2806 0.3989 0.0395 1.0000 Uiso H122 0.3394 0.3576 0.3776 0.0395 1.0000 Uiso H131 0.3148 0.3232 0.4896 0.0467 1.0000 Uiso H132 0.3559 0.1743 0.4835 0.0467 1.0000 Uiso H141 0.0462 0.2831 0.4232 0.0520 1.0000 Uiso H142 0.1244 0.3827 0.4626 0.0520 1.0000 Uiso H143 0.1523 0.3475 0.3887 0.0520 1.0000 Uiso H151 0.0705 0.1190 0.5089 0.0565 1.0000 Uiso H152 0.1500 0.2167 0.5487 0.0565 1.0000 Uiso H153 0.1928 0.0727 0.5302 0.0565 1.0000 Uiso H161 0.2961 -0.0002 0.0914 0.0644 1.0000 Uiso H162 0.3856 -0.0096 0.1491 0.0644 1.0000 Uiso H163 0.3339 0.1294 0.1300 0.0644 1.0000 Uiso H171 0.0464 0.0415 0.1218 0.0658 1.0000 Uiso H172 0.0054 0.0575 0.1953 0.0658 1.0000 Uiso H173 0.0730 0.1736 0.1610 0.0658 1.0000 Uiso H181 0.1602 -0.2191 0.1657 0.0702 1.0000 Uiso H182 0.2515 -0.2169 0.2226 0.0702 1.0000 Uiso H183 0.1229 -0.1923 0.2391 0.0702 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0178(2) 0.0214(2) 0.0229(2) 0.0024(1) 0.0020(1) 0.0002(1) N1 0.0267(9) 0.0247(9) 0.0281(9) 0.0024(7) -0.0006(7) 0.0008(7) N2 0.0224(9) 0.0244(9) 0.0244(9) -0.0016(7) 0.0003(7) -0.0050(7) N3 0.0196(8) 0.0236(8) 0.0228(9) -0.0037(7) 0.0017(6) -0.0019(7) N4 0.031(1) 0.0293(9) 0.0275(9) -0.0003(8) 0.0065(8) 0.0026(8) Si1 0.0397(4) 0.0315(3) 0.0251(3) -0.0027(2) -0.0068(2) -0.0079(3) Cl1 0.0193(3) 0.0487(4) 0.0495(3) 0.0118(3) 0.0001(2) -0.0030(2) C1 0.031(1) 0.023(1) 0.046(1) 0.011(1) -0.001(1) 0.0049(9) C2 0.053(2) 0.064(2) 0.089(2) 0.029(2) -0.035(2) -0.001(2) C3 0.055(2) 0.043(1) 0.055(2) 0.022(1) 0.012(1) 0.004(1) C4 0.071(2) 0.027(1) 0.077(2) 0.004(1) 0.016(2) 0.010(1) C5 0.0142(9) 0.023(1) 0.026(1) -0.0015(8) 0.0048(7) 0.0017(8) C6 0.023(1) 0.022(1) 0.024(1) -0.0010(8) 0.0009(8) -0.0032(8) C7 0.022(1) 0.028(1) 0.038(1) 0.0012(9) -0.0033(9) -0.0030(9) C8 0.032(1) 0.028(1) 0.042(1) 0.008(1) -0.009(1) -0.001(1) C9 0.039(1) 0.032(1) 0.037(1) 0.012(1) -0.002(1) -0.011(1) C10 0.023(1) 0.038(1) 0.044(1) 0.007(1) 0.003(1) -0.009(1) C11 0.020(1) 0.030(1) 0.036(1) 0.0060(9) -0.0009(9) -0.0008(9) C12 0.027(1) 0.030(1) 0.030(1) -0.0061(9) -0.0014(9) -0.0049(9) C13 0.039(1) 0.035(1) 0.028(1) -0.010(1) -0.0017(9) -0.001(1) C14 0.039(1) 0.028(1) 0.053(2) -0.003(1) 0.008(1) 0.010(1) C15 0.057(2) 0.047(1) 0.029(1) -0.003(1) 0.016(1) 0.000(1) C16 0.064(2) 0.061(2) 0.028(1) -0.010(1) 0.005(1) -0.007(2) C17 0.050(2) 0.053(2) 0.045(2) 0.005(1) -0.019(1) -0.010(1) C18 0.083(2) 0.034(1) 0.054(2) -0.008(1) -0.021(2) -0.011(1) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . N1 . 1.688(2) yes Ti1 . N2 . 2.126(2) yes Ti1 . N3 . 2.095(2) yes Ti1 . N4 . 2.248(2) yes Ti1 . Cl1 . 2.3231(6) yes Ti1 . C5 . 2.486(2) yes N1 . C1 . 1.454(3) yes N2 . Si1 . 1.735(2) yes N2 . C5 . 1.339(3) yes N3 . C5 . 1.325(3) yes N3 . C12 . 1.450(3) yes N4 . C13 . 1.486(3) yes N4 . C14 . 1.480(3) yes N4 . C15 . 1.485(3) yes Si1 . C16 . 1.863(3) yes Si1 . C17 . 1.861(3) yes Si1 . C18 . 1.854(3) yes C1 . C2 . 1.520(4) yes C1 . C3 . 1.532(3) yes C1 . C4 . 1.523(4) yes C5 . C6 . 1.490(3) yes C6 . C7 . 1.390(3) yes C6 . C11 . 1.391(3) yes C7 . C8 . 1.382(3) yes C8 . C9 . 1.383(3) yes C9 . C10 . 1.383(3) yes C10 . C11 . 1.386(3) yes C12 . C13 . 1.528(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ti1 . N2 . 116.07(8) yes N1 . Ti1 . N3 . 107.85(8) yes N2 . Ti1 . N3 . 63.14(6) yes N1 . Ti1 . N4 . 106.08(8) yes N2 . Ti1 . N4 . 126.47(7) yes N3 . Ti1 . N4 . 73.89(6) yes N1 . Ti1 . Cl1 . 109.42(6) yes N2 . Ti1 . Cl1 . 99.56(5) yes N3 . Ti1 . Cl1 . 142.73(5) yes N4 . Ti1 . Cl1 . 95.79(5) yes N1 . Ti1 . C5 . 123.53(8) yes N2 . Ti1 . C5 . 32.59(6) yes N3 . Ti1 . C5 . 32.20(6) yes N4 . Ti1 . C5 . 96.42(7) yes Cl1 . Ti1 . C5 . 119.08(5) yes Ti1 . N1 . C1 . 175.0(2) yes Ti1 . N2 . Si1 . 138.62(9) yes Ti1 . N2 . C5 . 88.7(1) yes Si1 . N2 . C5 . 132.3(1) yes Ti1 . N3 . C5 . 90.4(1) yes Ti1 . N3 . C12 . 123.8(1) yes C5 . N3 . C12 . 125.7(2) yes Ti1 . N4 . C13 . 107.9(1) yes Ti1 . N4 . C14 . 108.8(1) yes C13 . N4 . C14 . 109.8(2) yes Ti1 . N4 . C15 . 111.4(1) yes C13 . N4 . C15 . 109.9(2) yes C14 . N4 . C15 . 108.9(2) yes N2 . Si1 . C16 . 110.1(1) yes N2 . Si1 . C17 . 111.7(1) yes C16 . Si1 . C17 . 110.8(1) yes N2 . Si1 . C18 . 105.5(1) yes C16 . Si1 . C18 . 109.7(1) yes C17 . Si1 . C18 . 108.9(1) yes N1 . C1 . C2 . 108.7(2) yes N1 . C1 . C3 . 108.1(2) yes C2 . C1 . C3 . 111.0(2) yes N1 . C1 . C4 . 109.3(2) yes C2 . C1 . C4 . 110.3(2) yes C3 . C1 . C4 . 109.4(2) yes Ti1 . C5 . N2 . 58.8(1) yes Ti1 . C5 . N3 . 57.4(1) yes N2 . C5 . N3 . 112.1(2) yes Ti1 . C5 . C6 . 159.6(1) yes N2 . C5 . C6 . 125.3(2) yes N3 . C5 . C6 . 122.6(2) yes C5 . C6 . C7 . 121.5(2) yes C5 . C6 . C11 . 118.8(2) yes C7 . C6 . C11 . 119.6(2) yes C6 . C7 . C8 . 120.1(2) yes C7 . C8 . C9 . 119.8(2) yes C8 . C9 . C10 . 120.6(2) yes C9 . C10 . C11 . 119.6(2) yes C6 . C11 . C10 . 120.2(2) yes N3 . C12 . C13 . 103.8(2) yes N4 . C13 . C12 . 110.2(2) yes #===end data_Compound_5 _database_code_CSD 190461 _chemical_name_systematic ; [Ti(N-2,6-C6H3Me2){Me3SiNC(Ph)NCH2CH2CH2NMe2}Cl] ; _publ_section_exptl_refinement ; No special details ; _cell_length_a 8.8806(1) _cell_length_b 11.2263(1) _cell_length_c 15.0212(2) _cell_angle_alpha 70.6889(7) _cell_angle_beta 88.3802(5) _cell_angle_gamma 66.8105(5) _cell_volume 1290.11(3) _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'Ti ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C23 H35 Cl1 N4 Si1 Ti1 ' _chemical_formula_moiety ' C23 H35 Cl1 N4 Si1 Ti1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 479.00 _cell_measurement_reflns_used 5532 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _cell_measurement_temperature 150 _cell_formula_units_Z 2 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_min 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_max 0.50 _exptl_crystal_density_diffrn 1.23 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method none _exptl_crystal_F_000 508.94 _exptl_absorpt_coefficient_mu 0.50 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_T_max 0.819 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'CCD' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_ambient_temperature 150 _diffrn_reflns_number 11005 _reflns_number_total 5879 _diffrn_reflns_av_R_equivalents 0.01 _reflns_number_gt 4948 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 27.5 _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 -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -13 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _refine_diff_density_min -0.34 _refine_diff_density_max 0.31 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 4948 _refine_ls_number_parameters 272 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0318 _refine_ls_goodness_of_fit_ref 1.0209 _refine_ls_shift/su_max 0.0008 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 5 parameters, Carruthers & Watkin , 1979, 1.35 1.18 1.38 0.459 0.433 ; _refine_ls_hydrogen_treatment 'riding model' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens geometric _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack none _refine_ls_extinction_coef 184.8(400) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SIR92 (Altomare, et al., 1994)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al., 1996) ; _computing_molecular_graphics 'CAMERON (Watkin, Prout and Pearce, 1996)' _computing_publication_material ; CRYSTALS Issue 10 (Watkin et al., 1996) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Ti1 0.86234(2) 0.29915(2) 0.365297(14) 0.0171 1.0000 Uani Cl1 0.64067(4) 0.25939(4) 0.43344(2) 0.0320 1.0000 Uani N1 0.82563(13) 0.4707(1) 0.31766(7) 0.0217 1.0000 Uani N2 0.86715(12) 0.23708(11) 0.24575(7) 0.0210 1.0000 Uani N3 1.09342(12) 0.17899(11) 0.33840(7) 0.0237 1.0000 Uani N4 0.99853(13) 0.25035(11) 0.50351(7) 0.0222 1.0000 Uani Si1 0.72883(4) 0.31696(4) 0.14332(2) 0.0266 1.0000 Uani C1 0.79242(15) 0.60943(12) 0.28025(8) 0.0223 1.0000 Uani C2 0.64217(17) 0.70739(14) 0.29366(9) 0.0292 1.0000 Uani C3 0.6129(2) 0.84697(15) 0.25694(11) 0.0391 1.0000 Uani C4 0.7264(2) 0.89049(15) 0.20833(12) 0.0434 1.0000 Uani C5 0.8713(2) 0.79509(15) 0.19327(11) 0.0376 1.0000 Uani C6 0.90713(17) 0.65428(13) 0.22849(9) 0.0270 1.0000 Uani C7 0.5174(2) 0.66071(17) 0.34559(12) 0.0437 1.0000 Uani C8 1.06549(19) 0.55115(17) 0.21240(12) 0.0396 1.0000 Uani C9 1.03202(15) 0.18076(12) 0.25900(8) 0.0198 1.0000 Uani C10 1.13380(15) 0.12408(13) 0.18952(8) 0.0219 1.0000 Uani C11 1.14709(18) -0.00213(14) 0.1869(1) 0.0291 1.0000 Uani C12 1.23203(19) -0.05297(16) 0.1192(1) 0.0343 1.0000 Uani C13 1.30143(18) 0.02322(16) 0.0533(1) 0.0341 1.0000 Uani C14 1.2892(2) 0.14836(17) 0.05599(11) 0.0380 1.0000 Uani C15 1.20694(18) 0.19877(15) 0.1245(1) 0.0320 1.0000 Uani C16 1.26622(16) 0.14375(15) 0.3643(1) 0.0299 1.0000 Uani C17 1.29323(16) 0.13403(14) 0.46667(9) 0.0272 1.0000 Uani C18 1.16583(16) 0.25242(13) 0.49236(9) 0.0253 1.0000 Uani C19 1.01367(19) 0.11521(15) 0.57310(9) 0.0319 1.0000 Uani C20 0.90211(18) 0.35991(15) 0.5426(1) 0.0318 1.0000 Uani C21 0.5290(2) 0.3162(3) 0.18317(14) 0.0672 1.0000 Uani C22 0.7126(3) 0.49693(19) 0.08639(15) 0.0711 1.0000 Uani C23 0.7851(2) 0.23259(18) 0.0517(1) 0.0406 1.0000 Uani H31 0.5074 0.91688 0.26629 0.0438 1.0000 Uiso H41 0.7035 0.99104 0.18372 0.0499 1.0000 Uiso H51 0.9520 0.82763 0.15668 0.0457 1.0000 Uiso H71 0.4192 0.74250 0.34863 0.0481 1.0000 Uiso H72 0.5678 0.59629 0.41149 0.0481 1.0000 Uiso H73 0.4822 0.61170 0.31119 0.0481 1.0000 Uiso H81 1.13148 0.60064 0.17491 0.0486 1.0000 Uiso H82 1.13026 0.48501 0.27505 0.0486 1.0000 Uiso H83 1.04005 0.49914 0.17657 0.0486 1.0000 Uiso H111 1.09539 -0.05644 0.2341 0.0385 1.0000 Uiso H121 1.24324 -0.14469 0.1181 0.0452 1.0000 Uiso H131 1.36037 -0.01236 0.0036 0.0427 1.0000 Uiso H141 1.3402 0.20288 0.00849 0.0480 1.0000 Uiso H151 1.19993 0.28866 0.1271 0.0414 1.0000 Uiso H161 1.29827 0.21717 0.3212 0.0363 1.0000 Uiso H162 1.33573 0.05303 0.3574 0.0363 1.0000 Uiso H171 1.40487 0.13181 0.47803 0.0331 1.0000 Uiso H172 1.28887 0.04594 0.50936 0.0331 1.0000 Uiso H181 1.20992 0.25040 0.55361 0.0334 1.0000 Uiso H182 1.15203 0.34076 0.44080 0.0334 1.0000 Uiso H191 0.90160 0.11464 0.58003 0.0394 1.0000 Uiso H192 1.06594 0.10085 0.63603 0.0394 1.0000 Uiso H193 1.08363 0.03925 0.55000 0.0394 1.0000 Uiso H201 0.78942 0.36129 0.5512 0.0433 1.0000 Uiso H202 0.95969 0.34038 0.6054 0.0433 1.0000 Uiso H203 0.89253 0.45173 0.4977 0.0433 1.0000 Uiso H211 0.4430 0.3612 0.12703 0.0829 1.0000 Uiso H212 0.4939 0.3679 0.22836 0.0829 1.0000 Uiso H213 0.5430 0.2185 0.21578 0.0829 1.0000 Uiso H221 0.6333 0.54477 0.02707 0.0801 1.0000 Uiso H222 0.8239 0.49365 0.07027 0.0801 1.0000 Uiso H223 0.6732 0.54863 0.13130 0.0801 1.0000 Uiso H231 0.6984 0.28590 -0.0043 0.0524 1.0000 Uiso H232 0.8938 0.23103 0.0312 0.0524 1.0000 Uiso H233 0.7932 0.13580 0.0792 0.0524 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.01902(11) 0.01823(11) 0.01626(11) -0.00752(8) 0.00422(7) -0.00859(8) Cl1 0.03220(17) 0.04439(19) 0.03263(17) -0.01844(14) 0.01492(13) -0.02536(15) N1 0.0234(5) 0.0203(5) 0.0208(5) -0.0082(4) 0.0038(4) -0.0076(4) N2 0.0226(5) 0.0246(5) 0.0191(5) -0.0106(4) 0.0041(4) -0.0106(4) N3 0.0197(5) 0.0277(5) 0.0228(5) -0.0129(4) 0.0016(4) -0.0054(4) N4 0.0288(5) 0.0234(5) 0.0189(5) -0.0093(4) 0.0038(4) -0.0136(4) Si1 0.02702(18) 0.03192(19) 0.02155(17) -0.01091(14) -0.00147(13) -0.01116(15) C1 0.0279(6) 0.0204(6) 0.0181(5) -0.0072(4) -0.0007(4) -0.0088(5) C2 0.0329(7) 0.0260(6) 0.0238(6) -0.0113(5) -0.0006(5) -0.0047(5) C3 0.0486(9) 0.0227(6) 0.0353(7) -0.0121(6) -0.0065(6) -0.0015(6) C4 0.0649(11) 0.0200(6) 0.0404(8) -0.0056(6) -0.0116(7) -0.0152(7) C5 0.0526(9) 0.0302(7) 0.0319(7) -0.0023(6) -0.0048(6) -0.0251(7) C6 0.0329(7) 0.0262(6) 0.0228(6) -0.0065(5) -0.0015(5) -0.0142(5) C7 0.0342(8) 0.0377(8) 0.0441(8) -0.0129(7) 0.0137(7) -0.0013(6) C8 0.0363(8) 0.0393(8) 0.0432(8) -0.0103(7) 0.0142(6) -0.0193(7) C9 0.0233(6) 0.0184(5) 0.0191(5) -0.0074(4) 0.0048(4) -0.0094(4) C10 0.0221(6) 0.0249(6) 0.0206(5) -0.0108(5) 0.0039(4) -0.0093(5) C11 0.0373(7) 0.0305(7) 0.0285(6) -0.0166(5) 0.0131(5) -0.0182(6) C12 0.0413(8) 0.0365(7) 0.0363(7) -0.0244(6) 0.0135(6) -0.0181(6) C13 0.0339(7) 0.0450(8) 0.0284(7) -0.0217(6) 0.0122(5) -0.0143(6) C14 0.0442(8) 0.0422(8) 0.0335(7) -0.0161(6) 0.0214(6) -0.0220(7) C15 0.0378(7) 0.0301(7) 0.0342(7) -0.0150(6) 0.0155(6) -0.0175(6) C16 0.0195(6) 0.0387(7) 0.0301(7) -0.0167(6) 0.0018(5) -0.0067(5) C17 0.0234(6) 0.0275(6) 0.0301(6) -0.0101(5) -0.0032(5) -0.0092(5) C18 0.0291(6) 0.0268(6) 0.0249(6) -0.0107(5) -0.0003(5) -0.0149(5) C19 0.0442(8) 0.0323(7) 0.0205(6) -0.0030(5) 0.0022(5) -0.0220(6) C20 0.0388(7) 0.0377(7) 0.0290(6) -0.0228(6) 0.0074(6) -0.0167(6) C21 0.0277(8) 0.132(2) 0.0427(9) -0.0384(12) 0.0022(7) -0.026(1) C22 0.1128(19) 0.0354(9) 0.0494(11) 0.0022(8) -0.0433(12) -0.0248(11) C23 0.0464(9) 0.0540(9) 0.0258(7) -0.0194(7) -0.0000(6) -0.0200(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . Cl1 . 2.3234(4) yes Ti1 . N1 . 1.713(1) yes Ti1 . N2 . 2.124(1) yes Ti1 . N3 . 2.080(1) yes Ti1 . N4 . 2.223(1) yes N1 . C1 . 1.3771(16) yes N2 . Si1 . 1.734(1) yes N2 . C9 . 1.3369(16) yes N3 . C9 . 1.3163(15) yes N3 . C16 . 1.4547(16) yes N4 . C18 . 1.4988(16) yes N4 . C19 . 1.4869(16) yes N4 . C20 . 1.4873(16) yes Si1 . C21 . 1.8591(19) yes Si1 . C22 . 1.8626(19) yes Si1 . C23 . 1.8680(15) yes C1 . C2 . 1.4164(18) yes C1 . C6 . 1.4128(18) yes C2 . C3 . 1.394(2) yes C2 . C7 . 1.500(2) yes C3 . C4 . 1.377(3) yes C4 . C5 . 1.383(3) yes C5 . C6 . 1.3929(19) yes C6 . C8 . 1.503(2) yes C9 . C10 . 1.4981(16) yes C10 . C11 . 1.3882(18) yes C10 . C15 . 1.3894(18) yes C11 . C12 . 1.3904(18) yes C12 . C13 . 1.383(2) yes C13 . C14 . 1.380(2) yes C14 . C15 . 1.3895(19) yes C16 . C17 . 1.5246(18) yes C17 . C18 . 1.5251(18) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Ti1 . N1 . 113.67(4) yes Cl1 . Ti1 . N2 . 101.07(3) yes N1 . Ti1 . N2 . 104.53(4) yes Cl1 . Ti1 . N3 . 136.08(3) yes N1 . Ti1 . N3 . 110.09(5) yes N2 . Ti1 . N3 . 63.71(4) yes Cl1 . Ti1 . N4 . 94.13(3) yes N1 . Ti1 . N4 . 98.13(4) yes N2 . Ti1 . N4 . 144.58(4) yes N3 . Ti1 . N4 . 83.16(4) yes Ti1 . N1 . C1 . 178.58(9) yes Ti1 . N2 . Si1 . 129.04(6) yes Ti1 . N2 . C9 . 89.77(7) yes Si1 . N2 . C9 . 131.58(8) yes Ti1 . N3 . C9 . 92.26(7) yes Ti1 . N3 . C16 . 138.75(8) yes C9 . N3 . C16 . 125.4(1) yes Ti1 . N4 . C18 . 112.12(7) yes Ti1 . N4 . C19 . 111.76(8) yes C18 . N4 . C19 . 110.0(1) yes Ti1 . N4 . C20 . 107.41(8) yes C18 . N4 . C20 . 107.4(1) yes C19 . N4 . C20 . 108.0(1) yes N2 . Si1 . C21 . 105.60(7) yes N2 . Si1 . C22 . 108.60(7) yes C21 . Si1 . C22 . 111.01(13) yes N2 . Si1 . C23 . 115.37(6) yes C21 . Si1 . C23 . 109.33(9) yes C22 . Si1 . C23 . 106.97(9) yes N1 . C1 . C2 . 119.68(12) yes N1 . C1 . C6 . 120.35(11) yes C2 . C1 . C6 . 119.97(12) yes C1 . C2 . C3 . 118.63(14) yes C1 . C2 . C7 . 120.19(12) yes C3 . C2 . C7 . 121.18(13) yes C2 . C3 . C4 . 121.41(14) yes C3 . C4 . C5 . 119.93(13) yes C4 . C5 . C6 . 121.10(15) yes C1 . C6 . C5 . 118.92(13) yes C1 . C6 . C8 . 120.30(12) yes C5 . C6 . C8 . 120.78(13) yes Ti1 . C9 . N2 . 57.98(6) yes Ti1 . C9 . N3 . 56.07(6) yes N2 . C9 . N3 . 113.5(1) yes Ti1 . C9 . C10 . 174.07(8) yes N2 . C9 . C10 . 122.1(1) yes N3 . C9 . C10 . 124.35(11) yes C9 . C10 . C11 . 118.97(11) yes C9 . C10 . C15 . 121.27(11) yes C11 . C10 . C15 . 119.65(12) yes C10 . C11 . C12 . 120.16(13) yes C11 . C12 . C13 . 119.95(13) yes C12 . C13 . C14 . 120.02(12) yes C13 . C14 . C15 . 120.37(13) yes C10 . C15 . C14 . 119.82(13) yes N3 . C16 . C17 . 110.0(1) yes C16 . C17 . C18 . 114.57(11) yes N4 . C18 . C17 . 115.8(1) yes #===end data_Compound_6 _database_code_CSD 190462 _chemical_name_systematic ; [Ti(N-2,6-C6H3iPr2)(Me3SiNC(Ph)NCH2CH2CH2NMe2)Cl] ; _publ_section_exptl_refinement ; No special details ; _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; _cell_length_a 16.0613(5) _cell_length_b 11.3483(4) _cell_length_c 17.5211(6) _cell_angle_alpha 90.00 _cell_angle_beta 112.749(2) _cell_angle_gamma 90.00 _cell_volume 2945.1(2) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'Ti ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C27 H43 Cl1 N4 Si1 Ti1 ' _chemical_formula_moiety ' C27 H43 Cl1 N4 Si1 Ti1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 535.10 _cell_measurement_reflns_used 5532 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description 'block' _exptl_crystal_colour 'red-orange' _exptl_crystal_size_min 0.13 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_max 0.21 _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method none _exptl_crystal_F_000 1146.13 _exptl_absorpt_coefficient_mu 0.443 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_method 'CCD' _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.919 _exptl_absorpt_correction_T_max 0.944 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_number 10992 _reflns_number_total 6629 _diffrn_reflns_av_R_equivalents 0.03 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_gt 3325 _diffrn_reflns_theta_min 5.14 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -20 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _refine_diff_density_min -0.32 _refine_diff_density_max 0.35 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 3325 _refine_ls_number_parameters 308 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0254 _refine_ls_goodness_of_fit_ref 1.1162 _refine_ls_shift/su_max 0.006 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_extinction_coef 0 _refine_ls_hydrogen_treatment 'riding model' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens geometric _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack none _refine_ls_weighting_details ; Method= Tukey and Prince W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 0.230 -0.999 -0.571E-01 -0.428 ; _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SIR92 (Altomare, et al., 1994)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al., 2001) ; _computing_molecular_graphics 'CAMERON (Watkin, Prout and Pearce, 1996)' _computing_publication_material ; CRYSTALS Issue 10 (Watkin et al., 2001) ; 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_occupancy _atom_site_adp_type Ti1 Ti 0.75691(4) 0.21413(5) 0.20474(3) 0.0198 1.0000 Uani Cl1 Cl 0.73258(6) 0.30732(8) 0.31337(5) 0.0319 1.0000 Uani N1 N 0.70004(17) 0.0830(2) 0.17942(15) 0.0231 1.0000 Uani N2 N 0.89631(16) 0.1799(2) 0.26495(15) 0.0238 1.0000 Uani N3 N 0.83398(17) 0.2294(2) 0.13298(15) 0.0259 1.0000 Uani N4 N 0.66493(17) 0.3357(2) 0.10944(16) 0.0248 1.0000 Uani Si1 SI 0.96386(6) 0.12909(9) 0.36279(5) 0.0255 1.0000 Uani C1 C 0.66109(19) -0.0286(3) 0.16206(18) 0.0219 1.0000 Uani C2 C 0.6290(2) -0.0838(3) 0.21817(19) 0.0243 1.0000 Uani C3 C 0.5909(2) -0.1951(3) 0.1991(2) 0.0285 1.0000 Uani C4 C 0.5849(2) -0.2532(3) 0.1275(2) 0.0321 1.0000 Uani C5 C 0.6179(2) -0.1998(3) 0.0738(2) 0.0309 1.0000 Uani C6 C 0.6555(2) -0.0879(3) 0.08878(19) 0.0251 1.0000 Uani C7 C 0.6343(2) -0.0194(3) 0.29601(19) 0.0279 1.0000 Uani C8 C 0.6525(3) -0.1026(3) 0.3701(2) 0.0364 1.0000 Uani C9 C 0.5493(3) 0.0534(4) 0.2788(2) 0.0427 1.0000 Uani C10 C 0.6910(2) -0.0316(3) 0.0292(2) 0.0296 1.0000 Uani C11 C 0.6204(3) -0.0264(4) -0.0590(2) 0.0538 1.0000 Uani C12 C 0.7757(3) -0.0954(4) 0.0321(3) 0.0536 1.0000 Uani C13 C 0.9090(2) 0.1989(3) 0.19473(18) 0.0220 1.0000 Uani C14 C 0.9984(2) 0.1856(3) 0.18841(18) 0.0253 1.0000 Uani C15 C 1.0128(2) 0.0959(3) 0.1409(2) 0.0360 1.0000 Uani C16 C 1.0986(3) 0.0782(4) 0.1405(2) 0.0440 1.0000 Uani C17 C 1.1683(2) 0.1516(4) 0.1852(2) 0.0421 1.0000 Uani C18 C 1.1545(2) 0.2420(3) 0.2313(2) 0.0392 1.0000 Uani C19 C 1.0701(2) 0.2592(3) 0.2333(2) 0.0339 1.0000 Uani C20 C 0.8225(2) 0.2505(3) 0.04779(18) 0.0249 1.0000 Uani C21 C 0.7463(2) 0.3391(3) 0.0086(2) 0.0273 1.0000 Uani C22 C 0.6604(2) 0.3136(3) 0.02333(18) 0.0269 1.0000 Uani C23 C 0.6938(3) 0.4589(3) 0.1348(2) 0.0343 1.0000 Uani C24 C 0.5723(2) 0.3187(4) 0.1071(2) 0.0373 1.0000 Uani C25 C 1.0658(2) 0.0470(4) 0.3664(2) 0.0423 1.0000 Uani C26 C 0.9992(2) 0.2559(3) 0.4355(2) 0.0388 1.0000 Uani C27 C 0.8909(2) 0.0284(3) 0.3942(2) 0.0351 1.0000 Uani H31 H 0.5675 -0.2342 0.2380 0.0369 1.0000 Uiso H41 H 0.5563 -0.3329 0.1145 0.0400 1.0000 Uiso H51 H 0.6150 -0.2429 0.0231 0.0378 1.0000 Uiso H71 H 0.6871 0.0352 0.31124 0.0373 1.0000 Uiso H81 H 0.6557 -0.0559 0.4195 0.0477 1.0000 Uiso H82 H 0.7108 -0.1453 0.3829 0.0477 1.0000 Uiso H83 H 0.6020 -0.1608 0.3557 0.0477 1.0000 Uiso H91 H 0.5542 0.0957 0.3304 0.0553 1.0000 Uiso H92 H 0.5415 0.1121 0.2339 0.0553 1.0000 Uiso H93 H 0.4961 -0.0008 0.2611 0.0553 1.0000 Uiso H101 H 0.7071 0.0517 0.0475 0.0406 1.0000 Uiso H111 H 0.6466 0.0118 -0.0961 0.0653 1.0000 Uiso H112 H 0.6005 -0.1082 -0.0789 0.0653 1.0000 Uiso H113 H 0.5673 0.0204 -0.0597 0.0653 1.0000 Uiso H121 H 0.7986 -0.0571 -0.0074 0.0740 1.0000 Uiso H122 H 0.8232 -0.0917 0.0894 0.0740 1.0000 Uiso H123 H 0.7604 -0.1796 0.0159 0.0740 1.0000 Uiso H151 H 0.9613 0.0439 0.1075 0.0481 1.0000 Uiso H161 H 1.1092 0.0127 0.1072 0.0588 1.0000 Uiso H171 H 1.2296 0.1392 0.1842 0.0543 1.0000 Uiso H181 H 1.2056 0.2954 0.2635 0.0494 1.0000 Uiso H191 H 1.0599 0.3241 0.2673 0.0408 1.0000 Uiso H201 H 0.8800 0.2818 0.04622 0.0321 1.0000 Uiso H202 H 0.8064 0.1749 0.01611 0.0321 1.0000 Uiso H211 H 0.7690 0.4183 0.0328 0.0353 1.0000 Uiso H212 H 0.7310 0.3410 -0.0524 0.0353 1.0000 Uiso H221 H 0.6108 0.3635 -0.01550 0.0346 1.0000 Uiso H222 H 0.6453 0.2285 0.01039 0.0346 1.0000 Uiso H231 H 0.6972 0.4720 0.1924 0.0453 1.0000 Uiso H232 H 0.7544 0.4733 0.1329 0.0453 1.0000 Uiso H233 H 0.6487 0.5143 0.0961 0.0453 1.0000 Uiso H241 H 0.5722 0.3329 0.1634 0.0510 1.0000 Uiso H242 H 0.5299 0.3751 0.0668 0.0510 1.0000 Uiso H243 H 0.5525 0.2361 0.0895 0.0510 1.0000 Uiso H251 H 1.1014 0.0205 0.4244 0.0548 1.0000 Uiso H252 H 1.1041 0.0995 0.3475 0.0548 1.0000 Uiso H253 H 1.0465 -0.0232 0.3292 0.0548 1.0000 Uiso H261 H 1.0382 0.2271 0.4921 0.0477 1.0000 Uiso H262 H 1.0338 0.3133 0.4159 0.0477 1.0000 Uiso H263 H 0.9445 0.2955 0.4377 0.0477 1.0000 Uiso H271 H 0.9266 -0.0039 0.4506 0.0448 1.0000 Uiso H272 H 0.8695 -0.0379 0.3537 0.0448 1.0000 Uiso H273 H 0.8377 0.0729 0.3954 0.0448 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0184(3) 0.0238(3) 0.0184(3) 0.0005(3) 0.0084(2) -0.0003(3) Cl1 0.0383(5) 0.0344(5) 0.0271(4) -0.0049(4) 0.0171(4) 0.0013(4) N1 0.0211(14) 0.0233(15) 0.0272(13) 0.0004(12) 0.0120(11) -0.0002(11) N2 0.0196(13) 0.0316(16) 0.0219(13) 0.0032(12) 0.0100(11) 0.0020(12) N3 0.0222(13) 0.0368(17) 0.0224(13) 0.0042(12) 0.0125(11) 0.0027(13) N4 0.0210(14) 0.0290(16) 0.0259(13) 0.0006(12) 0.0106(11) 0.0007(12) Si1 0.0225(5) 0.0321(6) 0.0217(4) 0.0047(4) 0.0081(4) 0.0031(4) C1 0.0150(15) 0.0252(18) 0.0263(16) -0.0009(14) 0.0087(13) 0.0006(13) C2 0.0203(16) 0.0247(18) 0.0292(16) -0.0003(14) 0.0110(13) 0.0004(14) C3 0.0248(17) 0.030(2) 0.0344(17) 0.0036(16) 0.0158(14) 0.0006(15) C4 0.0272(18) 0.031(2) 0.0391(19) -0.0045(16) 0.0135(15) -0.0102(15) C5 0.0317(18) 0.031(2) 0.0312(17) -0.0072(16) 0.0131(14) -0.0023(16) C6 0.0218(17) 0.0255(18) 0.0300(17) 0.0001(15) 0.0123(14) 0.0015(14) C7 0.0301(18) 0.0280(19) 0.0290(17) -0.0004(15) 0.0150(15) -0.0034(15) C8 0.042(2) 0.038(2) 0.0326(19) 0.0007(17) 0.0178(16) -0.0058(18) C9 0.044(2) 0.053(3) 0.034(2) -0.0022(19) 0.0179(17) 0.015(2) C10 0.0333(19) 0.032(2) 0.0291(17) -0.0057(16) 0.0181(15) -0.0035(16) C11 0.056(3) 0.064(3) 0.037(2) 0.011(2) 0.0116(19) -0.016(2) C12 0.049(3) 0.058(3) 0.068(3) 0.005(2) 0.037(2) 0.004(2) C13 0.0231(15) 0.0199(17) 0.0240(15) -0.0008(14) 0.0103(12) -0.0001(14) C14 0.0224(16) 0.0297(19) 0.0256(16) 0.0084(14) 0.0114(13) 0.0031(14) C15 0.032(2) 0.041(2) 0.039(2) -0.0024(18) 0.0179(16) 0.0021(17) C16 0.037(2) 0.052(3) 0.051(2) 0.000(2) 0.0266(19) 0.011(2) C17 0.0248(19) 0.058(3) 0.048(2) 0.019(2) 0.0190(17) 0.0079(19) C18 0.0237(18) 0.046(2) 0.045(2) 0.0092(19) 0.0100(16) -0.0057(17) C19 0.0238(17) 0.043(2) 0.0342(18) -0.0008(17) 0.0100(14) -0.0039(16) C20 0.0231(16) 0.033(2) 0.0203(15) 0.0036(14) 0.0101(13) -0.0027(14) C21 0.0280(17) 0.0334(19) 0.0210(15) 0.0048(15) 0.0101(13) 0.0018(16) C22 0.0234(17) 0.032(2) 0.0237(15) 0.0049(15) 0.0070(13) 0.0028(15) C23 0.048(2) 0.024(2) 0.0344(19) 0.0027(16) 0.0195(17) 0.0024(17) C24 0.0215(17) 0.056(3) 0.0368(19) 0.0098(19) 0.0140(15) 0.0066(17) C25 0.036(2) 0.051(2) 0.043(2) 0.0201(19) 0.0187(18) 0.0170(19) C26 0.039(2) 0.046(2) 0.0286(18) -0.0053(17) 0.0095(15) -0.0077(18) C27 0.0326(19) 0.042(2) 0.0315(19) 0.0084(17) 0.0136(16) 0.0007(18) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . Cl1 . 2.3386(9) yes Ti1 . N1 . 1.713(3) yes Ti1 . N2 . 2.110(2) yes Ti1 . N3 . 2.085(2) yes Ti1 . N4 . 2.228(3) yes Ti1 . C13 . 2.522(3) yes N1 . C1 . 1.392(4) yes N2 . Si1 . 1.735(3) yes N2 . C13 . 1.340(4) yes N3 . C13 . 1.317(4) yes N3 . C20 . 1.451(3) yes N4 . C22 . 1.503(4) yes N4 . C23 . 1.486(4) yes N4 . C24 . 1.485(4) yes Si1 . C25 . 1.863(4) yes Si1 . C26 . 1.859(3) yes Si1 . C27 . 1.867(3) yes C1 . C2 . 1.420(4) yes C1 . C6 . 1.422(4) yes C2 . C3 . 1.387(5) yes C2 . C7 . 1.520(4) yes C3 . C4 . 1.387(4) yes C4 . C5 . 1.385(5) yes C5 . C6 . 1.387(5) yes C6 . C10 . 1.510(4) yes C7 . C8 . 1.538(4) yes C7 . C9 . 1.522(5) yes C10 . C11 . 1.524(5) yes C10 . C12 . 1.524(5) yes C13 . C14 . 1.490(4) yes C14 . C15 . 1.389(5) yes C14 . C19 . 1.393(5) yes C15 . C16 . 1.395(5) yes C16 . C17 . 1.372(5) yes C17 . C18 . 1.376(5) yes C18 . C19 . 1.384(5) yes C20 . C21 . 1.526(4) yes C21 . C22 . 1.526(4) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Ti1 . N1 . 111.32(9) yes Cl1 . Ti1 . N2 . 98.93(7) yes N1 . Ti1 . N2 . 109.03(12) yes Cl1 . Ti1 . N3 . 141.11(8) yes N1 . Ti1 . N3 . 107.30(11) yes N2 . Ti1 . N3 . 63.51(9) yes Cl1 . Ti1 . N4 . 93.38(7) yes N1 . Ti1 . N4 . 102.19(11) yes N2 . Ti1 . N4 . 139.2(1) yes N3 . Ti1 . N4 . 82.7(1) yes Cl1 . Ti1 . C13 . 123.97(7) yes N1 . Ti1 . C13 . 110.87(12) yes N2 . Ti1 . C13 . 32.09(9) yes N3 . Ti1 . C13 . 31.44(9) yes N4 . Ti1 . C13 . 111.7(1) yes Ti1 . N1 . C1 . 175.0(2) yes Ti1 . N2 . Si1 . 133.83(13) yes Ti1 . N2 . C13 . 91.17(18) yes Si1 . N2 . C13 . 134.5(2) yes Ti1 . N3 . C13 . 92.92(17) yes Ti1 . N3 . C20 . 139.9(2) yes C13 . N3 . C20 . 126.9(2) yes Ti1 . N4 . C22 . 114.19(19) yes Ti1 . N4 . C23 . 108.6(2) yes C22 . N4 . C23 . 110.2(2) yes Ti1 . N4 . C24 . 107.9(2) yes C22 . N4 . C24 . 107.0(2) yes C23 . N4 . C24 . 108.8(3) yes N2 . Si1 . C25 . 113.91(14) yes N2 . Si1 . C26 . 109.18(16) yes C25 . Si1 . C26 . 109.40(18) yes N2 . Si1 . C27 . 105.73(14) yes C25 . Si1 . C27 . 109.14(17) yes C26 . Si1 . C27 . 109.35(16) yes N1 . C1 . C2 . 120.2(3) yes N1 . C1 . C6 . 119.6(3) yes C2 . C1 . C6 . 120.2(3) yes C1 . C2 . C3 . 118.6(3) yes C1 . C2 . C7 . 120.0(3) yes C3 . C2 . C7 . 121.3(3) yes C2 . C3 . C4 . 121.4(3) yes C3 . C4 . C5 . 119.7(3) yes C4 . C5 . C6 . 121.7(3) yes C1 . C6 . C5 . 118.4(3) yes C1 . C6 . C10 . 121.0(3) yes C5 . C6 . C10 . 120.7(3) yes C2 . C7 . C8 . 112.8(3) yes C2 . C7 . C9 . 110.4(3) yes C8 . C7 . C9 . 111.3(3) yes C6 . C10 . C11 . 112.7(3) yes C6 . C10 . C12 . 110.3(3) yes C11 . C10 . C12 . 110.9(3) yes Ti1 . C13 . N2 . 56.74(15) yes Ti1 . C13 . N3 . 55.64(15) yes N2 . C13 . N3 . 112.4(3) yes Ti1 . C13 . C14 . 178.1(2) yes N2 . C13 . C14 . 123.1(3) yes N3 . C13 . C14 . 124.6(3) yes C13 . C14 . C15 . 120.4(3) yes C13 . C14 . C19 . 120.5(3) yes C15 . C14 . C19 . 119.0(3) yes C14 . C15 . C16 . 120.1(3) yes C15 . C16 . C17 . 120.0(4) yes C16 . C17 . C18 . 120.4(3) yes C17 . C18 . C19 . 120.1(4) yes C14 . C19 . C18 . 120.3(3) yes N3 . C20 . C21 . 109.4(3) yes C20 . C21 . C22 . 114.8(3) yes N4 . C22 . C21 . 116.2(3) yes #===end data_Compound_10 _database_code_CSD 190463 # Local code AEG2 _publ_section_exptl_refinement ; H atoms were located from Fourier difference syntheses. H atoms bonded to C were refined in a riding model with common U[iso] values for chemically related groups of atoms. H(1) was positionally and isotropically refined. The molecules lie across a crystallographic inversion centre. ; _chemical_name_systematic ; [Ti(N-t-Bu)Cl(mu-Cl){Me3SiN(H)C(Ph)NCH2CH2NMe2}]2 ; _cell_length_a 8.8140(3) _cell_angle_alpha 89.420(2) _cell_length_b 11.6000(5) _cell_angle_beta 107.252(2) _cell_length_c 12.6200(5) _cell_angle_gamma 105.453(2) _cell_volume 1184.4 _symmetry_cell_setting 'triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International_Tables_Vol_IV_Table_2.2B' 'Ti ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C36 H68 Cl4 N8 Si2 Ti2 ' _chemical_formula_moiety ' C36 H68 Cl4 N8 Si2 Ti2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 906.78 _cell_measurement_reflns_used 11043 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 175 _cell_formula_units_Z 1 _exptl_crystal_description 'prism ' _exptl_crystal_colour 'amber ' _exptl_crystal_size_min 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.50 _exptl_crystal_density_diffrn 1.27 _exptl_crystal_F_000 480 _exptl_crystal_density_method none _exptl_crystal_density_meas 'not measured' _diffrn_reflns_av_sigmaI/netI 0.041 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _exptl_absorpt_coefficient_mu 0.64 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.825 _exptl_absorpt_correction_T_max 0.825 _diffrn_radiation_monochromator graphite _diffrn_measurement_device-type 'Enraf-nonius DIP2000' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method omega _diffrn_ambient_temperature 175 _diffrn_reflns_number 11043 _reflns_number_total 4472 _diffrn_reflns_av_R_equivalents 0.02 _reflns_number_observed 4422 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.33 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min -14 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _refine_ls_hydrogen_treatment 'mixed' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens geometric _refine_ls_matrix_type full _refine_ls_weighting_scheme 'Chebychev polynomial' _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack 'not required' _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.41 _refine_diff_density_max 0.41 _refine_ls_number_reflns 4422 _refine_ls_number_parameters 245 _refine_ls_R_factor_obs 0.0459 _refine_ls_wR_factor_obs 0.0348 _refine_ls_goodness_of_fit_obs 1.0669 _refine_ls_shift/esd_max 0.002 _refine_ls_structure_factor_coef F _refine_ls_extinction_coef 56.6(101) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _computing_structure_solution 'SIR92 (Altomare, et al, 1994)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material ; CRYSTALS Issue 10 (Watkin et al, 1996) ; _computing_data_collection 'DIP2000 software 'Xpress' (MAC Science, 1989)' _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Ti1 -0.02420(3) -0.08315(2) 0.34849(2) 0.0165 1.0000 Uani Cl1 -0.12494(5) -0.27320(3) 0.41107(4) 0.0301 1.0000 Uani Cl2 -0.17780(5) 0.01913(3) 0.42616(3) 0.0233 1.0000 Uani N1 -0.1508(2) -0.1050(1) 0.2156(1) 0.0214 1.0000 Uani N2 0.1869(2) -0.1511(1) 0.3208(1) 0.0230 1.0000 Uani N3 0.1524(2) 0.0829(1) 0.3295(1) 0.0189 1.0000 Uani N4 -0.0333(2) 0.1902(1) 0.2481(1) 0.0249 1.0000 Uani Si1 -0.11879(6) 0.31361(4) 0.23173(4) 0.0274 1.0000 Uani C1 -0.2802(2) -0.1380(2) 0.1100(1) 0.0259 1.0000 Uani C2 -0.3198(3) -0.2729(2) 0.0809(2) 0.0426 1.0000 Uani C3 -0.2225(3) -0.0689(2) 0.0191(2) 0.0454 1.0000 Uani C4 -0.4336(3) -0.1103(3) 0.1222(2) 0.0605 1.0000 Uani C5 0.1208(3) -0.2462(2) 0.2287(2) 0.0346 1.0000 Uani C6 0.2798(2) -0.2016(2) 0.4198(2) 0.0300 1.0000 Uani C7 0.3027(2) -0.0472(2) 0.2900(2) 0.0290 1.0000 Uani C8 0.3183(2) 0.0669(1) 0.3540(1) 0.0255 1.0000 Uani C9 0.1229(2) 0.1818(1) 0.2896(1) 0.0194 1.0000 Uani C10 0.2564(2) 0.2914(1) 0.2860(1) 0.0221 1.0000 Uani C11 0.3821(2) 0.3443(2) 0.3819(1) 0.0273 1.0000 Uani C12 0.5026(2) 0.4475(2) 0.3771(2) 0.0352 1.0000 Uani C13 0.4954(3) 0.5001(2) 0.2772(2) 0.0387 1.0000 Uani C14 0.3710(3) 0.4472(2) 0.1814(2) 0.0362 1.0000 Uani C15 0.2520(2) 0.3426(2) 0.1853(1) 0.0271 1.0000 Uani C16 0.0034(3) 0.4365(2) 0.3402(2) 0.0457 1.0000 Uani C17 -0.1429(3) 0.3710(2) 0.0903(2) 0.0479 1.0000 Uani C18 -0.3295(3) 0.2448(2) 0.2428(2) 0.0456 1.0000 Uani H1 -0.100(3) 0.128(2) 0.247(2) 0.029(5) 1.0000 Uiso H21 -0.4107 -0.3002 0.0112 0.074 1.0000 Uiso H22 -0.2036 -0.2880 0.0669 0.074 1.0000 Uiso H23 -0.3282 -0.3052 0.1442 0.074 1.0000 Uiso H31 -0.1232 -0.0780 0.0130 0.074 1.0000 Uiso H32 -0.2171 0.0181 0.0317 0.074 1.0000 Uiso H33 -0.3164 -0.0966 -0.0568 0.074 1.0000 Uiso H41 -0.3984 -0.0148 0.1452 0.074 1.0000 Uiso H42 -0.4455 -0.1503 0.1902 0.074 1.0000 Uiso H43 -0.5270 -0.1464 0.0639 0.074 1.0000 Uiso H51 0.0619 -0.2159 0.1563 0.040 1.0000 Uiso H52 0.0362 -0.3134 0.2471 0.040 1.0000 Uiso H53 0.2166 -0.2681 0.2206 0.040 1.0000 Uiso H61 0.2045 -0.2655 0.4458 0.040 1.0000 Uiso H62 0.3638 -0.2275 0.3958 0.040 1.0000 Uiso H63 0.3328 -0.1463 0.4778 0.040 1.0000 Uiso H71 0.2499 -0.0363 0.2062 0.032 1.0000 Uiso H72 0.4127 -0.0607 0.3110 0.032 1.0000 Uiso H81 0.4036 0.1338 0.3381 0.032 1.0000 Uiso H82 0.3582 0.0574 0.4364 0.032 1.0000 Uiso H111 0.3827 0.3091 0.4549 0.042 1.0000 Uiso H121 0.5785 0.4898 0.4501 0.042 1.0000 Uiso H131 0.5829 0.5769 0.2677 0.042 1.0000 Uiso H141 0.3671 0.4952 0.1178 0.042 1.0000 Uiso H151 0.1558 0.3065 0.1192 0.042 1.0000 Uiso H161 0.1145 0.4777 0.3348 0.076 1.0000 Uiso H162 -0.0576 0.5057 0.3405 0.076 1.0000 Uiso H163 0.0174 0.4027 0.4143 0.076 1.0000 Uiso H171 -0.1793 0.4424 0.0965 0.076 1.0000 Uiso H172 -0.0383 0.4094 0.0905 0.076 1.0000 Uiso H173 -0.1908 0.3091 0.0290 0.076 1.0000 Uiso H181 -0.3134 0.2044 0.3219 0.076 1.0000 Uiso H182 -0.3926 0.2946 0.2339 0.076 1.0000 Uiso H183 -0.3955 0.1741 0.1804 0.076 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0164(1) 0.0169(1) 0.0156(1) 0.00175(9) 0.0062(1) 0.0024(1) Cl1 0.0331(2) 0.0208(2) 0.0330(2) 0.0067(2) 0.0115(2) 0.0003(2) Cl2 0.0217(2) 0.0308(2) 0.0199(2) 0.0019(1) 0.0082(1) 0.0094(2) N1 0.0201(7) 0.0238(6) 0.0196(6) 0.0016(5) 0.0071(5) 0.0038(5) N2 0.0263(8) 0.0235(7) 0.0223(6) 0.0020(5) 0.0098(6) 0.0094(6) N3 0.0170(7) 0.0193(6) 0.0212(6) 0.0028(5) 0.0087(5) 0.0033(5) N4 0.0208(7) 0.0185(6) 0.0332(7) 0.0058(6) 0.0089(6) 0.0011(6) Si1 0.0287(3) 0.0260(2) 0.0306(2) 0.0112(2) 0.0100(2) 0.0118(2) C1 0.0218(9) 0.0342(9) 0.0185(7) 0.0001(6) 0.0048(7) 0.0038(7) C2 0.052(1) 0.035(1) 0.0271(9) -0.0043(8) 0.0085(9) -0.0079(9) C3 0.055(1) 0.047(1) 0.0236(9) 0.0126(8) 0.0082(9) 0.002(1) C4 0.025(1) 0.099(2) 0.049(1) -0.028(1) -0.004(1) 0.019(1) C5 0.041(1) 0.0353(9) 0.0315(9) -0.0058(8) 0.0093(8) 0.0177(8) C6 0.029(1) 0.0336(9) 0.0309(9) 0.0065(7) 0.0078(7) 0.0161(7) C7 0.0274(9) 0.0344(9) 0.0353(9) 0.0095(7) 0.0199(8) 0.0141(7) C8 0.0172(8) 0.0263(8) 0.0349(9) 0.0063(7) 0.0121(7) 0.0044(6) C9 0.0198(8) 0.0203(7) 0.0178(7) 0.0004(6) 0.0084(6) 0.0021(6) C10 0.0229(8) 0.0187(7) 0.0255(8) 0.0006(6) 0.0122(7) 0.0016(6) C11 0.0277(9) 0.0280(8) 0.0240(8) -0.0016(6) 0.0107(7) 0.0006(7) C12 0.033(1) 0.0315(9) 0.0340(9) -0.0088(8) 0.0135(8) -0.0060(8) C13 0.041(1) 0.0256(9) 0.046(1) -0.0001(8) 0.0239(9) -0.0085(8) C14 0.044(1) 0.0303(9) 0.035(1) 0.0110(8) 0.0216(9) 0.0019(8) C15 0.0286(9) 0.0279(8) 0.0243(8) 0.0033(7) 0.0116(7) 0.0029(7) C16 0.063(2) 0.030(1) 0.045(1) 0.0021(8) 0.010(1) 0.020(1) C17 0.048(1) 0.059(1) 0.041(1) 0.027(1) 0.014(1) 0.023(1) C18 0.035(1) 0.051(1) 0.063(1) 0.024(1) 0.022(1) 0.0257(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . Cl1 . 2.3685(4) yes Ti1 . Cl2 . 2.4223(5) yes Ti1 . Cl2 2_556 2.8539(5) yes Ti1 . N1 . 1.694(1) yes Ti1 . N2 . 2.318(1) yes Ti1 . N3 . 2.192(1) yes N1 . C1 . 1.448(2) yes N2 . C5 . 1.480(2) yes N2 . C6 . 1.486(2) yes N2 . C7 . 1.489(2) yes N3 . C8 . 1.464(2) yes N3 . C9 . 1.307(2) yes N4 . H1 . 0.80(2) no N4 . Si1 . 1.771(2) yes N4 . C9 . 1.349(2) yes Si1 . C16 . 1.847(2) yes Si1 . C17 . 1.871(2) yes Si1 . C18 . 1.862(2) yes C1 . C2 . 1.533(3) yes C1 . C3 . 1.525(2) yes C1 . C4 . 1.520(3) yes C7 . C8 . 1.510(2) yes C9 . C10 . 1.496(2) yes C10 . C11 . 1.388(2) yes C10 . C15 . 1.391(2) yes C11 . C12 . 1.387(2) yes C12 . C13 . 1.387(3) yes C13 . C14 . 1.382(3) yes C14 . C15 . 1.388(2) yes Cl2 . H1 . 2.75(2) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Ti1 . Cl2 . 95.91(2) yes Cl1 . Ti1 . N1 . 99.11(5) yes Cl2 . Ti1 . N1 . 97.61(5) yes Cl1 . Ti1 . N2 . 88.02(4) yes Cl2 . Ti1 . N2 . 162.65(4) yes N1 . Ti1 . N2 . 98.44(6) yes Cl1 . Ti1 . N3 . 159.25(4) yes Cl2 . Ti1 . N3 . 94.18(4) yes N1 . Ti1 . N3 . 97.46(6) yes N2 . Ti1 . N3 . 77.25(5) yes Cl1 . Ti1 . Cl2 2_556 85.556(15) yes Cl2 . Ti1 . Cl2 2_556 76.370(15) yes Cl2 2_556 Ti1 . N1 . 172.81(5) yes Cl2 2_556 Ti1 . N2 . 87.14(4) yes Cl2 2_556 Ti1 . N3 . 79.26(4) yes Ti1 2_556 Cl2 . H1 . 123.9(5) yes Ti1 . Cl2 . Ti1 2_556 103.630(15) yes Ti1 . N1 . C1 . 169.8(1) yes Ti1 . N2 . C5 . 110.7(1) yes Ti1 . N2 . C6 . 114.0(1) yes C5 . N2 . C6 . 107.0(1) yes Ti1 . N2 . C7 . 107.2(1) yes C5 . N2 . C7 . 108.8(1) yes C6 . N2 . C7 . 109.1(1) yes Ti1 . N3 . C8 . 110.77(9) yes Ti1 . N3 . C9 . 128.6(1) yes C8 . N3 . C9 . 120.2(1) yes Si1 . N4 . C9 . 132.7(1) yes Si1 . N4 . H1 . 112.6(15) yes C9 . N4 . H1 . 112.2(15) yes N4 . Si1 . C16 . 111.69(9) yes N4 . Si1 . C17 . 112.3(1) yes C16 . Si1 . C17 . 110.2(1) yes N4 . Si1 . C18 . 102.21(8) yes C16 . Si1 . C18 . 112.4(1) yes C17 . Si1 . C18 . 107.7(1) yes N1 . C1 . C2 . 109.3(1) yes N1 . C1 . C3 . 109.7(1) yes C2 . C1 . C3 . 109.2(2) yes N1 . C1 . C4 . 108.2(1) yes C2 . C1 . C4 . 108.9(2) yes C3 . C1 . C4 . 111.4(2) yes N2 . C7 . C8 . 110.7(1) yes N3 . C8 . C7 . 107.5(1) yes N3 . C9 . N4 . 121.0(1) yes N3 . C9 . C10 . 123.2(1) yes N4 . C9 . C10 . 115.8(1) yes C9 . C10 . C11 . 121.0(1) yes C9 . C10 . C15 . 119.4(2) yes C11 . C10 . C15 . 119.6(1) yes C10 . C11 . C12 . 120.0(2) yes C11 . C12 . C13 . 120.2(2) yes C12 . C13 . C14 . 119.9(2) yes C13 . C14 . C15 . 120.2(2) yes C10 . C15 . C14 . 120.1(2) yes Cl2 . H1 . N4 . 127.0(18) no #===end data_Compound_11 _database_code_CSD 190464 # Local code CLB6 _chemical_name_systematic ; [Ti(N-2,6-C6H3Me2)Cl(mu-O){Me3SiN(H)C(Ph)NCH2CH2NMe2}]2 ; _publ_section_exptl_refinement ; The molecules lie on crystallographic 2-fold axes passing through O(1). H(1) was located from a Fourier difference map and positionally refined in the isotropic approximation. Other H atoms were placed geometrically and refined in a riding model. And equivalent isotropic displacement parameters were refined for chemically related groups of H atoms. ; _cell_length_a 13.9462(2) _cell_length_b 10.0038(2) _cell_length_c 17.9894(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.337(1) _cell_angle_gamma 90.00 _cell_volume 2494.45(7) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 2/n 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y,-z+1/2' 'x+1/2,-y,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'Si ' 0.0720 0.0710 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 'International_Tables_Vol_IV_Table_2.2B' 'Ti ' 0.2480 0.4460 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C44 H68 Cl2 N8 O1 Si2 Ti2 ' _chemical_formula_moiety ' C44 H68 Cl2 N8 O1 Si2 Ti2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 931.96 _cell_measurement_reflns_used 5531 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _cell_measurement_temperature 150 _cell_formula_units_Z 2 _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_min 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.24 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method none _exptl_crystal_F_000 1005.88 _exptl_absorpt_coefficient_mu 0.51 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.858 _exptl_absorpt_correction_T_max 0.858 _diffrn_standards_interval_time 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_number 'not measured' _diffrn_standards_decay_% 'not measured' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method 'CCD' _diffrn_ambient_temperature 150 _diffrn_reflns_number 9895 _reflns_number_total 5676 _diffrn_reflns_av_R_equivalents 0.02 _reflns_number_gt 3931 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -18 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _refine_diff_density_min -0.36 _refine_diff_density_max 0.37 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 3931 _refine_ls_number_parameters 278 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0399 _refine_ls_goodness_of_fit_ref 1.0420 _refine_ls_shift/su_max 0.003 _refine_ls_structure_factor_coef F _refine_ls_hydrogen_treatment mixed _atom_sites_solution_primary 'direct methods' _atom_sites_solution_hydrogens mixed _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_abs_structure_flack none _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 0.473 0.210 0.238 ; _refine_ls_extinction_coef 117(29) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SIR92 (Altomare, et al., 1994)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin et al., 1996) ; _computing_molecular_graphics 'CAMERON (Watkin, Prout and Pearce, 1996)' _computing_publication_material ; CRYSTALS Issue 10 (Watkin et al., 1996) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Ti1 0.16857(2) 0.47125(3) 1.182005(18) 0.0160 1.0000 Uani O1 0.2500 0.36841(19) 1.2500 0.0167 1.0000 Uani Cl1 0.13521(4) 0.61687(5) 1.28275(3) 0.0243 1.0000 Uani N1 0.06393(12) 0.37927(17) 1.16203(9) 0.0202 1.0000 Uani N2 0.12280(13) 0.64955(18) 1.1048(1) 0.0233 1.0000 Uani N3 0.24371(12) 0.42985(18) 1.08331(9) 0.0209 1.0000 Uani N4 0.33401(12) 0.24618(19) 1.12863(9) 0.0230 1.0000 Uani Si1 0.40888(4) 0.10351(6) 1.13016(3) 0.0221 1.0000 Uani C1 -0.01513(14) 0.2969(2) 1.1508(1) 0.0203 1.0000 Uani C2 -0.00835(16) 0.1746(2) 1.11169(11) 0.0244 1.0000 Uani C3 -0.08895(18) 0.0926(2) 1.09937(13) 0.0324 1.0000 Uani C4 -0.17640(18) 0.1287(3) 1.12321(14) 0.0359 1.0000 Uani C5 -0.18323(16) 0.2478(3) 1.16157(13) 0.0317 1.0000 Uani C6 -0.10411(15) 0.3322(2) 1.17686(12) 0.0248 1.0000 Uani C7 0.08548(17) 0.1382(2) 1.08323(13) 0.0297 1.0000 Uani C8 -0.11220(17) 0.4584(3) 1.22152(14) 0.0354 1.0000 Uani C9 0.02079(17) 0.6871(3) 1.10976(14) 0.0354 1.0000 Uani C10 0.18113(18) 0.7724(2) 1.11532(14) 0.0341 1.0000 Uani C11 0.12801(17) 0.5936(2) 1.02886(11) 0.0293 1.0000 Uani C12 0.22432(18) 0.5296(3) 1.02307(12) 0.0320 1.0000 Uani C13 0.30315(14) 0.3321(2) 1.07309(11) 0.0198 1.0000 Uani C14 0.33883(16) 0.3091(2) 0.99835(11) 0.0241 1.0000 Uani C15 0.27911(19) 0.2495(3) 0.94053(13) 0.0349 1.0000 Uani C16 0.3129(2) 0.2300(3) 0.87129(13) 0.0425 1.0000 Uani C17 0.4047(2) 0.2715(3) 0.85966(14) 0.0458 1.0000 Uani C18 0.4639(2) 0.3307(3) 0.91690(15) 0.0427 1.0000 Uani C19 0.43145(18) 0.3489(2) 0.98686(13) 0.0318 1.0000 Uani C20 0.53871(17) 0.1503(3) 1.13912(15) 0.0375 1.0000 Uani C21 0.37766(18) -0.0038(2) 1.04645(13) 0.0323 1.0000 Uani C22 0.3823(2) 0.0145(3) 1.21618(13) 0.0355 1.0000 Uani H1 0.315(2) 0.269(3) 1.1719(16) 0.036(7) 1.0000 Uiso H31 -0.08345 0.0055 1.07287 0.046 1.0000 Uiso H41 -0.23411 0.0695 1.11286 0.046 1.0000 Uiso H51 -0.24647 0.2741 1.17856 0.046 1.0000 Uiso H71 0.07871 0.0501 1.05694 0.084 1.0000 Uiso H72 0.13711 0.1319 1.12632 0.084 1.0000 Uiso H73 0.10316 0.2084 1.04762 0.084 1.0000 Uiso H81 -0.17945 0.4677 1.23521 0.084 1.0000 Uiso H82 -0.06594 0.4543 1.26808 0.084 1.0000 Uiso H83 -0.09636 0.5371 1.19084 0.084 1.0000 Uiso H91 -0.02086 0.6057 1.10288 0.050 1.0000 Uiso H92 0.01457 0.7275 1.15986 0.050 1.0000 Uiso H93 -0.00011 0.7536 1.06971 0.050 1.0000 Uiso H101 0.25056 0.7503 1.11244 0.050 1.0000 Uiso H102 0.17354 0.8120 1.16537 0.050 1.0000 Uiso H103 0.15886 0.8382 1.07522 0.050 1.0000 Uiso H111 0.07685 0.5239 1.01884 0.042 1.0000 Uiso H112 0.11675 0.6669 0.99108 0.042 1.0000 Uiso H121 0.27535 0.6003 1.02860 0.042 1.0000 Uiso H122 0.22445 0.4850 0.97335 0.042 1.0000 Uiso H151 0.21238 0.2213 0.94896 0.055 1.0000 Uiso H161 0.2707 0.1863 0.82968 0.055 1.0000 Uiso H171 0.4285 0.2582 0.80975 0.055 1.0000 Uiso H181 0.5300 0.3609 0.90794 0.055 1.0000 Uiso H191 0.47457 0.3905 1.02863 0.055 1.0000 Uiso H201 0.57904 0.0676 1.13958 0.075 1.0000 Uiso H202 0.55538 0.2008 1.18677 0.075 1.0000 Uiso H203 0.55148 0.2077 1.09579 0.075 1.0000 Uiso H211 0.42140 -0.0833 1.04913 0.075 1.0000 Uiso H212 0.30922 -0.0344 1.04506 0.075 1.0000 Uiso H213 0.38565 0.0486 1.00020 0.075 1.0000 Uiso H221 0.4216 -0.0693 1.22215 0.075 1.0000 Uiso H222 0.3988 0.0734 1.26064 0.075 1.0000 Uiso H223 0.3122 -0.0087 1.21201 0.075 1.0000 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.01689(16) 0.01725(17) 0.01415(16) -0.00101(13) 0.00264(11) 0.00080(14) O1 0.0160(9) 0.0180(9) 0.0166(9) 0.0000 0.0039(7) 0.0000 Cl1 0.0284(3) 0.0247(3) 0.0208(2) -0.00591(18) 0.00713(18) 0.0008(2) N1 0.0193(8) 0.0230(9) 0.0183(8) -0.0025(6) 0.0021(6) -0.0001(7) N2 0.0250(9) 0.0227(9) 0.0224(8) -0.0019(7) 0.0028(7) 0.0055(7) N3 0.0245(8) 0.0235(9) 0.0155(8) 0.0015(6) 0.0060(6) 0.0024(7) N4 0.0256(9) 0.0265(9) 0.0182(8) -0.0015(7) 0.0077(7) 0.0069(7) Si1 0.0232(3) 0.0221(3) 0.0216(3) -0.0021(2) 0.0053(2) 0.0037(2) C1 0.0201(9) 0.024(1) 0.0158(9) 0.0017(7) -0.0003(7) -0.0013(8) C2 0.029(1) 0.0231(11) 0.021(1) 0.0022(8) 0.0012(8) -0.0009(8) C3 0.0398(13) 0.0280(12) 0.0289(11) -0.0026(9) 0.001(1) -0.009(1) C4 0.0339(12) 0.0390(14) 0.0346(12) -0.003(1) 0.003(1) -0.0178(11) C5 0.024(1) 0.0430(14) 0.0281(11) -0.002(1) 0.0036(8) -0.008(1) C6 0.023(1) 0.0306(11) 0.021(1) -0.0010(8) 0.0031(8) -0.0009(9) C7 0.0356(12) 0.0239(11) 0.0300(11) -0.0032(9) 0.0057(9) 0.0040(9) C8 0.0279(11) 0.0377(13) 0.0428(13) -0.0114(11) 0.015(1) -0.004(1) C9 0.0291(11) 0.0418(14) 0.0349(12) 0.0054(11) 0.001(1) 0.0147(11) C10 0.0421(13) 0.0235(11) 0.0355(12) 0.0066(9) -0.001(1) -0.001(1) C11 0.0373(12) 0.0321(12) 0.0178(9) 0.0012(9) -0.0008(9) 0.008(1) C12 0.0432(13) 0.0335(12) 0.021(1) 0.0070(9) 0.0132(9) 0.0111(11) C13 0.0209(9) 0.021(1) 0.0181(9) -0.0025(7) 0.0054(7) -0.0031(8) C14 0.0309(11) 0.023(1) 0.021(1) 0.0024(8) 0.0117(8) 0.0047(8) C15 0.0423(13) 0.0398(14) 0.0238(11) -0.004(1) 0.009(1) 0.0008(11) C16 0.0638(18) 0.0431(15) 0.0217(11) -0.003(1) 0.0090(11) 0.0063(13) C17 0.0722(19) 0.0411(15) 0.0299(12) 0.0081(11) 0.0317(13) 0.0167(14) C18 0.0514(16) 0.0376(14) 0.0448(15) 0.0081(11) 0.0306(13) 0.0041(12) C19 0.0366(12) 0.0280(11) 0.0340(12) 0.0033(9) 0.018(1) -0.000(1) C20 0.0260(11) 0.0475(15) 0.0392(13) -0.0057(11) 0.004(1) 0.0033(11) C21 0.0388(12) 0.0276(12) 0.0306(11) -0.0071(9) 0.0048(9) 0.0018(9) C22 0.0463(14) 0.0318(12) 0.0291(12) 0.004(1) 0.008(1) 0.0056(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . O1 . 1.8808(11) yes Ti1 . Cl1 . 2.4103(6) yes Ti1 . N1 . 1.7291(17) yes Ti1 . N2 . 2.3068(18) yes Ti1 . N3 . 2.1984(16) yes O1 . H1 . 2.02(3) yes O1 . H1 3_557 2.02(3) yes N1 . C1 . 1.373(3) yes N2 . C9 . 1.484(3) yes N2 . C10 . 1.475(3) yes N2 . C11 . 1.486(3) yes N3 . C12 . 1.476(3) yes N3 . C13 . 1.308(3) yes N4 . Si1 . 1.7668(18) yes N4 . C13 . 1.352(3) yes N4 . H1 . 0.88(3) yes Si1 . C20 . 1.860(2) yes Si1 . C21 . 1.862(2) yes Si1 . C22 . 1.858(2) yes C1 . C2 . 1.421(3) yes C1 . C6 . 1.418(3) yes C2 . C3 . 1.389(3) yes C2 . C7 . 1.502(3) yes C3 . C4 . 1.385(4) yes C4 . C5 . 1.385(4) yes C5 . C6 . 1.393(3) yes C6 . C8 . 1.507(3) yes C11 . C12 . 1.502(3) yes C13 . C14 . 1.502(3) yes C14 . C15 . 1.393(3) yes C14 . C19 . 1.389(3) yes C15 . C16 . 1.393(3) yes C16 . C17 . 1.385(4) yes C17 . C18 . 1.380(4) yes C18 . C19 . 1.395(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Ti1 . Cl1 . 89.68(4) yes O1 . Ti1 . N1 . 106.21(7) yes Cl1 . Ti1 . N1 . 104.44(6) yes O1 . Ti1 . N2 . 157.15(6) yes Cl1 . Ti1 . N2 . 85.51(5) yes N1 . Ti1 . N2 . 96.62(7) yes O1 . Ti1 . N3 . 96.59(5) yes Cl1 . Ti1 . N3 . 150.45(5) yes N1 . Ti1 . N3 . 101.45(7) yes N2 . Ti1 . N3 . 77.55(6) yes Ti1 . O1 . Ti1 3_557 113.7(1) yes Ti1 . O1 . H1 . 95.9(8) yes Ti1 . O1 . H1 3_557 116.0(8) yes H1 . O1 . H1 3_557 120.8(16) yes O1 . H1 . N4 . 161.2(26) no Ti1 . N1 . C1 . 174.43(15) yes Ti1 . N2 . C9 . 111.31(14) yes Ti1 . N2 . C10 . 117.08(13) yes C9 . N2 . C10 . 107.47(18) yes Ti1 . N2 . C11 . 102.95(13) yes C9 . N2 . C11 . 107.16(17) yes C10 . N2 . C11 . 110.44(18) yes Ti1 . N3 . C12 . 113.61(13) yes Ti1 . N3 . C13 . 128.33(14) yes C12 . N3 . C13 . 118.04(17) yes Si1 . N4 . C13 . 131.64(14) yes Si1 . N4 . H1 . 115.5(19) yes C13 . N4 . H1 . 112.8(19) yes N4 . Si1 . C20 . 111.47(11) yes N4 . Si1 . C21 . 111.6(1) yes C20 . Si1 . C21 . 110.72(11) yes N4 . Si1 . C22 . 103.2(1) yes C20 . Si1 . C22 . 109.28(12) yes C21 . Si1 . C22 . 110.29(11) yes N1 . C1 . C2 . 119.55(18) yes N1 . C1 . C6 . 121.33(19) yes C2 . C1 . C6 . 119.11(19) yes C1 . C2 . C3 . 119.4(2) yes C1 . C2 . C7 . 119.08(19) yes C3 . C2 . C7 . 121.5(2) yes C2 . C3 . C4 . 121.4(2) yes C3 . C4 . C5 . 119.3(2) yes C4 . C5 . C6 . 121.6(2) yes C1 . C6 . C5 . 119.1(2) yes C1 . C6 . C8 . 120.26(19) yes C5 . C6 . C8 . 120.6(2) yes N2 . C11 . C12 . 111.05(17) yes N3 . C12 . C11 . 109.28(17) yes N3 . C13 . N4 . 121.77(17) yes N3 . C13 . C14 . 121.18(18) yes N4 . C13 . C14 . 117.05(17) yes C13 . C14 . C15 . 120.27(19) yes C13 . C14 . C19 . 119.7(2) yes C15 . C14 . C19 . 120.1(2) yes C14 . C15 . C16 . 119.6(2) yes C15 . C16 . C17 . 120.2(3) yes C16 . C17 . C18 . 120.2(2) yes C17 . C18 . C19 . 120.2(2) yes C14 . C19 . C18 . 119.8(2) yes #===end