#------------------------------------------------------------------------------ #$Date: 2009-11-23 07:50:56 +0200 (Mon, 23 Nov 2009) $ #$Revision: 903 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/7102561.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7102561 loop_ _publ_author_name 'Tamm, Matthias' 'Randoll, S\"oren' 'Bannenberg, Thomas' 'Herdtweck, Eberhardt' _publ_section_title ; Titanium complexes with imidazolin-2-iminato ligands. ; _journal_issue 7 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 876 _journal_page_last 877 _journal_year 2004 _chemical_formula_moiety 'C14 H29 N3 Si' _chemical_formula_sum 'C14 H29 N3 Si' _chemical_formula_weight 267.49 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 24-Oct-03 _audit_creation_method 'PLATON option' _audit_update_record ; 24-Oct-03 Updated by the Author E.H. Textwriting by E.H. Checkcif OK 14-Jan-04 Updated by the Author E.H. 20-Jan-04 Updated by the Author E.H. ; _cell_angle_alpha 84.7122(12) _cell_angle_beta 83.0332(13) _cell_angle_gamma 63.7546(9) _cell_formula_units_Z 2 _cell_length_a 9.0758(2) _cell_length_b 9.4187(2) _cell_length_c 11.0961(3) _cell_measurement_reflns_used 3090 _cell_measurement_temperature 173(1) _cell_measurement_theta_max 25.40 _cell_measurement_theta_min 1.85 _cell_volume 843.66(4) _computing_cell_refinement 'DENZO (Nonius, 2001b)' _computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)' _computing_data_reduction 'DENZO (Nonius, 2001b)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _diffrn_ambient_temperature 173(1) _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 18 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Nonius \k-CCD diffractometer' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 18531 _diffrn_reflns_theta_full 25.40 _diffrn_reflns_theta_max 25.40 _diffrn_reflns_theta_min 1.85 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 0.130 _exptl_absorpt_correction_T_max 0.965 _exptl_absorpt_correction_T_min 0.955 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(applied during the scaling procedure; Nonius, 2001b)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.053 _exptl_crystal_density_meas none _exptl_crystal_density_method none _exptl_crystal_description fragment _exptl_crystal_F_000 296 _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.35 _refine_diff_density_max 0.481 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.048 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 279 _refine_ls_number_reflns 3097 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.149 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0465 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0549P)^2^+0.5892P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_gt 0.1333 _refine_ls_wR_factor_ref 0.1367 _reflns_number_gt 2758 _reflns_number_total 3097 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file b401041h.txt _[local]_cod_data_source_block RANE-4317-173 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Si Si 0.0817 0.0704 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Si Si Uani 0.12347(7) 0.84057(7) 0.25932(6) 1.000 0.0344(2) N1 N Uani 0.3060(2) 0.6861(2) 0.26453(17) 1.000 0.0341(5) N2 N Uani 0.4735(2) 0.4093(2) 0.30412(16) 1.000 0.0308(5) N3 N Uani 0.5867(2) 0.5414(2) 0.18475(15) 1.000 0.0307(5) C1 C Uani 0.4396(3) 0.5593(2) 0.25118(18) 1.000 0.0290(6) C2 C Uani 0.6367(3) 0.3071(3) 0.2718(2) 1.000 0.0378(7) C3 C Uani 0.7050(3) 0.3865(3) 0.2000(2) 1.000 0.0376(7) C4 C Uani 0.3536(3) 0.3675(3) 0.38516(19) 1.000 0.0342(7) C5 C Uani 0.4370(4) 0.1922(3) 0.4246(3) 1.000 0.0506(9) C6 C Uani 0.2067(3) 0.3973(3) 0.3156(2) 1.000 0.0412(8) C7 C Uani 0.3005(3) 0.4656(3) 0.4987(2) 1.000 0.0418(8) C8 C Uani 0.6141(3) 0.6707(3) 0.11252(19) 1.000 0.0348(7) C9 C Uani 0.4925(3) 0.7392(3) 0.0152(2) 1.000 0.0442(8) C10 C Uani 0.5959(3) 0.7962(3) 0.1986(2) 1.000 0.0420(8) C11 C Uani 0.7889(3) 0.6015(4) 0.0491(3) 1.000 0.0478(9) C12 C Uani 0.0214(4) 0.8369(4) 0.1237(3) 1.000 0.0546(10) C13 C Uani 0.1384(4) 1.0337(3) 0.2517(3) 1.000 0.0531(9) C14 C Uani -0.0233(4) 0.8463(4) 0.3959(3) 1.000 0.0580(10) H21 H Uiso 0.685(3) 0.197(4) 0.296(2) 1.000 0.053(7) H31 H Uiso 0.814(4) 0.351(3) 0.164(3) 1.000 0.056(8) H51 H Uiso 0.475(4) 0.127(4) 0.353(3) 1.000 0.058(8) H52 H Uiso 0.357(3) 0.164(3) 0.476(2) 1.000 0.044(7) H53 H Uiso 0.530(4) 0.174(4) 0.474(3) 1.000 0.063(9) H61 H Uiso 0.240(3) 0.335(4) 0.246(3) 1.000 0.057(8) H62 H Uiso 0.152(3) 0.508(3) 0.285(2) 1.000 0.045(7) H63 H Uiso 0.127(3) 0.370(3) 0.369(2) 1.000 0.050(7) H71 H Uiso 0.256(3) 0.579(4) 0.477(2) 1.000 0.049(7) H72 H Uiso 0.391(4) 0.438(3) 0.546(3) 1.000 0.053(8) H73 H Uiso 0.215(3) 0.443(3) 0.549(2) 1.000 0.043(7) H91 H Uiso 0.379(4) 0.783(3) 0.046(2) 1.000 0.046(7) H92 H Uiso 0.504(4) 0.652(4) -0.042(3) 1.000 0.067(9) H93 H Uiso 0.511(3) 0.821(3) -0.035(3) 1.000 0.057(8) H101 H Uiso 0.683(4) 0.752(3) 0.254(3) 1.000 0.053(8) H102 H Uiso 0.483(4) 0.841(3) 0.246(3) 1.000 0.053(8) H103 H Uiso 0.610(3) 0.880(4) 0.151(3) 1.000 0.058(8) H111 H Uiso 0.869(4) 0.556(3) 0.109(3) 1.000 0.052(8) H112 H Uiso 0.804(4) 0.686(4) -0.002(3) 1.000 0.059(8) H113 H Uiso 0.800(3) 0.517(4) -0.010(3) 1.000 0.058(8) H121 H Uiso -0.002(4) 0.747(4) 0.131(3) 1.000 0.073(10) H122 H Uiso 0.078(4) 0.846(4) 0.046(3) 1.000 0.077(10) H123 H Uiso -0.086(5) 0.927(5) 0.121(3) 1.000 0.088(11) H131 H Uiso 0.208(5) 1.025(5) 0.168(4) 1.000 0.098(12) H132 H Uiso 0.204(4) 1.033(4) 0.321(3) 1.000 0.065(9) H133 H Uiso 0.032(4) 1.122(4) 0.258(3) 1.000 0.070(9) H141 H Uiso -0.042(3) 0.741(4) 0.396(2) 1.000 0.054(8) H142 H Uiso -0.127(5) 0.952(5) 0.400(3) 1.000 0.086(11) H143 H Uiso 0.027(4) 0.847(4) 0.474(3) 1.000 0.086(11) 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 Si 0.0291(3) 0.0261(3) 0.0446(4) 0.0002(2) -0.0018(2) -0.0097(3) N1 0.0305(9) 0.0274(9) 0.0403(10) 0.0004(7) 0.0000(8) -0.0101(8) N2 0.0312(9) 0.0261(9) 0.0329(9) 0.0001(7) -0.0030(7) -0.0108(7) N3 0.0279(9) 0.0308(9) 0.0321(9) -0.0016(7) -0.0017(7) -0.0117(7) C1 0.0317(10) 0.0308(10) 0.0269(10) -0.0014(8) -0.0046(8) -0.0154(9) C2 0.0329(12) 0.0278(11) 0.0429(12) 0.0003(9) -0.0062(9) -0.0041(9) C3 0.0278(11) 0.0348(12) 0.0421(12) -0.0032(9) -0.0026(9) -0.0061(9) C4 0.0408(12) 0.0308(11) 0.0331(11) 0.0026(9) -0.0026(9) -0.0184(10) C5 0.0568(17) 0.0351(13) 0.0562(16) 0.0104(12) -0.0020(14) -0.0199(12) C6 0.0452(14) 0.0417(14) 0.0440(13) 0.0005(11) -0.0040(11) -0.0261(12) C7 0.0496(14) 0.0473(15) 0.0325(12) 0.0010(10) -0.0009(11) -0.0260(12) C8 0.0356(11) 0.0404(12) 0.0328(11) 0.0011(9) -0.0013(9) -0.0216(10) C9 0.0456(15) 0.0563(16) 0.0354(12) 0.0098(11) -0.0063(11) -0.0279(13) C10 0.0467(14) 0.0428(13) 0.0445(13) -0.0011(11) -0.0025(12) -0.0273(12) C11 0.0408(14) 0.0566(16) 0.0485(15) -0.0030(13) 0.0055(12) -0.0257(13) C12 0.0465(16) 0.0562(17) 0.0654(19) 0.0096(14) -0.0183(14) -0.0252(14) C13 0.0473(15) 0.0291(13) 0.079(2) -0.0037(12) -0.0033(15) -0.0136(12) C14 0.0441(15) 0.0455(16) 0.0674(19) -0.0014(13) 0.0141(14) -0.0092(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Si N1 1.6554(19) yes Si C12 1.871(4) yes Si C13 1.877(3) yes Si C14 1.880(4) yes N1 C1 1.275(3) yes N2 C1 1.394(2) yes N2 C2 1.387(3) yes N2 C4 1.491(3) yes N3 C1 1.393(3) yes N3 C3 1.387(3) yes N3 C8 1.492(3) yes C2 C3 1.326(4) no C4 C5 1.527(4) no C4 C6 1.527(4) no C4 C7 1.532(3) no C8 C9 1.527(4) no C8 C10 1.528(3) no C8 C11 1.528(4) no C2 H21 0.96(3) no C3 H31 0.94(4) no C5 H51 0.98(3) no C5 H52 0.98(3) no C5 H53 1.00(4) no C6 H61 0.95(3) no C6 H62 0.98(3) no C6 H63 0.99(3) no C7 H71 0.98(3) no C7 H72 0.95(4) no C7 H73 0.99(3) no C9 H91 0.96(3) no C9 H92 1.05(3) no C9 H93 0.97(3) no C10 H101 0.98(4) no C10 H102 1.02(4) no C10 H103 0.96(3) no C11 H111 0.97(4) no C11 H112 0.98(4) no C11 H113 1.04(3) no C12 H121 0.95(4) no C12 H122 0.97(4) no C12 H123 0.97(5) no C13 H131 1.05(5) no C13 H132 1.03(4) no C13 H133 0.96(4) no C14 H141 1.08(3) no C14 H142 1.02(4) no C14 H143 1.03(4) no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N1 Si C12 110.96(13) yes N1 Si C13 112.26(13) yes N1 Si C14 112.85(13) yes C12 Si C13 107.84(15) yes C12 Si C14 106.34(17) yes C13 Si C14 106.24(15) yes Si N1 C1 169.33(18) yes C1 N2 C2 109.2(2) yes C1 N2 C4 125.05(19) yes C2 N2 C4 125.74(19) yes C1 N3 C3 109.39(18) yes C1 N3 C8 125.12(18) yes C3 N3 C8 125.4(2) yes N1 C1 N2 127.8(2) yes N1 C1 N3 127.65(19) yes N2 C1 N3 104.52(17) yes N2 C2 C3 108.6(2) yes N3 C3 C2 108.3(2) yes N2 C4 C5 109.4(2) yes N2 C4 C6 109.26(18) yes N2 C4 C7 109.0(2) yes C5 C4 C6 108.9(2) no C5 C4 C7 108.5(2) no C6 C4 C7 111.8(2) no N3 C8 C9 109.5(2) yes N3 C8 C10 108.91(17) yes N3 C8 C11 109.0(2) yes C9 C8 C10 112.1(2) no C9 C8 C11 108.3(2) no C10 C8 C11 109.1(2) no N2 C2 H21 123.1(18) no C3 C2 H21 128.2(18) no N3 C3 H31 122.5(17) no C2 C3 H31 129.2(17) no C4 C5 H51 110(2) no C4 C5 H52 109.3(15) no C4 C5 H53 109(2) no H51 C5 H52 108(3) no H51 C5 H53 112(3) no H52 C5 H53 108(2) no C4 C6 H61 111(2) no C4 C6 H62 111.9(17) no C4 C6 H63 109.5(15) no H61 C6 H62 106(2) no H61 C6 H63 108(2) no H62 C6 H63 110(2) no C4 C7 H71 111.2(14) no C4 C7 H72 111.1(18) no C4 C7 H73 108.5(14) no H71 C7 H72 108(2) no H71 C7 H73 109(2) no H72 C7 H73 108(3) no C8 C9 H91 114.6(15) no C8 C9 H92 112(2) no C8 C9 H93 110.8(18) no H91 C9 H92 104(3) no H91 C9 H93 108(2) no H92 C9 H93 108(3) no C8 C10 H101 110.3(16) no C8 C10 H102 111.5(19) no C8 C10 H103 108(2) no H101 C10 H102 111(3) no H101 C10 H103 107(3) no H102 C10 H103 109(2) no C8 C11 H111 110(2) no C8 C11 H112 109(2) no C8 C11 H113 108.7(18) no H111 C11 H112 112(3) no H111 C11 H113 111(2) no H112 C11 H113 106(3) no Si C12 H121 110(2) no Si C12 H122 115(2) no Si C12 H123 111(2) no H121 C12 H122 113(3) no H121 C12 H123 104(4) no H122 C12 H123 103(3) no Si C13 H131 100(2) no Si C13 H132 108.7(19) no Si C13 H133 112(2) no H131 C13 H132 110(3) no H131 C13 H133 116(3) no H132 C13 H133 110(3) no Si C14 H141 106.8(14) no Si C14 H142 112(2) no Si C14 H143 110(2) no H141 C14 H142 117(3) no H141 C14 H143 110(2) no H142 C14 H143 101(3) no