# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2090 data_ticlose_[TiCl4(oC6H4(SeMe)2)] #------------------------------------------------------------------------------ _audit_creation_date '19100-04-10' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' Dalton Transactions' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Dr G. Reid' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; This is the CIF file for [TiCl4{o-C6H4(SeMe)2}] included in Dalton manuscript B002792H. ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 8.2588(9) _cell_length_b 11.091(2) _cell_length_c 8.232(1) _cell_angle_alpha 90.74(1) _cell_angle_beta 97.72(1) _cell_angle_gamma 108.93(1) _cell_volume 705.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.8 _cell_measurement_theta_max 18.6 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 2.136 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 453.80 _chemical_formula_analytical ? _chemical_formula_sum 'C8 H10 Cl4 Se2 Ti ' _chemical_formula_moiety 'C8 H10 Cl4 Se2 Ti ' _chemical_formula_structural [TiCl4{o-C6H4(SeMe)2}] _chemical_compound_source ? _exptl_crystal_F_000 432.00 _exptl_absorpt_coefficient_mu 6.489 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.716 _exptl_special_details ; The scan width was (1.26+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_ambient_temperature 150.0 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.52 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -2 3 0 -1 3 0 -2 3 _diffrn_reflns_number 2669 _reflns_number_total 2478 _reflns_number_gt 1972 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.05566 _diffrn_reflns_av_sigmaI/netI 0.060 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.07649 _diffrn_orient_matrix_UB_12 -0.01263 _diffrn_orient_matrix_UB_13 0.08713 _diffrn_orient_matrix_UB_21 -0.00534 _diffrn_orient_matrix_UB_22 -0.09127 _diffrn_orient_matrix_UB_23 0.00397 _diffrn_orient_matrix_UB_31 0.10423 _diffrn_orient_matrix_UB_32 0.02508 _diffrn_orient_matrix_UB_33 0.08646 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 16 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 20 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Se 0 4 -0.178 2.223 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 8 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ti 0 2 0.248 0.446 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Se(1) 0.11810(7) 0.25507(5) 0.47971(6) 0.0166(1) 1.000 . Uani d ? Se(2) -0.16769(7) 0.08877(5) 0.70765(7) 0.0172(1) 1.000 . Uani d ? Ti(1) 0.1675(1) 0.24016(9) 0.8121(1) 0.0152(2) 1.000 . Uani d ? Cl(1) 0.0514(2) 0.3984(1) 0.8290(2) 0.0271(4) 1.000 . Uani d ? Cl(2) 0.1321(2) 0.1790(1) 1.0658(2) 0.0269(4) 1.000 . Uani d ? Cl(3) 0.2180(2) 0.0565(1) 0.7338(2) 0.0216(4) 1.000 . Uani d ? Cl(4) 0.4406(2) 0.3677(1) 0.8127(2) 0.0298(4) 1.000 . Uani d ? C(1) 0.2218(7) 0.4361(6) 0.4438(8) 0.032(2) 1.000 . Uani d ? C(2) -0.1212(6) 0.2438(5) 0.4291(6) 0.017(1) 1.000 . Uani d ? C(3) -0.1754(7) 0.2939(5) 0.2867(6) 0.020(1) 1.000 . Uani d ? C(4) -0.3469(7) 0.2861(6) 0.2489(7) 0.025(2) 1.000 . Uani d ? C(5) -0.4645(7) 0.2248(6) 0.3507(7) 0.025(2) 1.000 . Uani d ? C(6) -0.4118(7) 0.1709(5) 0.4925(7) 0.021(1) 1.000 . Uani d ? C(7) -0.2390(7) 0.1800(5) 0.5301(6) 0.016(1) 1.000 . Uani d ? C(8) -0.2986(7) 0.1231(7) 0.8713(7) 0.031(2) 1.000 . Uani d ? H(1) 0.3443 0.4594 0.4650 0.038 1.000 . Uiso c ? H(2) 0.1875 0.4512 0.3332 0.038 1.000 . Uiso c ? H(3) 0.1840 0.4857 0.5156 0.038 1.000 . Uiso c ? H(4) -0.0949 0.3335 0.2153 0.023 1.000 . Uiso c ? H(5) -0.3839 0.3227 0.1532 0.030 1.000 . Uiso c ? H(6) -0.5823 0.2192 0.3242 0.030 1.000 . Uiso c ? H(7) -0.4930 0.1288 0.5620 0.025 1.000 . Uiso c ? H(8) -0.2654 0.2127 0.8946 0.037 1.000 . Uiso c ? H(9) -0.4187 0.0905 0.8303 0.037 1.000 . Uiso c ? H(10) -0.2758 0.0830 0.9689 0.037 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Se(1) 0.0116(3) 0.0237(3) 0.0152(3) 0.0055(2) 0.0040(2) 0.0069(2) Se(2) 0.0112(3) 0.0225(3) 0.0174(3) 0.0039(2) 0.0032(2) 0.0094(2) Ti(1) 0.0119(5) 0.0184(5) 0.0140(5) 0.0039(4) 0.0003(4) 0.0045(4) Cl(1) 0.0327(8) 0.0226(7) 0.0302(8) 0.0137(6) 0.0068(7) 0.0047(6) Cl(2) 0.0289(8) 0.0389(9) 0.0152(7) 0.0134(7) 0.0042(6) 0.0098(6) Cl(3) 0.0190(7) 0.0232(7) 0.0264(7) 0.0105(6) 0.0064(6) 0.0066(6) Cl(4) 0.0150(7) 0.0331(8) 0.0324(8) -0.0025(6) -0.0013(6) 0.0069(7) C(1) 0.020(3) 0.033(4) 0.035(4) -0.002(3) 0.004(3) 0.020(3) C(2) 0.011(3) 0.019(3) 0.022(3) 0.006(2) 0.003(2) 0.007(2) C(3) 0.019(3) 0.018(3) 0.018(3) 0.002(2) 0.002(2) 0.005(2) C(4) 0.027(3) 0.028(3) 0.020(3) 0.012(3) -0.002(3) 0.007(3) C(5) 0.013(3) 0.033(3) 0.031(3) 0.012(3) -0.003(2) 0.000(3) C(6) 0.015(3) 0.028(3) 0.020(3) 0.006(2) 0.005(2) 0.007(2) C(7) 0.016(3) 0.018(3) 0.012(3) 0.005(2) 0.001(2) 0.004(2) C(8) 0.020(3) 0.058(4) 0.020(3) 0.017(3) 0.010(3) 0.014(3) _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 1972 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_all 0.0352 _refine_ls_wR_factor_ref 0.0352 _refine_ls_goodness_of_fit_all 1.634 _refine_ls_goodness_of_fit_ref 1.634 _refine_ls_shift/su_max 0.0099 _refine_ls_shift/su_mean 0.0019 _refine_diff_density_min -0.84 _refine_diff_density_max 0.61 #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se(1) Ti(1) 2.727(1) . . yes Se(1) C(1) 1.954(6) . . yes Se(1) C(2) 1.927(5) . . yes Se(2) Ti(1) 2.744(1) . . yes Se(2) C(7) 1.924(5) . . yes Se(2) C(8) 1.941(6) . . yes Ti(1) Cl(1) 2.267(2) . . yes Ti(1) Cl(2) 2.231(2) . . yes Ti(1) Cl(3) 2.308(2) . . yes Ti(1) Cl(4) 2.239(2) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.96 . . no C(1) H(3) 0.96 . . no C(2) C(3) 1.386(7) . . yes C(2) C(7) 1.387(7) . . yes C(3) C(4) 1.384(8) . . yes C(3) H(4) 0.97 . . no C(4) C(5) 1.383(8) . . yes C(4) H(5) 0.96 . . no C(5) C(6) 1.400(8) . . yes C(5) H(6) 0.97 . . no C(6) C(7) 1.389(7) . . yes C(6) H(7) 0.97 . . no C(8) H(8) 0.96 . . no C(8) H(9) 0.96 . . no C(8) H(10) 0.96 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ti(1) Se(1) C(1) 105.0(2) . . . yes Ti(1) Se(1) C(2) 103.9(2) . . . yes C(1) Se(1) C(2) 97.9(2) . . . yes Ti(1) Se(2) C(7) 102.5(2) . . . yes Ti(1) Se(2) C(8) 104.8(2) . . . yes C(7) Se(2) C(8) 99.8(2) . . . yes Se(1) Ti(1) Se(2) 74.42(3) . . . yes Se(1) Ti(1) Cl(1) 87.20(5) . . . yes Se(1) Ti(1) Cl(2) 162.48(6) . . . yes Se(1) Ti(1) Cl(3) 80.74(5) . . . yes Se(1) Ti(1) Cl(4) 87.69(5) . . . yes Se(2) Ti(1) Cl(1) 84.41(5) . . . yes Se(2) Ti(1) Cl(2) 88.46(5) . . . yes Se(2) Ti(1) Cl(3) 81.00(4) . . . yes Se(2) Ti(1) Cl(4) 162.05(6) . . . yes Cl(1) Ti(1) Cl(2) 94.94(6) . . . yes Cl(1) Ti(1) Cl(3) 163.11(7) . . . yes Cl(1) Ti(1) Cl(4) 96.42(7) . . . yes Cl(2) Ti(1) Cl(3) 93.14(6) . . . yes Cl(2) Ti(1) Cl(4) 109.28(7) . . . yes Cl(3) Ti(1) Cl(4) 94.87(6) . . . yes Se(1) C(1) H(1) 110.8 . . . no Se(1) C(1) H(2) 110.5 . . . no Se(1) C(1) H(3) 110.1 . . . no H(1) C(1) H(2) 109.1 . . . no H(1) C(1) H(3) 108.4 . . . no H(2) C(1) H(3) 107.9 . . . no Se(1) C(2) C(3) 119.3(4) . . . yes Se(1) C(2) C(7) 120.0(4) . . . yes C(3) C(2) C(7) 120.6(5) . . . yes C(2) C(3) C(4) 119.8(5) . . . yes C(2) C(3) H(4) 120.2 . . . no C(4) C(3) H(4) 120.0 . . . no C(3) C(4) C(5) 119.8(5) . . . yes C(3) C(4) H(5) 120.6 . . . no C(5) C(4) H(5) 119.6 . . . no C(4) C(5) C(6) 120.8(5) . . . yes C(4) C(5) H(6) 119.9 . . . no C(6) C(5) H(6) 119.3 . . . no C(5) C(6) C(7) 119.0(5) . . . yes C(5) C(6) H(7) 120.7 . . . no C(7) C(6) H(7) 120.3 . . . no Se(2) C(7) C(2) 119.7(4) . . . yes Se(2) C(7) C(6) 120.0(4) . . . yes C(2) C(7) C(6) 119.9(5) . . . yes Se(2) C(8) H(8) 110.6 . . . no Se(2) C(8) H(9) 111.2 . . . no Se(2) C(8) H(10) 111.1 . . . no H(8) C(8) H(9) 107.8 . . . no H(8) C(8) H(10) 107.6 . . . no H(9) C(8) H(10) 108.4 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Se(1) Cl(2) 3.526(1) . 1_554 no Se(2) Cl(2) 3.598(2) . 2_557 no Cl(1) C(3) 3.418(5) . 2_566 no Cl(3) C(2) 3.377(5) . 2_556 no Cl(3) C(7) 3.447(5) . 2_556 no #------------------------------------------------------------------------------ data_bptisecc_[TiCl3(MeSC2SMe)]2(O) #------------------------------------------------------------------------------ _audit_creation_date '19100-04-10' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' Dalton Transactions' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Dr G. Reid' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; This is the CIF file for [{TiCl3(MeS(CH2)2SMe)}2(O)] included in Dalton manuscript number B002792H. ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Sheldrick, G.M. (1985). In: "Crystallographic Computing 3" (Eds G.M. Sheldrick, C. Kruger and R. Goddard) Oxford University Press, pp. 175-189. ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SHELXS86 (Sheldrick, 1985) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 8.963(1) _cell_length_b 10.672(2) _cell_length_c 11.196(1) _cell_angle_alpha 90 _cell_angle_beta 90.36(1) _cell_angle_gamma 90 _cell_volume 1070.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.6 _cell_measurement_theta_max 16.8 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.765 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 569.00 _chemical_formula_analytical ? _chemical_formula_sum 'C8 H20 Cl6 O S4 Ti2 ' _chemical_formula_moiety 'C8 H20 Cl6 O S4 Ti2 ' _chemical_formula_structural [{TiCl3(MeS(CH2)2SMe)}2(O)] _chemical_compound_source ? _exptl_crystal_F_000 572.00 _exptl_absorpt_coefficient_mu 1.877 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.877 _exptl_special_details ; The scan width was (1.37+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_ambient_temperature 150.0 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.48 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 1 0 3 2 0 1 3 -2 _diffrn_reflns_number 2146 _reflns_number_total 2013 _reflns_number_gt 1412 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.03851 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00401 _diffrn_orient_matrix_UB_12 0.09362 _diffrn_orient_matrix_UB_13 -0.00176 _diffrn_orient_matrix_UB_21 0.04329 _diffrn_orient_matrix_UB_22 0.00041 _diffrn_orient_matrix_UB_23 0.08254 _diffrn_orient_matrix_UB_31 0.10276 _diffrn_orient_matrix_UB_32 -0.00383 _diffrn_orient_matrix_UB_33 -0.03409 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 16 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 40 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 12 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ti 0 4 0.248 0.446 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 8 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 2 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ti(1) 0.0417(1) 0.6638(1) -0.00236(9) 0.0257(3) 1.000 . Uani d ? Cl(2) 0.0322(2) 0.6893(2) 0.2014(1) 0.0396(5) 1.000 . Uani d ? Cl(3) 0.1236(2) 0.6750(2) -0.1959(1) 0.0358(4) 1.000 . Uani d ? Cl(5) -0.1817(2) 0.7510(2) -0.0441(2) 0.0400(5) 1.000 . Uani d ? S(1) 0.1633(2) 0.8885(1) 0.0268(1) 0.0294(4) 1.000 . Uani d ? S(2) 0.3221(2) 0.5981(2) 0.0234(1) 0.0320(4) 1.000 . Uani d ? O(1) 0.0000 0.5000 0.0000 0.034(2) 0.500 S Uani d ? C(1) 0.4216(6) 0.7455(6) 0.0222(6) 0.037(2) 1.000 . Uani d ? C(2) 0.3434(7) 0.8494(6) 0.0899(6) 0.037(2) 1.000 . Uani d ? C(3) 0.2175(7) 0.9606(6) -0.1114(6) 0.038(2) 1.000 . Uani d ? C(4) 0.3607(7) 0.5434(7) 0.1735(6) 0.044(2) 1.000 . Uani d ? H(1) 0.3198 0.8236 0.1794 0.062 1.000 . Uiso c ? H(2) 0.4037 0.9358 0.1055 0.062 1.000 . Uiso c ? H(3) 0.5158 0.7163 0.0517 0.062 1.000 . Uiso c ? H(4) 0.4436 0.7705 -0.0600 0.062 1.000 . Uiso c ? H(5) 0.3388 0.6205 0.2302 0.062 1.000 . Uiso c ? H(6) 0.2928 0.4792 0.1887 0.062 1.000 . Uiso c ? H(7) 0.4627 0.5235 0.1891 0.062 1.000 . Uiso c ? H(8) 0.2773 0.8986 -0.1638 0.062 1.000 . Uiso c ? H(9) 0.2792 1.0461 -0.0934 0.062 1.000 . Uiso c ? H(10) 0.1317 1.0150 -0.1287 0.062 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti(1) 0.0231(5) 0.0277(6) 0.0263(6) -0.0016(5) 0.0058(4) -0.0019(5) Cl(2) 0.0397(9) 0.052(1) 0.0267(8) -0.0080(8) 0.0143(6) -0.0027(7) Cl(3) 0.0391(9) 0.045(1) 0.0237(8) 0.0022(7) 0.0036(6) -0.0043(7) Cl(5) 0.0266(8) 0.042(1) 0.051(1) 0.0050(7) 0.0029(7) -0.0022(8) S(1) 0.0277(8) 0.0298(8) 0.0307(9) -0.0047(7) 0.0076(6) -0.0031(6) S(2) 0.0262(8) 0.042(1) 0.0280(8) 0.0058(7) 0.0031(6) -0.0038(7) O(1) 0.033(3) 0.030(3) 0.039(4) -0.003(3) 0.001(3) -0.001(3) C(1) 0.023(3) 0.049(4) 0.039(4) -0.001(3) 0.007(3) 0.009(3) C(2) 0.031(3) 0.046(4) 0.033(4) -0.014(3) -0.005(3) 0.003(3) C(3) 0.042(4) 0.032(4) 0.040(4) 0.001(3) 0.010(3) 0.005(3) C(4) 0.046(4) 0.052(4) 0.034(4) 0.002(4) -0.008(3) 0.002(3) #------------------------------------------------------------------------------ _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00011|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 1412 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_all 0.0601 _refine_ls_wR_factor_ref 0.0601 _refine_ls_goodness_of_fit_all 2.188 _refine_ls_goodness_of_fit_ref 2.188 _refine_ls_shift/su_max 0.0040 _refine_ls_shift/su_mean 0.0010 _refine_diff_density_min -0.72 _refine_diff_density_max 0.52 #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti(1) Cl(2) 2.300(2) . . yes Ti(1) Cl(3) 2.295(2) . . yes Ti(1) Cl(5) 2.255(2) . . yes Ti(1) S(1) 2.653(2) . . yes Ti(1) S(2) 2.624(2) . . yes Ti(1) O(1) 1.788(1) . . yes S(1) C(2) 1.807(6) . . yes S(1) C(3) 1.797(6) . . yes S(2) C(1) 1.808(7) . . yes S(2) C(4) 1.810(7) . . yes C(1) C(2) 1.517(9) . . yes C(1) H(3) 0.96 . . no C(1) H(4) 0.98 . . no C(2) H(1) 1.06 . . no C(2) H(2) 1.08 . . no C(3) H(8) 1.04 . . no C(3) H(9) 1.09 . . no C(3) H(10) 0.98 . . no C(4) H(5) 1.06 . . no C(4) H(6) 0.93 . . no C(4) H(7) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(2) Ti(1) Cl(3) 160.80(7) . . . yes Cl(2) Ti(1) Cl(5) 96.79(7) . . . yes Cl(2) Ti(1) S(1) 77.82(6) . . . yes Cl(2) Ti(1) S(2) 87.94(6) . . . yes Cl(2) Ti(1) O(1) 95.27(6) . . . yes Cl(3) Ti(1) Cl(5) 94.12(7) . . . yes Cl(3) Ti(1) S(1) 86.28(6) . . . yes Cl(3) Ti(1) S(2) 78.80(6) . . . yes Cl(3) Ti(1) O(1) 97.66(6) . . . yes Cl(5) Ti(1) S(1) 90.92(6) . . . yes Cl(5) Ti(1) S(2) 169.18(7) . . . yes Cl(5) Ti(1) O(1) 102.77(6) . . . yes S(1) Ti(1) S(2) 80.54(6) . . . yes S(1) Ti(1) O(1) 165.39(7) . . . yes S(2) Ti(1) O(1) 86.40(5) . . . yes Ti(1) S(1) C(2) 101.8(2) . . . yes Ti(1) S(1) C(3) 113.2(2) . . . yes C(2) S(1) C(3) 101.0(3) . . . yes Ti(1) S(2) C(1) 103.8(2) . . . yes Ti(1) S(2) C(4) 111.5(2) . . . yes C(1) S(2) C(4) 101.3(3) . . . yes Ti(1) O(1) Ti(1) 180.00 . . 3_565 yes S(2) C(1) C(2) 113.8(4) . . . yes S(2) C(1) H(3) 98.5 . . . no S(2) C(1) H(4) 110.3 . . . no C(2) C(1) H(3) 118.4 . . . no C(2) C(1) H(4) 111.5 . . . no H(3) C(1) H(4) 103.3 . . . no S(1) C(2) C(1) 112.8(4) . . . yes S(1) C(2) H(1) 104.2 . . . no S(1) C(2) H(2) 108.1 . . . no C(1) C(2) H(1) 112.2 . . . no C(1) C(2) H(2) 118.1 . . . no H(1) C(2) H(2) 99.9 . . . no S(1) C(3) H(8) 110.9 . . . no S(1) C(3) H(9) 109.9 . . . no S(1) C(3) H(10) 102.0 . . . no H(8) C(3) H(9) 112.1 . . . no H(8) C(3) H(10) 132.3 . . . no H(9) C(3) H(10) 86.4 . . . no S(2) C(4) H(5) 105.7 . . . no S(2) C(4) H(6) 106.6 . . . no S(2) C(4) H(7) 114.8 . . . no H(5) C(4) H(6) 109.8 . . . no H(5) C(4) H(7) 104.1 . . . no H(6) C(4) H(7) 115.4 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ti(1) Ti(1) 3.576(2) . 3_565 no Cl(3) C(3) 3.459(6) . 2_544 no Cl(3) C(2) 3.472(6) . 4_464 no Cl(5) C(3) 3.552(7) . 3_575 no #------------------------------------------------------------------------------ data_bptisc2_[TiCl4{MeS(CH2)2SMe}] #------------------------------------------------------------------------------ _audit_creation_date '19100-04-10' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' Dalton Transactions' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Dr G. Reid' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; This is the CIF file for [TiCl4{MeS(CH2)2SMe}] included in manuscript number B002792H. ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' _publ_section_exptl_refinement ; Solution and refinement were routine. ; _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Sheldrick, G.M. (1985). In: "Crystallographic Computing 3" (Eds G.M. Sheldrick, C. Kruger and R. Goddard) Oxford University Press, pp. 175-189. ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SHELXS86 (Sheldrick, 1985) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 6.922(2) _cell_length_b 13.335(1) _cell_length_c 12.678(1) _cell_angle_alpha 90 _cell_angle_beta 95.17(1) _cell_angle_gamma 90 _cell_volume 1165.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 22.6 _cell_measurement_theta_max 24.9 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.32 _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 311.95 _chemical_formula_analytical ? _chemical_formula_sum 'C4 H10 Cl4 S2 Ti ' _chemical_formula_moiety 'C4 H10 Cl4 S2 Ti ' _chemical_formula_structural [TiCl4{MeS(CH2)2SMe}] _chemical_compound_source ? _exptl_crystal_F_000 624.00 _exptl_absorpt_coefficient_mu 1.951 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.801 _exptl_special_details ; The scan width was (1.42+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_ambient_temperature 150.0 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.99 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 0 -2 -2 -2 -2 -2 1 3 _diffrn_reflns_number 2334 _reflns_number_total 2151 _reflns_number_gt 1755 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.01932 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.09705 _diffrn_orient_matrix_UB_12 -0.05017 _diffrn_orient_matrix_UB_13 0.02076 _diffrn_orient_matrix_UB_21 -0.00912 _diffrn_orient_matrix_UB_22 0.03637 _diffrn_orient_matrix_UB_23 0.06836 _diffrn_orient_matrix_UB_31 -0.10743 _diffrn_orient_matrix_UB_32 0.04224 _diffrn_orient_matrix_UB_33 -0.03420 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 16 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 40 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 16 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ti 0 4 0.248 0.446 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 8 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ti(1) 0.04371(7) 0.61534(3) 0.28386(3) 0.0215(1) 1.000 . Uani d ? Cl(1) 0.1108(1) 0.76949(5) 0.35805(5) 0.0313(2) 1.000 . Uani d ? Cl(2) -0.0096(1) 0.48691(5) 0.16455(6) 0.0356(2) 1.000 . Uani d ? Cl(3) 0.2574(1) 0.53100(5) 0.39301(6) 0.0369(2) 1.000 . Uani d ? Cl(4) -0.2402(1) 0.59899(5) 0.35160(5) 0.0328(2) 1.000 . Uani d ? S(1) 0.33935(9) 0.66722(5) 0.18186(5) 0.0256(2) 1.000 . Uani d ? S(2) -0.13729(9) 0.71013(5) 0.12508(5) 0.0264(2) 1.000 . Uani d ? C(1) 0.4059(4) 0.5672(2) 0.0978(2) 0.0385(9) 1.000 . Uani d ? C(2) 0.2404(4) 0.7578(2) 0.0865(2) 0.0327(8) 1.000 . Uani d ? C(3) 0.0446(4) 0.7286(2) 0.0324(2) 0.0324(8) 1.000 . Uani d ? C(4) -0.1932(4) 0.8369(2) 0.1587(2) 0.0413(9) 1.000 . Uani d ? H(1) 0.2952 0.5418 0.0479 0.053 1.000 . Uiso c ? H(2) 0.4580 0.5170 0.1420 0.053 1.000 . Uiso c ? H(3) 0.5105 0.5902 0.0625 0.053 1.000 . Uiso c ? H(4) 0.3403 0.7703 0.0359 0.053 1.000 . Uiso c ? H(5) 0.2392 0.8222 0.1279 0.053 1.000 . Uiso c ? H(6) -0.0132 0.7777 -0.0192 0.053 1.000 . Uiso c ? H(7) 0.0457 0.6609 -0.0079 0.053 1.000 . Uiso c ? H(8) -0.2599 0.8683 0.1013 0.053 1.000 . Uiso c ? H(9) -0.0801 0.8739 0.1798 0.053 1.000 . Uiso c ? H(10) -0.2647 0.8327 0.2198 0.053 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti(1) 0.0293(3) 0.0184(2) 0.0171(2) -0.0003(2) 0.0046(2) -0.0005(2) Cl(1) 0.0422(4) 0.0236(3) 0.0273(4) -0.0008(3) -0.0010(3) -0.0079(3) Cl(2) 0.0489(4) 0.0256(4) 0.0344(4) -0.0109(3) 0.0145(3) -0.0120(3) Cl(3) 0.0464(4) 0.0302(4) 0.0333(4) 0.0094(3) 0.0004(3) 0.0083(3) Cl(4) 0.0348(4) 0.0355(4) 0.0297(4) -0.0021(3) 0.0124(3) -0.0017(3) S(1) 0.0266(3) 0.0247(4) 0.0257(3) -0.0002(3) 0.0045(3) 0.0007(3) S(2) 0.0286(4) 0.0290(4) 0.0216(3) -0.0007(3) 0.0018(3) 0.0026(3) C(1) 0.037(2) 0.034(2) 0.047(2) 0.003(1) 0.015(1) -0.009(1) C(2) 0.037(2) 0.029(2) 0.033(2) -0.002(1) 0.008(1) 0.011(1) C(3) 0.035(2) 0.042(2) 0.020(1) 0.001(1) 0.004(1) 0.008(1) C(4) 0.049(2) 0.037(2) 0.038(2) 0.016(1) 0.002(1) 0.003(1) #------------------------------------------------------------------------------ _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00004|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack - _refine_ls_number_reflns 1755 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0229 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0294 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.786 _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.29 _refine_diff_density_max 0.28 #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti(1) Cl(1) 2.2907(8) . . yes Ti(1) Cl(2) 2.2926(8) . . yes Ti(1) Cl(3) 2.2358(8) . . yes Ti(1) Cl(4) 2.2253(9) . . yes Ti(1) S(1) 2.6106(9) . . yes Ti(1) S(2) 2.6010(8) . . yes S(1) C(1) 1.793(3) . . yes S(1) C(2) 1.800(3) . . yes S(2) C(3) 1.815(3) . . yes S(2) C(4) 1.794(3) . . yes C(1) H(1) 1.01 . . no C(1) H(2) 0.93 . . no C(1) H(3) 0.94 . . no C(2) C(3) 1.514(4) . . yes C(2) H(4) 1.00 . . no C(2) H(5) 1.01 . . no C(3) H(6) 0.98 . . no C(3) H(7) 1.04 . . no C(4) H(8) 0.93 . . no C(4) H(9) 0.94 . . no C(4) H(10) 0.96 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Ti(1) Cl(2) 162.91(3) . . . yes Cl(1) Ti(1) Cl(3) 95.68(3) . . . yes Cl(1) Ti(1) Cl(4) 94.75(3) . . . yes Cl(1) Ti(1) S(1) 80.02(3) . . . yes Cl(1) Ti(1) S(2) 86.98(3) . . . yes Cl(2) Ti(1) Cl(3) 95.20(3) . . . yes Cl(2) Ti(1) Cl(4) 94.95(3) . . . yes Cl(2) Ti(1) S(1) 87.58(3) . . . yes Cl(2) Ti(1) S(2) 79.33(3) . . . yes Cl(3) Ti(1) Cl(4) 105.66(3) . . . yes Cl(3) Ti(1) S(1) 86.30(3) . . . yes Cl(3) Ti(1) S(2) 165.73(3) . . . yes Cl(4) Ti(1) S(1) 167.45(3) . . . yes Cl(4) Ti(1) S(2) 88.03(3) . . . yes S(1) Ti(1) S(2) 80.34(3) . . . yes Ti(1) S(1) C(1) 110.6(1) . . . yes Ti(1) S(1) C(2) 104.05(9) . . . yes C(1) S(1) C(2) 101.7(1) . . . yes Ti(1) S(2) C(3) 104.67(9) . . . yes Ti(1) S(2) C(4) 111.9(1) . . . yes C(3) S(2) C(4) 101.7(1) . . . yes S(1) C(1) H(1) 113.7 . . . no S(1) C(1) H(2) 106.5 . . . no S(1) C(1) H(3) 107.0 . . . no H(1) C(1) H(2) 111.7 . . . no H(1) C(1) H(3) 112.8 . . . no H(2) C(1) H(3) 104.5 . . . no S(1) C(2) C(3) 113.7(2) . . . yes S(1) C(2) H(4) 107.4 . . . no S(1) C(2) H(5) 104.0 . . . no C(3) C(2) H(4) 113.3 . . . no C(3) C(2) H(5) 114.0 . . . no H(4) C(2) H(5) 103.4 . . . no S(2) C(3) C(2) 112.7(2) . . . yes S(2) C(3) H(6) 104.8 . . . no S(2) C(3) H(7) 103.7 . . . no C(2) C(3) H(6) 115.0 . . . no C(2) C(3) H(7) 113.6 . . . no H(6) C(3) H(7) 105.8 . . . no S(2) C(4) H(8) 110.0 . . . no S(2) C(4) H(9) 111.6 . . . no S(2) C(4) H(10) 106.0 . . . no H(8) C(4) H(9) 109.2 . . . no H(8) C(4) H(10) 113.9 . . . no H(9) C(4) H(10) 106.1 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(3) 3.564(3) . 4_565 no Cl(4) C(4) 3.526(3) . 2_445 no Cl(4) C(2) 3.550(3) . 4_465 no Cl(4) S(1) 3.577(1) . 1_455 no C(1) C(1) 3.411(5) . 3_665 no #------------------------------------------------------------------------------ data_timesc3_[TiCl4{MeS(CH2)3SMe}] #------------------------------------------------------------------------------ _audit_creation_date '19100-04-10' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' Dalton Transactions' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Dr G. Reid' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _publ_contact_letter ; This is the CIF file for [TiCl4{MeS(CH2)3SMe}] included in Dalton manuscript number B002792H. ; _publ_contact_author_phone ' 01703 593609 ' _publ_contact_author_fax ' 01703 593781 ' _publ_contact_author_email ' gr@soton.ac.uk ' _publ_section_references ; Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Sheldrick, G.M. (1985). In: "Crystallographic Computing 3" (Eds G.M. Sheldrick, C. Kruger and R. Goddard) Oxford University Press, pp. 175-189. ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SHELXS86 (Sheldrick, 1985) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 10.071(1) _cell_length_b 10.0710 _cell_length_c 24.542(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2489.1(7) _cell_formula_units_Z 8 _cell_measurement_temperature 150.0 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 7.2 _cell_measurement_theta_max 8.8 #------------------------------------------------------------------------------ _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I -4 2 d ' _symmetry_Int_Tables_number 122 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2+y,1/2+z' ' -x,1/2+y,1/4-z' '1/2-x, +y,3/4-z' ' -x, -y, +z' '1/2-x,1/2-y,1/2+z' ' +x,1/2-y,1/4-z' '1/2+x, -y,3/4-z' ' -y, +x, -z' '1/2-y,1/2+x,1/2-z' ' +y,1/2+x,1/4+z' '1/2+y, +x,3/4+z' ' +y, -x, -z' '1/2+y,1/2-x,1/2-z' ' -y,1/2-x,1/4+z' '1/2-y, -x,3/4+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 325.98 _chemical_formula_analytical ? _chemical_formula_sum 'C5 H12 Cl4 S2 Ti ' _chemical_formula_moiety 'C5 H12 Cl4 S2 Ti ' _chemical_formula_structural [TiCl4{MeS(CH2)3SMe}] _chemical_compound_source ? _exptl_crystal_F_000 1312.00 _exptl_absorpt_coefficient_mu 1.831 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.885 _exptl_special_details ; The scan width was (1.26+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_ambient_temperature 150.0 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.32 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -1 7 1 -2 7 -1 -2 7 _diffrn_reflns_number 683 _reflns_number_total 683 _reflns_number_gt 525 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.070 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.04208 _diffrn_orient_matrix_UB_12 -0.08901 _diffrn_orient_matrix_UB_13 0.00527 _diffrn_orient_matrix_UB_21 0.08991 _diffrn_orient_matrix_UB_22 0.04125 _diffrn_orient_matrix_UB_23 -0.00354 _diffrn_orient_matrix_UB_31 0.00240 _diffrn_orient_matrix_UB_32 0.01529 _diffrn_orient_matrix_UB_33 0.04025 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 40 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 96 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 32 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 16 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ti 0 8 0.248 0.446 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ti(1) 0.5000 0.0000 0.00374(7) 0.0289(5) 0.500 ST Uani d ? Cl(1) 0.5730(2) -0.1572(2) 0.06057(7) 0.0423(6) 1.000 . Uani d ? Cl(2) 0.6998(2) 0.1034(2) -0.00830(8) 0.0460(6) 1.000 . Uani d ? S(1) 0.5866(3) -0.1464(3) -0.07831(8) 0.0418(7) 1.000 . Uani d ? C(1) 0.547(1) -0.3150(9) -0.0630(3) 0.047(3) 1.000 . Uani d ? C(2) 0.470(1) -0.1242(9) -0.1344(3) 0.051(3) 1.000 . Uani d ? C(3) 0.5000 0.0000 -0.1678(4) 0.047(4) 0.500 ST Uani d ? H(1) 0.5627 -0.3690 -0.0939 0.000 1.000 . Uiso c ? H(2) 0.6013 -0.3447 -0.0335 0.000 1.000 . Uiso c ? H(3) 0.4563 -0.3213 -0.0525 0.000 1.000 . Uiso c ? H(4) 0.4745 -0.2000 -0.1574 0.000 1.000 . Uiso c ? H(5) 0.3828 -0.1171 -0.1198 0.000 1.000 . Uiso c ? H(6) 0.4251 0.0181 -0.1904 0.000 0.500 . Uiso d ? H(7) 0.5749 -0.0181 -0.1904 0.000 0.500 . Uiso 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti(1) 0.030(1) 0.039(1) 0.0172(8) 0.005(1) 0.0000 0.0000 Cl(1) 0.053(2) 0.046(1) 0.0284(9) 0.007(1) -0.008(1) 0.007(1) Cl(2) 0.038(1) 0.057(1) 0.044(1) -0.006(1) 0.004(1) 0.000(1) S(1) 0.046(1) 0.050(2) 0.0288(9) 0.003(1) 0.005(1) -0.008(1) C(1) 0.065(7) 0.042(6) 0.034(4) 0.008(5) 0.007(5) -0.006(4) C(2) 0.084(9) 0.044(6) 0.025(4) -0.013(6) 0.002(5) -0.010(4) C(3) 0.07(1) 0.06(1) 0.014(5) -0.02(1) 0.0000 0.0000 #------------------------------------------------------------------------------ _refine_special_details ; Absolute configuration checked in SHELXL97 ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details - _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 525 _refine_ls_number_parameters 56 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_all 0.0412 _refine_ls_wR_factor_ref 0.0412 _refine_ls_goodness_of_fit_all 2.138 _refine_ls_goodness_of_fit_ref 2.138 _refine_ls_shift/su_max 0.0600 _refine_ls_shift/su_mean 0.0080 _refine_diff_density_min -0.41 _refine_diff_density_max 0.74 #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti(1) Cl(1) 2.235(2) . . yes Ti(1) Cl(1) 2.235(2) . 3_655 yes Ti(1) Cl(2) 2.285(2) . . yes Ti(1) Cl(2) 2.285(2) . 3_655 yes Ti(1) S(1) 2.644(2) . . yes Ti(1) S(1) 2.644(2) . 3_655 yes S(1) C(1) 1.78(1) . . yes S(1) C(2) 1.822(9) . . yes C(1) H(1) 0.95 . . no C(1) H(2) 0.96 . . no C(1) H(3) 0.95 . . no C(2) C(3) 1.525(9) . . yes C(2) H(4) 0.95 . . no C(2) H(5) 0.95 . . no C(3) H(6) 0.95 . . no C(3) H(7) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) Ti(1) Cl(1) 102.8(1) . . 3_655 yes Cl(1) Ti(1) Cl(2) 96.53(9) . . . yes Cl(1) Ti(1) Cl(2) 92.73(9) . . 3_655 yes Cl(1) Ti(1) S(1) 88.37(7) . . . yes Cl(1) Ti(1) S(1) 168.3(1) . . 3_655 yes Cl(1) Ti(1) Cl(2) 92.73(9) 3_655 . . yes Cl(1) Ti(1) Cl(2) 96.53(9) 3_655 . 3_655 yes Cl(1) Ti(1) S(1) 168.3(1) 3_655 . . yes Cl(1) Ti(1) S(1) 88.37(7) 3_655 . 3_655 yes Cl(2) Ti(1) Cl(2) 165.1(1) . . 3_655 yes Cl(2) Ti(1) S(1) 82.24(9) . . . yes Cl(2) Ti(1) S(1) 86.44(9) . . 3_655 yes Cl(2) Ti(1) S(1) 86.44(9) 3_655 . . yes Cl(2) Ti(1) S(1) 82.24(9) 3_655 . 3_655 yes S(1) Ti(1) S(1) 80.8(1) . . 3_655 yes Ti(1) S(1) C(1) 107.2(3) . . . yes Ti(1) S(1) C(2) 107.2(3) . . . yes C(1) S(1) C(2) 97.5(4) . . . yes S(1) C(1) H(1) 109.9 . . . no S(1) C(1) H(2) 109.1 . . . no S(1) C(1) H(3) 109.7 . . . no H(1) C(1) H(2) 109.2 . . . no H(1) C(1) H(3) 110.1 . . . no H(2) C(1) H(3) 108.9 . . . no S(1) C(2) C(3) 112.4(6) . . . yes S(1) C(2) H(4) 108.8 . . . no S(1) C(2) H(5) 108.6 . . . no C(3) C(2) H(4) 109.4 . . . no C(3) C(2) H(5) 108.7 . . . no H(4) C(2) H(5) 108.9 . . . no C(2) C(3) C(2) 115.0(8) . . 3_655 yes C(2) C(3) H(6) 108.3 . . . no C(2) C(3) H(7) 108.1 . . . no C(2) C(3) H(6) 108.1 3_655 . . no C(2) C(3) H(7) 108.3 3_655 . . no H(6) C(3) H(7) 109.0 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(1) C(2) 3.573(9) . 6_645 no #------------------------------------------------------------------------------ data_tisec-[TiCl4{MeSe(CH2)3SeMe}] ; This is the CIF file for [TiCl4{MeSe(CH2)3SeMe}] included in Dalton manuscript number B002792H. ; _contact_name 'Dr G. Reid' _contact_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ ; _audit_creation_method SHELXL-97 _chemical_formula_moiety [TiCl4{MeSe(CH2)3SeMe}] _chemical_formula_sum 'C5 H12 Cl4 Se2 Ti' _chemical_formula_weight 419.77 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 '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 ? _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 10.029(6) _cell_length_b 10.029(6) _cell_length_c 25.698(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2585(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 18 _cell_measurement_theta_min 10.41 _cell_measurement_theta_max 17.00 _exptl_crystal_description red _exptl_crystal_colour block _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.31 _exptl_crystal_density_diffrn 2.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 7.074 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.734 _exptl_absorpt_correction_T_max 1.000 _diffrn_ambient_temperature 150.0(1) _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 AFC7S _diffrn_measurement_method omega/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time - _diffrn_standards_decay_% ? _diffrn_reflns_number 1328 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.07 _reflns_number_total 1145 _reflns_number_gt 792 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC AFC7 diffractometer control' _computing_cell_refinement 'MSC AFC7 diffractometer control' _computing_data_reduction 'MSC AFC7 diffractometer control' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material 'Texsan' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] 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 1145 _refine_ls_number_parameters 56 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1609 _refine_ls_wR_factor_gt 0.1421 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 Se1 Se 0.09758(13) 0.60036(14) 0.20064(5) 0.0310(4) Uani 1 d . . . Ti1 Ti 0.0000 0.7500 0.11918(13) 0.0292(8) Uani 1 d S . . Cl1 Cl -0.1954(3) 0.6388(4) 0.13173(13) 0.0399(9) Uani 1 d . . . Cl2 Cl 0.0846(4) 0.5950(4) 0.06540(13) 0.0433(8) Uani 1 d . . . C1 C 0.0000 0.7500 0.2893(8) 0.048(5) Uani 1 d S . . C2 C -0.0323(13) 0.6252(12) 0.2580(5) 0.034(3) Uani 1 d . . . C3 C 0.0415(14) 0.4197(12) 0.1827(6) 0.041(4) 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 Se1 0.0246(6) 0.0313(7) 0.0370(7) 0.0007(6) 0.0011(6) 0.0027(6) Ti1 0.0236(16) 0.0263(17) 0.0378(19) 0.000 0.000 -0.0018(13) Cl1 0.0270(16) 0.046(2) 0.046(2) 0.0020(16) -0.0074(13) -0.0070(15) Cl2 0.051(2) 0.0347(18) 0.0445(18) -0.0036(17) 0.0102(17) 0.0043(16) C1 0.026(10) 0.068(15) 0.049(12) 0.000 0.000 0.006(10) C2 0.034(8) 0.035(8) 0.033(7) 0.004(6) 0.013(6) 0.003(6) C3 0.050(9) 0.013(7) 0.059(9) 0.001(6) -0.013(7) -0.005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se1 C3 1.952(12) . ? Se1 C2 1.982(12) . ? Se1 Ti1 2.755(3) . ? Ti1 Cl2 2.247(4) 2_565 ? Ti1 Cl2 2.247(4) . ? Ti1 Cl1 2.278(3) 2_565 ? Ti1 Cl1 2.278(3) . ? Ti1 Se1 2.755(3) 2_565 ? C1 C2 1.523(15) 2_565 ? C1 C2 1.523(15) . ? 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 C3 Se1 C2 95.9(6) . . ? C3 Se1 Ti1 103.0(4) . . ? C2 Se1 Ti1 105.2(4) . . ? Cl2 Ti1 Cl2 104.1(2) 2_565 . ? Cl2 Ti1 Cl1 94.19(14) 2_565 2_565 ? Cl2 Ti1 Cl1 95.79(13) . 2_565 ? Cl2 Ti1 Cl1 95.79(13) 2_565 . ? Cl2 Ti1 Cl1 94.19(14) . . ? Cl1 Ti1 Cl1 163.7(2) 2_565 . ? Cl2 Ti1 Se1 168.09(14) 2_565 . ? Cl2 Ti1 Se1 87.50(11) . . ? Cl1 Ti1 Se1 81.58(11) 2_565 . ? Cl1 Ti1 Se1 86.07(11) . . ? Cl2 Ti1 Se1 87.50(11) 2_565 2_565 ? Cl2 Ti1 Se1 168.09(14) . 2_565 ? Cl1 Ti1 Se1 86.07(11) 2_565 2_565 ? Cl1 Ti1 Se1 81.58(11) . 2_565 ? Se1 Ti1 Se1 81.12(12) . 2_565 ? C2 C1 C2 116.2(16) 2_565 . ? C1 C2 Se1 110.9(9) . . ? _diffrn_measured_fraction_theta_max 0.489 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.489 _refine_diff_density_max 1.113 _refine_diff_density_min -1.131 _refine_diff_density_rms 0.224