Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global #[HfCl4{MeS(CH2)2SMe}2] #============================================================================== _audit_creation_date '2002-02-18' _audit_creation_method 'by teXsan for Windows v1.06' #============================================================================== # SUBMISSION DETAILS _journal_coden_Cambridge 186 loop_ _publ_author_name 'Reid, Gillian' 'Hart, Richard' 'Levason, W.' 'Patel, Bhavesh' _publ_contact_author_name 'Dr Gillian Reid' _publ_contact_author_address ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ UNITED KINGDOM ; _publ_requested_journal ' J. Chem. Soc., Dalton Trans.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_letter ; This is the CIF file for the structure of [HfCl4{MeS(CH2)2SMe}2]. ; _publ_section_title ; Synthesis, Properties and Crystal Structures of 6-, 7- and 8-Coordinate Zr(IV) and Hf(IV) Complexes Involving Thioether and Selenoether Ligans ; _publ_contact_author_phone ' 023 8059 3609' _publ_contact_author_fax ' 023 8059 3781 ' _publ_contact_author_email ' gr@soton.ac.uk ' _publ_section_references ; Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. 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. ; data__01bp009 #[(ZrCl4)2{MeS(CH2)3SMe}2] _database_code_CSD 164532 _audit_creation_date '2001-05-31' _audit_creation_method 'by teXsan for Windows v1.06' #============================================================================== _computing_data_collection 'Enraf Nonius Kappa CCD diffractometer' _computing_cell_refinement 'Enraf Nonius Kappa CCD diffractometer' _computing_data_reduction 'CrystalClear (Rigaku Corporation, 1999)' _computing_structure_solution ; SHELX97 (Sheldrick, 1997) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 15.8646(2) _cell_length_b 15.4382(2) _cell_length_c 21.6118(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5293.18(12) _cell_formula_units_Z 8 _cell_measurement_temperature 150.0(1) #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_Int_Tables_number 61 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' '1/2-x, -y,1/2+z' ' -x, -y, -z' '1/2-x,1/2+y, +z' ' +x,1/2-y,1/2+z' '1/2+x, +y,1/2-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'rhomboid' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.854 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 738.60 _chemical_formula_analytical ? _chemical_formula_sum 'C10 H24 Cl8 S4 Zr2 ' _chemical_formula_moiety 'C10 H24 Cl8 S4 Zr2 ' _chemical_formula_structural [(ZrCl4)2{MeS(CH2)3SMe}2] _chemical_compound_source CH2Cl2 _exptl_crystal_F_000 2912.00 _exptl_absorpt_coefficient_mu 1.906 _exptl_absorpt_correction_type SORTAV _exptl_special_details ; Min and max transmission factos: 0.786, 0.849 ; #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device 'Mercury CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 30995 _reflns_number_total 5961 _reflns_number_gt 3205 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.06222 _diffrn_reflns_av_sigmaI/netI 0.147 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ 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 80 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 192 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 32 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 64 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Zr 0 16 -2.965 0.560 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Zr(1) 0.25080(3) 0.04569(3) 0.01068(3) 0.0210(2) 1.000 . Uani d ? Zr(2) 0.50011(4) 0.21499(3) -0.25691(3) 0.0239(2) 1.000 . Uani d ? Cl(1) 0.21672(10) 0.17359(8) -0.04590(8) 0.0343(4) 1.000 . Uani d ? Cl(2) 0.11695(10) -0.02200(10) 0.00526(8) 0.0383(5) 1.000 . Uani d ? Cl(3) 0.33102(10) -0.08148(9) 0.03619(7) 0.0343(4) 1.000 . Uani d ? Cl(4) 0.24267(10) 0.10418(10) 0.11189(7) 0.0373(5) 1.000 . Uani d ? Cl(5) 0.53183(10) 0.08832(8) -0.19728(7) 0.0315(4) 1.000 . Uani d ? Cl(6) 0.63305(11) 0.28466(10) -0.25017(8) 0.0444(5) 1.000 . Uani d ? Cl(7) 0.41641(10) 0.34031(8) -0.28190(7) 0.0367(5) 1.000 . Uani d ? Cl(8) 0.51391(11) 0.15397(11) -0.35704(7) 0.0442(5) 1.000 . Uani d ? S(1) 0.41367(9) 0.11037(8) -0.00175(6) 0.0224(4) 1.000 . Uani d ? S(2) 0.46363(9) 0.28547(8) -0.14099(7) 0.0247(4) 1.000 . Uani d ? S(3) 0.33775(10) 0.15078(8) -0.25285(7) 0.0256(4) 1.000 . Uani d ? S(4) 0.29098(10) -0.01422(9) -0.10681(7) 0.0253(4) 1.000 . Uani d ? C(1) 0.4722(4) 0.0821(4) 0.0664(3) 0.030(2) 1.000 . Uani d ? C(2) 0.4172(4) 0.2290(3) 0.0018(3) 0.026(2) 1.000 . Uani d ? C(3) 0.5034(4) 0.2639(3) -0.0161(3) 0.025(2) 1.000 . Uani d ? C(4) 0.5314(4) 0.2411(3) -0.0813(3) 0.027(2) 1.000 . Uani d ? C(5) 0.4999(4) 0.3967(3) -0.1421(3) 0.035(2) 1.000 . Uani d ? C(6) 0.2915(4) 0.1677(4) -0.3286(3) 0.039(2) 1.000 . Uani d ? C(7) 0.3326(4) 0.0336(3) -0.2497(3) 0.027(2) 1.000 . Uani d ? C(8) 0.2460(4) 0.0022(4) -0.2301(3) 0.029(2) 1.000 . Uani d ? C(9) 0.2204(4) 0.0282(3) -0.1656(3) 0.028(2) 1.000 . Uani d ? C(10) 0.2629(4) -0.1273(4) -0.1091(3) 0.040(2) 1.000 . Uani d ? H(1) 0.4402 0.0964 0.1021 0.036 1.000 . Uiso c ? H(2) 0.4835 0.0217 0.0662 0.036 1.000 . Uiso c ? H(3) 0.5239 0.1132 0.0669 0.036 1.000 . Uiso c ? H(4) 0.3763 0.2519 -0.0258 0.031 1.000 . Uiso c ? H(5) 0.4045 0.2470 0.0428 0.031 1.000 . Uiso c ? H(6) 0.5020 0.3252 -0.0126 0.030 1.000 . Uiso c ? H(7) 0.5437 0.2411 0.0121 0.030 1.000 . Uiso c ? H(8) 0.5318 0.1798 -0.0853 0.032 1.000 . Uiso c ? H(9) 0.5868 0.2629 -0.0874 0.032 1.000 . Uiso c ? H(10) 0.5074 0.4166 -0.1009 0.041 1.000 . Uiso c ? H(11) 0.5520 0.4000 -0.1637 0.041 1.000 . Uiso c ? H(12) 0.4593 0.4319 -0.1624 0.041 1.000 . Uiso c ? H(13) 0.2358 0.1891 -0.3241 0.046 1.000 . Uiso c ? H(14) 0.3244 0.2084 -0.3510 0.046 1.000 . Uiso c ? H(15) 0.2902 0.1143 -0.3505 0.046 1.000 . Uiso c ? H(16) 0.3451 0.0109 -0.2895 0.032 1.000 . Uiso c ? H(17) 0.3731 0.0133 -0.2208 0.032 1.000 . Uiso c ? H(18) 0.2058 0.0251 -0.2583 0.035 1.000 . Uiso c ? H(19) 0.2456 -0.0593 -0.2324 0.035 1.000 . Uiso c ? H(20) 0.1652 0.0069 -0.1578 0.034 1.000 . Uiso c ? H(21) 0.2203 0.0896 -0.1630 0.034 1.000 . Uiso c ? H(22) 0.2566 -0.1484 -0.0681 0.047 1.000 . Uiso c ? H(23) 0.2113 -0.1341 -0.1308 0.047 1.000 . Uiso c ? H(24) 0.3060 -0.1590 -0.1296 0.047 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 Zr(1) 0.0170(3) 0.0207(3) 0.0252(3) -0.0002(2) 0.0015(3) 0.0012(2) Zr(2) 0.0204(4) 0.0282(3) 0.0231(3) 0.0034(3) 0.0016(3) 0.0050(3) Cl(1) 0.0309(9) 0.0220(7) 0.0501(10) 0.0036(7) -0.0097(8) 0.0064(7) Cl(2) 0.0250(10) 0.0411(9) 0.0487(10) -0.0107(7) 0.0035(8) -0.0047(7) Cl(3) 0.0355(10) 0.0291(7) 0.0382(9) 0.0068(7) 0.0016(8) 0.0109(7) Cl(4) 0.0340(10) 0.0470(9) 0.0309(9) -0.0060(8) 0.0057(8) -0.0109(7) Cl(5) 0.0338(9) 0.0295(7) 0.0311(9) 0.0071(7) -0.0061(7) 0.0043(7) Cl(6) 0.0274(10) 0.0546(10) 0.0513(11) -0.0080(8) 0.0059(8) 0.0073(9) Cl(7) 0.0403(10) 0.0322(8) 0.0374(9) 0.0074(7) -0.0048(8) 0.0096(7) Cl(8) 0.0416(11) 0.0652(11) 0.0259(9) 0.0125(9) 0.0066(8) -0.0023(8) S(1) 0.0204(8) 0.0241(7) 0.0227(8) -0.0006(6) 0.0005(7) 0.0013(6) S(2) 0.0215(8) 0.0262(7) 0.0264(8) 0.0027(6) 0.0012(7) 0.0033(6) S(3) 0.0250(9) 0.0253(7) 0.0265(8) 0.0017(7) -0.0009(7) 0.0023(6) S(4) 0.0251(9) 0.0227(7) 0.0281(9) 0.0016(7) 0.0015(7) 0.0038(6) C(1) 0.022(3) 0.041(4) 0.028(4) 0.002(3) -0.002(3) 0.004(3) C(2) 0.029(4) 0.022(3) 0.027(3) 0.000(3) 0.005(3) 0.000(2) C(3) 0.023(4) 0.023(3) 0.029(3) -0.004(3) -0.001(3) 0.000(3) C(4) 0.030(4) 0.021(3) 0.029(3) 0.000(3) -0.001(3) 0.007(3) C(5) 0.039(4) 0.027(3) 0.038(4) 0.001(3) -0.002(3) 0.001(3) C(6) 0.038(4) 0.044(4) 0.034(4) 0.004(3) -0.014(3) 0.010(3) C(7) 0.029(4) 0.030(3) 0.022(3) 0.006(3) 0.000(3) -0.003(2) C(8) 0.032(4) 0.035(3) 0.020(3) 0.000(3) -0.003(3) 0.003(3) C(9) 0.013(3) 0.034(3) 0.036(4) -0.007(3) 0.001(3) 0.007(3) C(10) 0.064(5) 0.022(3) 0.033(4) 0.001(3) 0.001(4) -0.005(3) #============================================================================== # REFINEMENT DATA _refine_special_details ; Sinc ethe molecule appeared (to the eye) to have sme symmetry, attempts were made to identify a higher symmetry space group. However, no such space group was found and so refinement proceeded in Pbca. ; _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)]' _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 3205 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_all 0.0490 _refine_ls_wR_factor_ref 0.0490 _refine_ls_goodness_of_fit_all 1.200 _refine_ls_goodness_of_fit_ref 1.200 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.75 _refine_diff_density_max 0.79 #============================================================================== # MOLECULAR GEOMETRY 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 ZR1 CL1 2.385(2) . . ? ZR1 CL2 2.370(2) . . ? ZR1 CL3 2.404(2) . . ? ZR1 CL4 2.370(2) . . ? ZR1 S1 2.783(2) . . ? ZR1 S4 2.777(2) . . ? ZR2 CL5 2.395(2) . . ? ZR2 CL6 2.372(2) . . ? ZR2 CL7 2.408(2) . . ? ZR2 CL8 2.370(2) . . ? ZR2 S2 2.792(2) . . ? ZR2 S3 2.761(2) . . ? S1 C1 1.795(6) . . ? S1 C2 1.834(6) . . ? S2 C4 1.813(6) . . ? S2 C5 1.811(6) . . ? S3 C6 1.813(7) . . ? S3 C7 1.812(5) . . ? S4 C9 1.816(7) . . ? S4 C10 1.802(6) . . ? C1 H1 0.95 . . no C1 H2 0.95 . . no C1 H3 0.95 . . no C2 C3 1.520(8) . . ? C2 H4 0.95 . . no C2 H5 0.95 . . no C3 C4 1.519(8) . . ? C3 H6 0.95 . . no C3 H7 0.95 . . no C4 H8 0.95 . . no C4 H9 0.95 . . no C5 H10 0.95 . . no C5 H11 0.95 . . no C5 H12 0.95 . . no C6 H13 0.95 . . no C6 H14 0.95 . . no C6 H15 0.95 . . no C7 C8 1.516(9) . . ? C7 H16 0.95 . . no C7 H17 0.95 . . no C8 C9 1.507(9) . . ? C8 H18 0.95 . . no C8 H19 0.95 . . no C9 H20 0.95 . . no C9 H21 0.95 . . no C10 H22 0.95 . . no C10 H23 0.95 . . no C10 H24 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 CL1 ZR1 CL2 97.85(6) . . . ? CL1 ZR1 CL3 156.05(7) . . . ? CL1 ZR1 CL4 98.37(6) . . . ? CL1 ZR1 S1 82.18(5) . . . ? CL1 ZR1 S4 81.89(6) . . . ? CL2 ZR1 CL3 97.21(6) . . . ? CL2 ZR1 CL4 99.49(6) . . . ? CL2 ZR1 S1 170.21(6) . . . ? CL2 ZR1 S4 90.78(6) . . . ? CL3 ZR1 CL4 97.37(6) . . . ? CL3 ZR1 S1 79.84(5) . . . ? CL3 ZR1 S4 79.40(5) . . . ? CL4 ZR1 S1 90.17(5) . . . ? CL4 ZR1 S4 169.57(6) . . . ? S1 ZR1 S4 79.52(5) . . . ? CL5 ZR2 CL6 98.65(6) . . . ? CL5 ZR2 CL7 153.18(6) . . . ? CL5 ZR2 CL8 98.47(6) . . . ? CL5 ZR2 S2 83.05(5) . . . ? CL5 ZR2 S3 83.44(5) . . . ? CL6 ZR2 CL7 98.03(6) . . . ? CL6 ZR2 CL8 98.87(7) . . . ? CL6 ZR2 S2 87.28(6) . . . ? CL6 ZR2 S3 171.99(6) . . . ? CL7 ZR2 CL8 99.53(6) . . . ? CL7 ZR2 S2 76.93(5) . . . ? CL7 ZR2 S3 77.36(5) . . . ? CL8 ZR2 S2 173.33(6) . . . ? CL8 ZR2 S3 88.42(6) . . . ? S2 ZR2 S3 85.29(5) . . . ? ZR1 S1 C1 108.3(2) . . . ? ZR1 S1 C2 112.5(2) . . . ? C1 S1 C2 101.1(3) . . . ? ZR2 S2 C4 111.6(2) . . . ? ZR2 S2 C5 106.9(2) . . . ? C4 S2 C5 100.3(3) . . . ? ZR2 S3 C6 107.3(2) . . . ? ZR2 S3 C7 113.7(2) . . . ? C6 S3 C7 99.2(3) . . . ? ZR1 S4 C9 112.2(2) . . . ? ZR1 S4 C10 106.9(2) . . . ? C9 S4 C10 100.2(3) . . . ? S1 C1 H1 109.5 . . . no S1 C1 H2 109.5 . . . no S1 C1 H3 109.5 . . . no H1 C1 H2 109.5 . . . no H1 C1 H3 109.5 . . . no H2 C1 H3 109.5 . . . no S1 C2 C3 111.8(4) . . . ? S1 C2 H4 108.9 . . . no S1 C2 H5 108.9 . . . no C3 C2 H4 108.9 . . . no C3 C2 H5 108.9 . . . no H4 C2 H5 109.5 . . . no C2 C3 C4 114.6(5) . . . ? C2 C3 H6 108.2 . . . no C2 C3 H7 108.2 . . . no C4 C3 H6 108.2 . . . no C4 C3 H7 108.2 . . . no H6 C3 H7 109.5 . . . no S2 C4 C3 113.5(4) . . . ? S2 C4 H8 108.4 . . . no S2 C4 H9 108.4 . . . no C3 C4 H8 108.5 . . . no C3 C4 H9 108.5 . . . no H8 C4 H9 109.5 . . . no S2 C5 H10 109.5 . . . no S2 C5 H11 109.5 . . . no S2 C5 H12 109.5 . . . no H10 C5 H11 109.5 . . . no H10 C5 H12 109.5 . . . no H11 C5 H12 109.5 . . . no S3 C6 H13 109.5 . . . no S3 C6 H14 109.5 . . . no S3 C6 H15 109.5 . . . no H13 C6 H14 109.5 . . . no H13 C6 H15 109.5 . . . no H14 C6 H15 109.5 . . . no S3 C7 C8 111.7(4) . . . ? S3 C7 H16 108.9 . . . no S3 C7 H17 108.9 . . . no C8 C7 H16 108.9 . . . no C8 C7 H17 108.9 . . . no H16 C7 H17 109.5 . . . no C7 C8 C9 114.7(5) . . . ? C7 C8 H18 108.2 . . . no C7 C8 H19 108.2 . . . no C9 C8 H18 108.2 . . . no C9 C8 H19 108.2 . . . no H18 C8 H19 109.5 . . . no S4 C9 C8 112.6(4) . . . ? S4 C9 H20 108.7 . . . no S4 C9 H21 108.7 . . . no C8 C9 H20 108.7 . . . no C8 C9 H21 108.7 . . . no H20 C9 H21 109.5 . . . no S4 C10 H22 109.5 . . . no S4 C10 H23 109.5 . . . no S4 C10 H24 109.5 . . . no H22 C10 H23 109.5 . . . no H22 C10 H24 109.5 . . . no H23 C10 H24 109.5 . . . 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 ? ? ? ? ? ? #------------------------------------------------------------------------------ data__01bp022 #[ZrCl4([9]aneS3)] _database_code_CSD 164533 _audit_creation_date '2001-04-25' _audit_creation_method 'by teXsan for Windows v1.06' #============================================================================== _computing_data_collection 'Enraf Nonius Kappa CCD diffractometer control' _computing_cell_refinement 'Enraf Nonius Kappa CCD diffractometer control' _computing_data_reduction 'CrystalClear (Rigaku Corporation, 1999)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 11.5442(10) _cell_length_b 8.4604(7) _cell_length_c 13.9222(13) _cell_angle_alpha 90 _cell_angle_beta 98.270(4) _cell_angle_gamma 90 _cell_volume 1345.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; Slow diffusion of CH2Cl2 solutions of [ZrCl4(tht)2] and [9]aneS3, yielding very small crystals. ; _exptl_crystal_description 'plate' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 2.040 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 413.37 _chemical_formula_analytical ? _chemical_formula_sum 'C6 H12 Cl4 S3 Zr ' _chemical_formula_moiety 'C6 H12 Cl4 S3 Zr ' _chemical_formula_structural '[ZrCl4([9]aneS3)]' _chemical_compound_source 'CH2Cl2 - see above' _exptl_crystal_F_000 816.00 _exptl_absorpt_coefficient_mu 2.036 _exptl_absorpt_correction_type SORTAV _exptl_special_details ; Max and min transmission factors 0.848, 0.848. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device 'Mercury CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h ? _diffrn_standard_refln_index_k ? _diffrn_standard_refln_index_l ? _diffrn_reflns_number 16315 _reflns_number_total 3973 _reflns_number_gt 725 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.21836 _diffrn_reflns_av_sigmaI/netI 0.341 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 30.04 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ 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 24 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 48 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 12 0.110 0.124 ;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) ; Zr 0 4 -2.965 0.560 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Zr(1) 0.2504(2) 0.0419(3) 0.2327(2) 0.0381(9) 1.000 . Uani d ? Cl(1) 0.0811(6) 0.1744(8) 0.1426(5) 0.062(3) 1.000 . Uani d ? Cl(2) 0.2280(7) -0.2193(7) 0.2943(6) 0.062(3) 1.000 . Uani d ? Cl(3) 0.4382(6) 0.1330(8) 0.1963(6) 0.068(3) 1.000 . Uani d ? Cl(4) 0.2435(7) -0.1029(8) 0.0792(6) 0.073(3) 1.000 . Uani d ? S(1) 0.0944(7) 0.0756(8) 0.3655(6) 0.056(3) 1.000 . Uani d ? S(2) 0.3819(6) 0.0481(9) 0.4100(6) 0.059(3) 1.000 . Uani d ? S(3) 0.2665(7) 0.3540(8) 0.2892(6) 0.052(3) 1.000 . Uani d ? C(1) 0.170(3) -0.006(3) 0.477(2) 0.075(10) 1.000 . Uiso d ? C(2) 0.295(2) 0.050(3) 0.504(2) 0.051(7) 1.000 . Uiso d ? C(3) 0.440(3) 0.249(4) 0.422(2) 0.083(10) 1.000 . Uiso d ? C(4) 0.372(3) 0.376(3) 0.398(2) 0.078(10) 1.000 . Uiso d ? C(5) 0.133(2) 0.395(3) 0.332(2) 0.056(8) 1.000 . Uiso d ? C(6) 0.088(2) 0.285(3) 0.392(2) 0.035(7) 1.000 . Uiso d ? H(1) 0.1275 0.0216 0.5284 0.090 1.000 . Uiso c ? H(2) 0.1710 -0.1182 0.4709 0.090 1.000 . Uiso c ? H(3) 0.3312 -0.0165 0.5548 0.061 1.000 . Uiso c ? H(4) 0.2921 0.1550 0.5273 0.061 1.000 . Uiso c ? H(5) 0.4715 0.2617 0.4889 0.099 1.000 . Uiso c ? H(6) 0.5015 0.2539 0.3839 0.099 1.000 . Uiso c ? H(7) 0.4216 0.4630 0.3888 0.093 1.000 . Uiso c ? H(8) 0.3303 0.3991 0.4507 0.093 1.000 . Uiso c ? H(9) 0.1431 0.4915 0.3673 0.068 1.000 . Uiso c ? H(10) 0.0753 0.4090 0.2767 0.068 1.000 . Uiso c ? H(11) 0.0081 0.3102 0.3921 0.043 1.000 . Uiso c ? H(12) 0.1298 0.2993 0.4556 0.043 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 Zr(1) 0.054(2) 0.0210(13) 0.042(2) -0.001(2) 0.018(2) 0.001(2) Cl(1) 0.063(6) 0.067(5) 0.054(6) 0.019(4) -0.001(5) 0.028(5) Cl(2) 0.098(7) 0.019(4) 0.074(7) 0.002(4) 0.027(5) -0.001(4) Cl(3) 0.067(6) 0.077(5) 0.070(6) 0.005(5) 0.042(5) 0.003(5) Cl(4) 0.116(7) 0.040(5) 0.069(7) -0.005(4) 0.031(6) -0.016(4) S(1) 0.071(6) 0.050(5) 0.051(6) -0.009(4) 0.025(5) 0.003(5) S(2) 0.054(6) 0.062(5) 0.064(6) -0.009(5) 0.019(4) 0.007(5) S(3) 0.081(6) 0.029(4) 0.050(6) -0.018(4) 0.026(5) 0.004(4) #============================================================================== # REFINEMENT DATA _refine_special_details ; Data very weak as a result of the very small crystal size, hence reflections:parameter ratio restricted C atoms to isotropic refinement. Final residuals also rather high, but confirm coordination geometry and connectivities, but care should be taken when drawing conclusions re specific parameters. ; _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)]' _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 725 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0981 _refine_ls_R_factor_gt 0.0980 _refine_ls_wR_factor_all 0.1160 _refine_ls_wR_factor_ref 0.1160 _refine_ls_goodness_of_fit_all 2.322 _refine_ls_goodness_of_fit_ref 2.320 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0002 _refine_diff_density_min -1.20 _refine_diff_density_max 1.38 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; 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 ZR1 CL1 2.438(11) . . ? ZR1 CL2 2.398(10) . . ? ZR1 CL3 2.422(10) . . ? ZR1 CL4 2.454(12) . . ? ZR1 S1 2.775(10) . . ? ZR1 S2 2.706(13) . . ? ZR1 S3 2.754(11) . . ? S1 C1 1.81(5) . . ? S1 C6 1.81(3) . . ? S2 C2 1.77(4) . . ? S2 C3 1.83(4) . . ? S3 C4 1.82(5) . . ? S3 C5 1.77(4) . . ? C1 C2 1.51(5) . . ? C1 H1 0.95 . . no C1 H2 0.95 . . no C2 H3 0.95 . . no C2 H4 0.95 . . no C3 C4 1.35(5) . . ? C3 H5 0.95 . . no C3 H6 0.95 . . no C4 H7 0.95 . . no C4 H8 0.95 . . no C5 C6 1.40(4) . . ? C5 H9 0.95 . . no C5 H10 0.95 . . no C6 H11 0.95 . . no C6 H12 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 CL1 ZR1 CL2 119.2(4) . . . ? CL1 ZR1 CL3 114.9(4) . . . ? CL1 ZR1 CL4 81.8(4) . . . ? CL1 ZR1 S1 75.3(4) . . . ? CL1 ZR1 S2 139.7(4) . . . ? CL1 ZR1 S3 73.8(4) . . . ? CL2 ZR1 CL3 121.0(4) . . . ? CL2 ZR1 CL4 82.0(4) . . . ? CL2 ZR1 S1 75.1(3) . . . ? CL2 ZR1 S2 76.5(4) . . . ? CL2 ZR1 S3 142.0(4) . . . ? CL3 ZR1 CL4 84.0(4) . . . ? CL3 ZR1 S1 142.5(4) . . . ? CL3 ZR1 S2 77.5(4) . . . ? CL3 ZR1 S3 74.3(3) . . . ? CL4 ZR1 S1 133.5(4) . . . ? CL4 ZR1 S2 138.4(4) . . . ? CL4 ZR1 S3 136.0(4) . . . ? S1 ZR1 S2 73.9(4) . . . ? S1 ZR1 S3 74.6(3) . . . ? S2 ZR1 S3 73.4(4) . . . ? ZR1 S1 C1 104.8(14) . . . ? ZR1 S1 C6 106.6(12) . . . ? C1 S1 C6 103.1(19) . . . ? ZR1 S2 C2 111.8(14) . . . ? ZR1 S2 C3 104.7(16) . . . ? C2 S2 C3 99.5(19) . . . ? ZR1 S3 C4 110.4(16) . . . ? ZR1 S3 C5 105.0(13) . . . ? C4 S3 C5 102.1(20) . . . ? S1 C1 C2 114.7(30) . . . ? S1 C1 H1 108.1 . . . no S1 C1 H2 108.1 . . . no C2 C1 H1 108.2 . . . no C2 C1 H2 108.2 . . . no H1 C1 H2 109.5 . . . no S2 C2 C1 116.1(30) . . . ? S2 C2 H3 107.8 . . . no S2 C2 H4 107.8 . . . no C1 C2 H3 107.8 . . . no C1 C2 H4 107.8 . . . no H3 C2 H4 109.5 . . . no S2 C3 C4 121.9(37) . . . ? S2 C3 H5 106.4 . . . no S2 C3 H6 106.3 . . . no C4 C3 H5 106.3 . . . no C4 C3 H6 106.2 . . . no H5 C3 H6 109.5 . . . no S3 C4 C3 115.0(37) . . . ? S3 C4 H7 108.1 . . . no S3 C4 H8 108.0 . . . no C3 C4 H7 108.1 . . . no C3 C4 H8 108.1 . . . no H7 C4 H8 109.4 . . . no S3 C5 C6 119.0(28) . . . ? S3 C5 H9 107.1 . . . no S3 C5 H10 107.0 . . . no C6 C5 H9 107.0 . . . no C6 C5 H10 107.0 . . . no H9 C5 H10 109.5 . . . no S1 C6 C5 120.0(27) . . . ? S1 C6 H11 106.8 . . . no S1 C6 H12 106.8 . . . no C5 C6 H11 106.8 . . . no C5 C6 H12 106.8 . . . no H11 C6 H12 109.5 . . . 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 S1 H10 2.9377 . 2_545 no S2 S2 3.52(2) . 3_656 no #------------------------------------------------------------------------------ data__01bp8mesc2 _database_code_CSD 164534 _audit_creation_date '2001-04-25' _audit_creation_method 'by teXsan for Windows v1.06' #============================================================================== _computing_data_collection 'Enraf Nonius Kappa CCD diffractometer control' _computing_cell_refinement 'Enraf Nonius Kappa CCD diffractometer control' _computing_data_reduction 'CrystalClear (Rigaku Corporation, 1999)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 9.9696(3) _cell_length_b 9.9696(3) _cell_length_c 17.5265(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1742.01(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) #------------------------------------------------------------------------------ _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 41 21 2' _symmetry_Int_Tables_number 92 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y,1/2+z' '1/2-y,1/2+x,1/4+z' '1/2+y,1/2-x,3/4+z' ' +y, +x, -z' ' -y, -x,1/2-z' '1/2-x,1/2+y,1/4-z' '1/2+x,1/2-y,3/4-z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; Slow evaporation from a solution of the complex in CH2Cl2. ; _exptl_crystal_description 'rhomboid' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 477.52 _chemical_formula_analytical ? _chemical_formula_sum 'C8 H20 Cl4 S4 Zr ' _chemical_formula_moiety 'C8 H20 Cl4 S4 Zr ' _chemical_formula_structural [ZrCl4{MeS(CH2)2SMe}2] _chemical_compound_source CH2Cl2 _exptl_crystal_F_000 960.00 _exptl_absorpt_coefficient_mu 1.701 _exptl_absorpt_correction_type SORTAV _exptl_special_details ; Max and min transmission factors 0.849, 0.786. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device 'Mercury CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method \w _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 7359 _reflns_number_total 1111 _reflns_number_gt 867 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.06701 _diffrn_reflns_av_sigmaI/netI 0.095 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ 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 32 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 80 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 16 0.110 0.124 ;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) ; Zr 0 4 -2.965 0.560 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Zr(1) 0.02425(6) 0.0242 0.0000 0.02085(12) 1.000 S Uani d ? Cl(1) -0.1966(2) 0.1394(2) -0.00661(10) 0.0299(4) 1.000 . Uani d ? Cl(2) 0.0703(2) 0.0832(2) 0.13525(9) 0.0300(5) 1.000 . Uani d ? S(1) -0.1386(2) -0.1418(2) 0.09483(9) 0.0321(6) 1.000 . Uani d ? S(2) 0.3039(2) 0.0693(2) -0.00806(10) 0.0340(5) 1.000 . Uani d ? C(1) -0.2379(7) -0.0450(8) 0.1583(4) 0.041(2) 1.000 . Uani d ? C(2) -0.2685(8) -0.2038(7) 0.0348(5) 0.041(2) 1.000 . Uani d ? C(3) 0.3916(8) 0.0250(9) 0.0774(4) 0.052(3) 1.000 . Uani d ? C(4) 0.3249(12) 0.2466(13) -0.0270(6) 0.034(3) 0.667 S Uiso d ? C(5) 0.344(2) 0.256(2) 0.0196(11) 0.025(5) 0.333 S Uiso d ? H(1) -0.2126 -0.0659 0.2095 0.051 1.000 . Uiso c ? H(2) -0.2202 0.0480 0.1494 0.051 1.000 . Uiso c ? H(3) -0.3287 -0.0635 0.1506 0.051 1.000 . Uiso c ? H(4) -0.3259 -0.2653 0.0621 0.049 1.000 . Uiso c ? H(5) -0.3267 -0.1301 0.0183 0.049 1.000 . Uiso c ? H(6) 0.3385 0.0498 0.1202 0.063 1.000 . Uiso c ? H(7) 0.4051 -0.0696 0.0780 0.063 1.000 . Uiso c ? H(8) 0.4745 0.0697 0.0788 0.063 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 Zr(1) 0.0222(3) 0.0222 0.0182(4) 0.0018(4) 0.0007 -0.0007(3) Cl(1) 0.0275(9) 0.0280(9) 0.0342(8) 0.0046(7) -0.0023(8) -0.0011(9) Cl(2) 0.0262(10) 0.0467(12) 0.0173(7) 0.0003(8) 0.0015(7) -0.0023(7) S(1) 0.0303(12) 0.0303(12) 0.0358(9) -0.0011(8) 0.0075(9) 0.0044(9) S(2) 0.0281(9) 0.0326(11) 0.0412(10) -0.0000(8) 0.0087(10) 0.0027(10) C(1) 0.038(5) 0.037(5) 0.047(4) -0.004(4) 0.015(4) 0.013(4) C(2) 0.030(4) 0.032(4) 0.063(5) -0.010(4) 0.016(4) -0.010(4) C(3) 0.031(5) 0.079(6) 0.046(4) 0.006(5) -0.001(4) -0.011(5) #============================================================================== # REFINEMENT DATA _refine_special_details ; Some disorder identified in the dimethylene linkage between the two S atoms of one ligand. Modelled satisfactorilly using partial occupancies giving C(4)-C(4)' as the major (2/3) conformation and C(5)-C(5)' as the minor (1/3) component. Alternative sites for the Me carbons were not identified. Refinement in the enantiomorphic space group did not proceed satisfactorilly, hence confirming the correct choice of space group. ; _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)]' _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 867 _refine_ls_number_parameters 77 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_all 0.0530 _refine_ls_wR_factor_ref 0.0530 _refine_ls_goodness_of_fit_all 1.442 _refine_ls_goodness_of_fit_ref 1.440 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_min -0.53 _refine_diff_density_max 0.63 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; the symmetry operation for equivalents is: +y, +x, -z. ; 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 ZR1 CL1 2.486(2) . . ? ZR1 CL1 2.486(2) . 5 ? ZR1 CL2 2.485(2) . . ? ZR1 CL2 2.485(2) . 5 ? ZR1 S1 2.853(2) . . ? ZR1 S1 2.853(2) . 5 ? ZR1 S2 2.828(2) . . ? ZR1 S2 2.828(2) . 5 ? S1 C1 1.775(9) . . ? S1 C2 1.780(10) . . ? S2 C3 1.790(9) . . ? S2 C4 1.81(2) . . ? S2 C5 1.96(3) . . ? C1 H1 0.96 . . no C1 H2 0.96 . . no C1 H3 0.93 . . no C2 C2 1.52(2) . . ? C2 H4 0.97 . . no C2 H5 0.98 . . no C3 H6 0.95 . . no C3 H7 0.95 . . no C3 H8 0.94 . . no C4 C4 1.45(3) . 5 ? C5 C5 1.42(5) . 5 ? #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag CL1 ZR1 CL1 145.09(10) . . 5 ? CL1 ZR1 CL2 95.68(7) . . . ? CL1 ZR1 CL2 94.58(7) . . 5 ? CL1 ZR1 S1 77.94(7) . . . ? CL1 ZR1 S1 73.83(7) . . 5 ? CL1 ZR1 S2 142.92(7) . . . ? CL1 ZR1 S2 71.81(6) . . 5 ? CL2 ZR1 CL2 145.31(10) . . 5 ? CL2 ZR1 S1 71.75(6) . . . ? CL2 ZR1 S1 142.91(7) . . 5 ? CL2 ZR1 S2 80.08(7) . . . ? CL2 ZR1 S2 71.92(7) . . 5 ? S1 ZR1 S1 71.28(9) . . 5 ? S1 ZR1 S2 133.03(7) . . . ? S1 ZR1 S2 129.31(6) . . 5 ? S2 ZR1 S2 71.89(9) . . . ? ZR1 S1 C1 111.6(3) . . . ? ZR1 S1 C2 105.7(3) . . . ? C1 S1 C2 98.8(4) . . . ? ZR1 S2 C3 113.6(3) . . . ? ZR1 S2 C4 106.2(5) . . . ? ZR1 S2 C5 109.8(7) . . . ? C3 S2 C4 109.8(6) . . . ? C3 S2 C5 85.8(8) . . . ? S1 C1 H1 108.9 . . . no S1 C1 H2 108.7 . . . no S1 C1 H3 110.1 . . . no H1 C1 H2 108.4 . . . no H1 C1 H3 110.5 . . . no H2 C1 H3 110.3 . . . no S1 C2 C2 108.2(6) . . 5 ? S1 C2 H4 110.9 . . . no S1 C2 H5 110.2 . . . no H4 C2 H5 105.8 . . . no S2 C3 H6 108.9 . . . no S2 C3 H7 108.8 . . . no S2 C3 H8 109.5 . . . no H6 C3 H7 109.2 . . . no H6 C3 H8 110.2 . . . no H7 C3 H8 110.2 . . . no S2 C4 C4 110.0(8) . . 5 ? S2 C5 C5 109.9(12) . . 5 ? #----------------------------------------------------------------------------- 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 C1 C2 3.546(13) . 7_455 no C1 C2 3.584(13) . 3_455 no C3 C4 3.52(2) . 3_545 no #------------------------------------------------------------------------------ data__01bp029 _database_code_CSD 179859 _audit_creation_date '2002-02-18' _audit_creation_method 'by teXsan for Windows v1.06' #============================================================================== _computing_data_collection 'Nonius CCD Diffractometer Control' _computing_cell_refinement 'Nonius CCD Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 9.9760(2) _cell_length_b 9.9760(2) _cell_length_c 17.4881(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1740.43(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120.0(1) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 43 21 2 ' _symmetry_Int_Tables_number 96 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y,1/2+z' '1/2-y,1/2+x,3/4+z' '1/2+y,1/2-x,1/4+z' ' +y, +x, -z' ' -y, -x,1/2-z' '1/2-x,1/2+y,3/4-z' '1/2+x,1/2-y,1/4-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'colourless' _exptl_crystal_colour 'rod' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 2.155 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 564.79 _chemical_formula_analytical ? _chemical_formula_sum 'C8 H20 Cl4 Hf S4 ' _chemical_formula_moiety 'C8 H20 Cl4 Hf S4 ' _chemical_formula_structural [HfCl4{MeS(CH2)2SMe}2] _chemical_compound_source ? _exptl_crystal_F_000 1088.00 _exptl_absorpt_coefficient_mu 7.054 _exptl_absorpt_correction_type SORTAV _exptl_special_details ; The scan width was (0.00+0.00tan\q)\% with an \w scan speed of 0\% per minute . Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. SORTAV absorption correction: max and min transmission factors = 0.401, 0.107. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 120.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius CCD rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 5914 _reflns_number_total 1112 _reflns_number_gt 898 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.11969 _diffrn_reflns_av_sigmaI/netI 0.097 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ 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 32 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 80 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 16 0.110 0.124 ;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) ; Hf 0 4 -1.118 6.185 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Hf(1) 0.02421(6) 0.0242 0.0000 0.0203(1) 1.000 S Uani d ? Cl(1) 0.0817(5) 0.0699(4) 0.1350(2) 0.0280(11) 1.000 . Uani d ? Cl(2) -0.1958(4) 0.1379(4) 0.0075(2) 0.0279(11) 1.000 . Uani d ? S(1) 0.3030(4) 0.0674(4) 0.0098(2) 0.0287(12) 1.000 . Uani d ? S(2) -0.1414(4) -0.1384(5) 0.0947(2) 0.0289(13) 1.000 . Uani d ? C(1) 0.394(2) 0.030(2) -0.0765(9) 0.042(6) 1.000 . Uani d ? C(2) 0.329(3) 0.246(2) 0.023(1) 0.079(10) 1.000 . Uani d ? C(3) -0.046(2) -0.233(2) 0.1585(10) 0.044(5) 1.000 . Uiso d ? C(4) -0.202(2) -0.268(2) 0.0348(11) 0.041(6) 1.000 . Uani d ? H(1) 0.4762 -0.0100 -0.0641 0.046 1.000 . Uiso c ? H(2) 0.3414 -0.0302 -0.1068 0.046 1.000 . Uiso c ? H(3) 0.4076 0.1105 -0.1043 0.046 1.000 . Uiso c ? H(4) 0.3141 0.2700 0.0760 0.091 1.000 . Uiso c ? H(5) 0.4233 0.2674 0.0128 0.091 1.000 . Uiso c ? H(6) -0.0711 -0.2091 0.2104 0.065 1.000 . Uiso c ? H(7) -0.0605 -0.3248 0.1515 0.065 1.000 . Uiso c ? H(8) 0.0468 -0.2123 0.1526 0.065 1.000 . Uiso c ? H(9) -0.1296 -0.3245 0.0188 0.045 1.000 . Uiso c ? H(10) -0.2653 -0.3219 0.0621 0.045 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 Hf(1) 0.0272(4) 0.0272 0.0064(5) 0.0022(4) -0.0005 0.0005(3) Cl(1) 0.051(3) 0.028(2) 0.005(2) 0.005(2) 0.001(2) 0.002(2) Cl(2) 0.030(2) 0.032(2) 0.021(2) 0.000(2) 0.002(2) 0.004(2) S(1) 0.031(2) 0.034(2) 0.021(2) 0.003(2) -0.007(2) -0.003(2) S(2) 0.032(3) 0.034(3) 0.020(2) 0.001(2) 0.004(2) 0.002(2) C(1) 0.06(1) 0.058(12) 0.007(8) 0.012(10) -0.014(9) -0.007(9) C(2) 0.12(2) 0.042(13) 0.08(2) -0.04(2) -0.01(2) -0.01(1) C(4) 0.032(11) 0.055(13) 0.036(11) -0.024(9) -0.014(9) 0.021(10) #============================================================================== # REFINEMENT DATA _refine_special_details ; All non-H atoms aniso, except for C3 which goes NPD, hence this was refined isotropically. ; _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)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details checked _refine_ls_abs_structure_Flack -0.0122(0.00121) _refine_ls_number_reflns 898 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_all 0.1090 _refine_ls_wR_factor_ref 0.1090 _refine_ls_goodness_of_fit_all 2.868 _refine_ls_goodness_of_fit_ref 2.870 _refine_ls_shift/su_max 0.0400 _refine_ls_shift/su_mean 0.0060 _refine_diff_density_min 3.97_close_to_Hf _refine_diff_density_max -4.33_close_to_Hf #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; The symmetry operation for equivalents is: +y, +x, -z. ; 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 HF1 CL1 2.472(6) . . ? HF1 CL1 2.472(6) . 5 ? HF1 CL2 2.474(6) . . ? HF1 CL2 2.474(6) . 5 ? HF1 S1 2.820(7) . . ? HF1 S1 2.820(7) . 5 ? HF1 S2 2.846(7) . . ? HF1 S2 2.846(7) . 5 ? S1 C1 1.80(3) . . ? S1 C2 1.81(4) . . ? S2 C3 1.75(3) . . ? S2 C4 1.77(3) . . ? C1 H1 0.94 . . no C1 H2 0.96 . . no C1 H3 0.95 . . no C2 C2 1.42(9) . . ? C2 H4 0.97 . . no C2 H5 0.98 . . no C3 H6 0.97 . . no C3 H7 0.93 . . no C3 H8 0.96 . . no C4 C4 1.53(6) . 5 ? C4 H9 0.96 . . no C4 H10 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 CL1 HF1 CL1 145.7(3) . . 5 ? CL1 HF1 CL2 94.0(2) . . . ? CL1 HF1 CL2 96.2(2) . . 5 ? CL1 HF1 S1 71.6(2) . . . ? CL1 HF1 S1 80.8(2) . . 5 ? CL1 HF1 S2 71.6(2) . . . ? CL1 HF1 S2 142.6(2) . . 5 ? CL2 HF1 CL2 144.7(3) . . 5 ? CL2 HF1 S1 143.3(2) . . . ? CL2 HF1 S1 71.7(2) . . 5 ? CL2 HF1 S2 73.5(2) . . . ? CL2 HF1 S2 78.0(2) . . 5 ? S1 HF1 S1 72.7(3) . . 5 ? S1 HF1 S2 128.6(2) . . . ? S1 HF1 S2 133.3(2) . . 5 ? S2 HF1 S2 71.2(3) . . 5 ? HF1 S1 C1 114.4(11) . . . ? HF1 S1 C2 107.4(15) . . . ? C1 S1 C2 103.7(20) . . . ? HF1 S2 C3 111.4(11) . . . ? HF1 S2 C4 105.7(10) . . . ? C3 S2 C4 99.8(16) . . . ? S1 C1 H1 109.6 . . . no S1 C1 H2 108.8 . . . no S1 C1 H3 109.2 . . . no H1 C1 H2 109.8 . . . no H1 C1 H3 110.4 . . . no H2 C1 H3 109.1 . . . no S1 C2 C2 114.8(23) . . 5 ? S1 C2 H4 110.0 . . . no S1 C2 H5 109.4 . . . no H4 C2 H5 105.4 . . . no S2 C3 H6 108.7 . . . no S2 C3 H7 111.3 . . . no S2 C3 H8 109.8 . . . no H6 C3 H7 109.2 . . . no H6 C3 H8 107.1 . . . no H7 C3 H8 110.6 . . . no S2 C4 C4 107.9(23) . . 5 ? S2 C4 H9 110.0 . . . no S2 C4 H10 110.0 . . . no H9 C4 H10 107.8 . . . 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 C1 C2 3.59(5) . 3_544 no C3 C4 3.57(5) . 8_545 no #------------------------------------------------------------------------------ #============================================================================== # End of CIF #============================================================================== data__01bp034 _database_code_CSD 179860 _audit_creation_date '2001-12-07' _audit_creation_method 'by teXsan for Windows v1.06' #============================================================================== _computing_data_collection 'Nonius CCD Diffractometer Control' _computing_cell_refinement 'Nonius CCD Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 7.4864(2) _cell_length_b 11.5652(4) _cell_length_c 8.1257(2) _cell_angle_alpha 90 _cell_angle_beta 116.501(2) _cell_angle_gamma 90 _cell_volume 629.61(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120.0(1) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21 ' _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 2.829 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 536.34 _chemical_formula_analytical ? _chemical_formula_sum 'C4 H10 Cl4 Hf Se2 ' _chemical_formula_moiety 'C4 H10 Cl4 Hf Se2 ' _chemical_formula_structural '[HfCl4{MeSe(CH2)SeMe}]' _chemical_compound_source ? _exptl_crystal_F_000 484.00 _exptl_absorpt_coefficient_mu 14.847 _exptl_absorpt_correction_type SORTAV _exptl_special_details ; The scan width was (0.00+0.00tan\q)\% with an \w scan speed of 0\% per minute . Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. Max and min transmission factors: 0.391, 0.145 ; #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 120.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD counter' _diffrn_measurement_device 'Nonius CCD' _diffrn_measurement_method - _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 4733 _reflns_number_total 1359 _reflns_number_gt 1281 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.10435 _diffrn_reflns_av_sigmaI/netI 0.067 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ 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 8 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 20 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 8 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Se 0 4 -0.178 2.223 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Hf 0 2 -1.118 6.185 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Hf(1) 0.18266(8) -0.5011 -0.74145(7) 0.0166(2) 1.000 . Uani d ? Se(1) 0.4086(2) -0.6743(1) -0.8131(2) 0.0177(4) 1.000 . Uani d ? Se(2) 0.2562(2) -0.3875(2) -1.0162(2) 0.0190(4) 1.000 . Uani d ? Cl(1) 0.4879(6) -0.4014(4) -0.5572(5) 0.0281(10) 1.000 . Uani d ? Cl(2) -0.0732(5) -0.6049(3) -0.9906(5) 0.0207(9) 1.000 . Uani d ? Cl(3) 0.2016(6) -0.6257(4) -0.5059(5) 0.0279(10) 1.000 . Uani d ? Cl(4) -0.0318(6) -0.3508(3) -0.7422(5) 0.0231(10) 1.000 . Uani d ? C(1) 0.689(3) -0.648(2) -0.649(3) 0.036(5) 1.000 . Uani d ? C(2) 0.398(3) -0.617(2) -1.044(2) 0.031(4) 1.000 . Uani d ? C(3) 0.449(2) -0.496(2) -1.044(2) 0.027(4) 1.000 . Uani d ? C(4) 0.029(2) -0.414(1) -1.246(3) 0.026(4) 1.000 . Uani d ? H(1) 0.7089 -0.6475 -0.5255 0.043 1.000 . Uiso c ? H(2) 0.7672 -0.7079 -0.6651 0.043 1.000 . Uiso c ? H(3) 0.7294 -0.5756 -0.6774 0.043 1.000 . Uiso c ? H(4) 0.4881 -0.6620 -1.0710 0.037 1.000 . Uiso c ? H(5) 0.2659 -0.6285 -1.1381 0.037 1.000 . Uiso c ? H(6) 0.4525 -0.4792 -1.1572 0.033 1.000 . Uiso c ? H(7) 0.5774 -0.4831 -0.9452 0.033 1.000 . Uiso c ? H(8) -0.0855 -0.4258 -1.2263 0.031 1.000 . Uiso c ? H(9) 0.0079 -0.3487 -1.3238 0.031 1.000 . Uiso c ? H(10) 0.0511 -0.4804 -1.3033 0.031 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 Hf(1) 0.0152(3) 0.0152(3) 0.0201(3) -0.0007(3) 0.0087(2) -0.0010(3) Se(1) 0.0185(7) 0.0131(7) 0.0224(7) 0.0030(6) 0.0100(6) 0.0025(6) Se(2) 0.0200(8) 0.0139(7) 0.0266(8) -0.0003(6) 0.0137(6) 0.0011(6) Cl(1) 0.021(2) 0.027(2) 0.031(2) -0.001(2) 0.006(2) -0.011(2) Cl(2) 0.017(2) 0.018(2) 0.026(2) -0.004(2) 0.008(2) 0.000(2) Cl(3) 0.034(2) 0.027(2) 0.025(2) 0.005(2) 0.015(2) 0.003(2) Cl(4) 0.026(2) 0.017(2) 0.026(2) 0.007(2) 0.013(2) -0.001(2) C(1) 0.027(9) 0.040(12) 0.037(9) 0.001(9) 0.010(8) -0.005(9) C(2) 0.036(9) 0.014(8) 0.034(9) 0.011(8) 0.009(7) -0.014(7) C(3) 0.044(9) 0.021(8) 0.018(6) -0.005(11) 0.015(6) -0.000(9) C(4) 0.029(9) 0.012(8) 0.049(10) -0.002(7) 0.029(8) 0.005(7) #============================================================================== # REFINEMENT DATA _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)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details checked _refine_ls_abs_structure_Flack -0.0241(0.00794) _refine_ls_number_reflns 1281 _refine_ls_number_parameters 99 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_all 0.0680 _refine_ls_wR_factor_ref 0.0680 _refine_ls_goodness_of_fit_all 2.282 _refine_ls_goodness_of_fit_ref 2.280 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -2.53 close to Hf _refine_diff_density_max 1.96 close to Hf #============================================================================== # MOLECULAR GEOMETRY 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 HF1 SE1 2.844(2) . . ? HF1 SE2 2.848(2) . . ? HF1 CL1 2.396(6) . . ? HF1 CL2 2.397(5) . . ? HF1 CL3 2.348(6) . . ? HF1 CL4 2.364(6) . . ? SE1 C1 1.95(3) . . ? SE1 C2 1.96(3) . . ? SE2 C3 2.00(3) . . ? SE2 C4 1.91(3) . . ? C1 H1 0.95 . . no C1 H2 0.95 . . no C1 H3 0.95 . . no C2 C3 1.46(4) . . ? C2 H4 0.95 . . no C2 H5 0.95 . . no C3 H6 0.95 . . no C3 H7 0.95 . . no C4 H8 0.95 . . no C4 H9 0.95 . . no C4 H10 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 SE1 HF1 SE2 79.86(7) . . . ? SE1 HF1 CL1 88.8(2) . . . ? SE1 HF1 CL2 78.4(2) . . . ? SE1 HF1 CL3 84.8(2) . . . ? SE1 HF1 CL4 169.2(2) . . . ? SE2 HF1 CL1 78.7(2) . . . ? SE2 HF1 CL2 86.0(2) . . . ? SE2 HF1 CL3 163.6(2) . . . ? SE2 HF1 CL4 91.6(2) . . . ? CL1 HF1 CL2 161.6(2) . . . ? CL1 HF1 CL3 95.3(2) . . . ? CL1 HF1 CL4 96.0(2) . . . ? CL2 HF1 CL3 96.7(2) . . . ? CL2 HF1 CL4 94.6(2) . . . ? CL3 HF1 CL4 104.3(2) . . . ? HF1 SE1 C1 108.0(9) . . . ? HF1 SE1 C2 100.7(7) . . . ? C1 SE1 C2 100.0(12) . . . ? HF1 SE2 C3 101.6(7) . . . ? HF1 SE2 C4 107.1(7) . . . ? C3 SE2 C4 99.3(10) . . . ? SE1 C1 H1 109.5 . . . no SE1 C1 H2 109.5 . . . no SE1 C1 H3 109.5 . . . no H1 C1 H2 109.5 . . . no H1 C1 H3 109.5 . . . no H2 C1 H3 109.5 . . . no SE1 C2 C3 115.2(17) . . . ? SE1 C2 H4 108.0 . . . no SE1 C2 H5 108.0 . . . no C3 C2 H4 108.0 . . . no C3 C2 H5 108.0 . . . no H4 C2 H5 109.5 . . . no SE2 C3 C2 113.6(18) . . . ? SE2 C3 H6 108.4 . . . no SE2 C3 H7 108.4 . . . no C2 C3 H6 108.4 . . . no C2 C3 H7 108.4 . . . no H6 C3 H7 109.5 . . . no SE2 C4 H8 109.5 . . . no SE2 C4 H9 109.5 . . . no SE2 C4 H10 109.5 . . . no H8 C4 H9 109.5 . . . no H8 C4 H10 109.5 . . . no H9 C4 H10 109.5 . . . no #------------------------------------------------------------------------------ #============================================================================== # End of CIF #============================================================================== data__test _database_code_CSD 179861 _audit_creation_date '2001-12-07' _audit_creation_method 'by teXsan for Windows v1.06' #============================================================================== _computing_data_collection 'Nonius CCD Diffractometer Control' _computing_cell_refinement 'Nonius CCD Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 9.2646(3) _cell_length_b 14.5290(5) _cell_length_c 9.3074(4) _cell_angle_alpha 90 _cell_angle_beta 91.9700(11) _cell_angle_gamma 90 _cell_volume 1252.09(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _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 'colourless' _exptl_crystal_colour 'block' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 2.016 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 760.19 _chemical_formula_analytical ? _chemical_formula_sum 'C6 H16 Cl12 S2 Zr2 ' _chemical_formula_moiety '?' _chemical_formula_structural [Me2SCH2Cl]2[Zr2Cl10] _chemical_compound_source ? _exptl_crystal_F_000 736.00 _exptl_absorpt_coefficient_mu 2.269 _exptl_absorpt_correction_type SORTAV _exptl_special_details ; The scan width was (0.00+0.00tan\q)\% with an \w scan speed of 0\% per minute . Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. Max and min transmission factors: 0.475, 0.387. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 100.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_measurement_method - _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 16590 _reflns_number_total 2659 _reflns_number_gt 1349 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.09997 _diffrn_reflns_av_sigmaI/netI 0.185 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 26.34 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ 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 12 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 32 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 24 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Zr 0 4 -2.965 0.560 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 4 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Zr(1) 0.13180(9) 0.05037(7) 0.15922(10) 0.0186(3) 1.000 . Uani d ? Cl(1) 0.0991(3) 0.3154(2) 0.8829(3) 0.0337(8) 1.000 . Uani d ? Cl(2) 0.3038(3) -0.0158(2) 0.3209(3) 0.0332(8) 1.000 . Uani d ? Cl(3) 0.0671(2) -0.1034(2) 0.0349(2) 0.0205(6) 1.000 . Uani d ? Cl(4) -0.0664(2) 0.0213(2) 0.3151(2) 0.0235(7) 1.000 . Uani d ? Cl(5) 0.1467(2) 0.2079(2) 0.2317(3) 0.0267(7) 1.000 . Uani d ? Cl(6) 0.3078(2) 0.0719(2) -0.0262(3) 0.0244(7) 1.000 . Uani d ? S(1) 0.1225(2) 0.2826(2) 0.5671(3) 0.0232(7) 1.000 . Uani d ? C(1) 0.2628(10) 0.2051(7) 0.6264(11) 0.027(3) 1.000 . Uani d ? C(2) -0.0310(9) 0.2124(6) 0.5851(11) 0.025(3) 1.000 . Uani d ? C(3) 0.1133(10) 0.3617(7) 0.7119(10) 0.027(3) 1.000 . Uani d ? H(1) 0.2666 0.2006 0.7291 0.033 1.000 . Uiso c ? H(2) 0.2442 0.1443 0.5885 0.033 1.000 . Uiso c ? H(3) 0.3541 0.2249 0.5951 0.033 1.000 . Uiso c ? H(4) -0.0523 0.2038 0.6849 0.033 1.000 . Uiso c ? H(5) -0.1145 0.2390 0.5381 0.033 1.000 . Uiso c ? H(6) -0.0165 0.1525 0.5443 0.033 1.000 . Uiso c ? H(7) 0.0307 0.4022 0.6951 0.033 1.000 . Uiso c ? H(8) 0.1977 0.4011 0.7134 0.033 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 Zr(1) 0.0229(5) 0.0179(5) 0.0148(5) -0.0004(4) -0.0004(4) -0.0007(5) Cl(1) 0.047(2) 0.034(2) 0.021(2) -0.0047(13) 0.0002(12) 0.0011(13) Cl(2) 0.0322(13) 0.038(2) 0.029(2) 0.0008(12) -0.0073(11) 0.0108(13) Cl(3) 0.0272(11) 0.017(1) 0.0175(13) 0.0012(10) -0.0010(10) 0.0019(11) Cl(4) 0.0294(12) 0.022(1) 0.0189(13) -0.0007(11) 0.0034(10) 0.0015(11) Cl(5) 0.0351(13) 0.021(2) 0.025(1) -0.0054(11) 0.0047(11) -0.0053(12) Cl(6) 0.0270(12) 0.025(2) 0.022(1) -0.0029(11) 0.0024(10) -0.0029(11) S(1) 0.0285(12) 0.022(2) 0.019(1) -0.0008(11) 0.0017(11) 0.0023(12) C(1) 0.031(5) 0.018(6) 0.032(6) -0.008(5) 0.007(5) 0.004(5) C(2) 0.025(5) 0.011(6) 0.040(7) -0.007(4) 0.001(5) -0.006(5) C(3) 0.033(5) 0.022(6) 0.024(6) -0.007(5) -0.008(5) -0.000(5) #============================================================================== # REFINEMENT DATA _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)]' _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 1349 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_all 0.0610 _refine_ls_wR_factor_ref 0.0610 _refine_ls_goodness_of_fit_all 1.174 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.95 _refine_diff_density_max 0.91 #============================================================================== # MOLECULAR GEOMETRY 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 ZR1 CL2 2.358(3) . . ? ZR1 CL3 2.577(3) . . ? ZR1 CL3 2.650(3) . 3 ? ZR1 CL4 2.416(2) . . ? ZR1 CL5 2.389(3) . . ? ZR1 CL6 2.435(3) . . ? CL1 C3 1.737(11) . . ? S1 C1 1.791(11) . . ? S1 C2 1.763(10) . . ? S1 C3 1.775(11) . . ? C1 H1 0.96 . . no C1 H2 0.96 . . no C1 H3 0.95 . . no C2 H4 0.96 . . no C2 H5 0.96 . . no C2 H6 0.96 . . no C3 H7 0.97 . . no C3 H8 0.97 . . 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 CL2 ZR1 CL3 94.30(10) . . . ? CL2 ZR1 CL3 172.77(10) . . 3 ? CL2 ZR1 CL4 93.22(9) . . . ? CL2 ZR1 CL5 100.31(10) . . . ? CL2 ZR1 CL6 92.89(9) . . . ? CL3 ZR1 CL3 78.47(9) . . 3 ? CL3 ZR1 CL4 87.03(9) . . . ? CL3 ZR1 CL5 165.39(9) . . . ? CL3 ZR1 CL6 86.80(8) . . . ? CL4 ZR1 CL5 92.06(9) . . . ? CL4 ZR1 CL6 171.62(9) . . . ? CL5 ZR1 CL6 92.49(9) . . . ? ZR1 CL3 ZR1 101.53(9) . . 3 ? C1 S1 C2 100.7(5) . . . ? C1 S1 C3 103.1(5) . . . ? C2 S1 C3 104.0(5) . . . ? S1 C1 H1 110.6 . . . no S1 C1 H2 110.2 . . . no S1 C1 H3 111.1 . . . no H1 C1 H2 107.6 . . . no H1 C1 H3 108.9 . . . no H2 C1 H3 108.4 . . . no S1 C2 H4 111.0 . . . no S1 C2 H5 111.4 . . . no S1 C2 H6 111.2 . . . no H4 C2 H5 107.7 . . . no H4 C2 H6 107.4 . . . no H5 C2 H6 107.9 . . . no CL1 C3 S1 116.9(6) . . . ? CL1 C3 H7 107.3 . . . no CL1 C3 H8 107.6 . . . no S1 C3 H7 109.1 . . . no S1 C3 H8 109.5 . . . no H7 C3 H8 105.9 . . . no #------------------------------------------------------------------------------ #============================================================================== # End of CIF #============================================================================== data__01bp033 _database_code_CSD 179862 _audit_creation_date '2001-12-07' _audit_creation_method 'by teXsan for Windows v1.06' #============================================================================== _computing_data_collection 'Nonius CCD Diffractometer Control' _computing_cell_refinement 'Nonius CCD Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 6.4219(2) _cell_length_b 25.7274(8) _cell_length_c 8.3971(3) _cell_angle_alpha 90 _cell_angle_beta 106.9505(11) _cell_angle_gamma 90 _cell_volume 1327.09(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120.0(1) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c ' _symmetry_Int_Tables_number 9 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' +x, -y,1/2+z' '1/2+x,1/2+y, +z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.788 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 357.29 _chemical_formula_analytical ? _chemical_formula_sum 'C4 H12 Cl4 S2 Zr ' _chemical_formula_moiety 'C4 H12 Cl4 S2 Zr ' _chemical_formula_structural [ZrCl4(Me2S)2] _chemical_compound_source ? _exptl_crystal_F_000 704.00 _exptl_absorpt_coefficient_mu 1.897 _exptl_absorpt_correction_type SORTAV _exptl_special_details ; The scan width was (0.00+0.00tan\q)\% with an \w scan speed of 0\% per minute . Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. Max. and min. transmission factors: 0.635, 0.514. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 120.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device 'Nonius CCD' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 3815 _reflns_number_total 1376 _reflns_number_gt 1308 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.04824 _diffrn_reflns_av_sigmaI/netI 0.058 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ 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, Table 6.1.1.2) ; H 0 48 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; S 0 8 0.110 0.124 ;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) ; Zr 0 4 -2.965 0.560 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Zr(1) -0.0011 -0.10807(2) -0.4992 0.0117(1) 1.000 . Uani d ? Cl(1) 0.3008(3) -0.07674(5) -0.5828(2) 0.0184(3) 1.000 . Uani d ? Cl(2) -0.1920(3) -0.16155(5) -0.3494(2) 0.0212(4) 1.000 . Uani d ? Cl(3) -0.1210(3) -0.02666(6) -0.4302(2) 0.0234(4) 1.000 . Uani d ? Cl(4) -0.2332(3) -0.12648(7) -0.7716(2) 0.0281(4) 1.000 . Uani d ? S(1) 0.2989(3) -0.11077(5) -0.1886(2) 0.0157(4) 1.000 . Uani d ? S(2) 0.2033(3) -0.20280(5) -0.5137(2) 0.0207(4) 1.000 . Uani d ? C(1) 0.1614(12) -0.0878(3) -0.0435(9) 0.030(2) 1.000 . Uani d ? C(2) 0.4908(11) -0.0589(3) -0.1743(8) 0.023(2) 1.000 . Uani d ? C(3) -0.003(1) -0.2521(3) -0.5725(10) 0.035(2) 1.000 . Uani d ? C(4) 0.289(2) -0.2026(3) -0.6992(11) 0.038(2) 1.000 . Uani d ? H(1) 0.0409 -0.0669 -0.1006 0.036 1.000 . Uiso c ? H(2) 0.2594 -0.0677 0.0407 0.036 1.000 . Uiso c ? H(3) 0.1115 -0.1166 0.0059 0.036 1.000 . Uiso c ? H(4) 0.5136 -0.0537 -0.2799 0.028 1.000 . Uiso c ? H(5) 0.6249 -0.0678 -0.0950 0.028 1.000 . Uiso c ? H(6) 0.4353 -0.0279 -0.1405 0.028 1.000 . Uiso c ? H(7) -0.0344 -0.2589 -0.6884 0.042 1.000 . Uiso c ? H(8) -0.1306 -0.2405 -0.5485 0.042 1.000 . Uiso c ? H(9) 0.0485 -0.2830 -0.5118 0.042 1.000 . Uiso c ? H(10) 0.1649 -0.2035 -0.7942 0.046 1.000 . Uiso c ? H(11) 0.3770 -0.2323 -0.6995 0.046 1.000 . Uiso c ? H(12) 0.3708 -0.1720 -0.7019 0.046 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 Zr(1) 0.0129(3) 0.0133(3) 0.0086(3) -0.0012(2) 0.0025(2) 0.0024(2) Cl(1) 0.0199(7) 0.0239(6) 0.0133(7) -0.0064(6) 0.0078(6) 0.0001(5) Cl(2) 0.0245(8) 0.0213(7) 0.0211(8) -0.0055(6) 0.0118(7) 0.0035(6) Cl(3) 0.0246(8) 0.0169(6) 0.0306(8) 0.0060(6) 0.0110(6) 0.0057(6) Cl(4) 0.0241(9) 0.0429(10) 0.0134(8) -0.0106(8) -0.0008(7) 0.0027(7) S(1) 0.0214(9) 0.0165(8) 0.0088(7) 0.0030(6) 0.0035(7) 0.0002(5) S(2) 0.0298(9) 0.0152(7) 0.0163(8) -0.0017(6) 0.0054(7) -0.0053(6) C(1) 0.028(4) 0.050(4) 0.017(3) 0.004(3) 0.012(3) -0.004(3) C(2) 0.022(3) 0.031(3) 0.015(3) -0.014(3) 0.003(3) -0.007(3) C(3) 0.062(5) 0.016(3) 0.038(4) -0.019(3) 0.032(4) -0.010(3) C(4) 0.060(6) 0.025(3) 0.045(5) -0.011(3) 0.039(5) -0.020(3) #============================================================================== # REFINEMENT DATA _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)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_abs_structure_details checked _refine_ls_abs_structure_Flack -0.0262(0074) _refine_ls_number_reflns 1308 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_all 0.0630 _refine_ls_wR_factor_ref 0.0630 _refine_ls_goodness_of_fit_all 2.306 _refine_ls_goodness_of_fit_ref 2.310 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -1.35 _refine_diff_density_max 0.87 #============================================================================== # MOLECULAR GEOMETRY 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 ZR1 CL1 2.386(2) . . ? ZR1 CL2 2.425(2) . . ? ZR1 CL3 2.361(2) . . ? ZR1 CL4 2.386(3) . . ? ZR1 S1 2.754(3) . . ? ZR1 S2 2.788(2) . . ? S1 C1 1.800(11) . . ? S1 C2 1.796(9) . . ? S2 C3 1.794(11) . . ? S2 C4 1.797(12) . . ? C1 H1 0.95 . . no C1 H2 0.95 . . no C1 H3 0.95 . . no C2 H4 0.95 . . no C2 H5 0.95 . . no C2 H6 0.95 . . no C3 H7 0.95 . . no C3 H8 0.95 . . no C3 H9 0.95 . . no C4 H10 0.95 . . no C4 H11 0.95 . . no C4 H12 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 CL1 ZR1 CL2 157.14(8) . . . ? CL1 ZR1 CL3 97.09(8) . . . ? CL1 ZR1 CL4 96.83(8) . . . ? CL1 ZR1 S1 83.29(8) . . . ? CL1 ZR1 S2 81.32(8) . . . ? CL2 ZR1 CL3 97.23(8) . . . ? CL2 ZR1 CL4 96.65(8) . . . ? CL2 ZR1 S1 79.30(8) . . . ? CL2 ZR1 S2 80.94(7) . . . ? CL3 ZR1 CL4 104.72(10) . . . ? CL3 ZR1 S1 88.75(8) . . . ? CL3 ZR1 S2 167.87(9) . . . ? CL4 ZR1 S1 166.37(9) . . . ? CL4 ZR1 S2 87.41(9) . . . ? S1 ZR1 S2 79.12(7) . . . ? ZR1 S1 C1 106.7(4) . . . ? ZR1 S1 C2 108.7(3) . . . ? C1 S1 C2 100.0(5) . . . ? ZR1 S2 C3 108.2(4) . . . ? ZR1 S2 C4 107.7(4) . . . ? C3 S2 C4 98.7(5) . . . ? S1 C1 H1 109.5 . . . no S1 C1 H2 109.5 . . . no S1 C1 H3 109.5 . . . no H1 C1 H2 109.5 . . . no H1 C1 H3 109.5 . . . no H2 C1 H3 109.5 . . . no S1 C2 H4 109.5 . . . no S1 C2 H5 109.5 . . . no S1 C2 H6 109.5 . . . no H4 C2 H5 109.5 . . . no H4 C2 H6 109.5 . . . no H5 C2 H6 109.5 . . . no S2 C3 H7 109.5 . . . no S2 C3 H8 109.5 . . . no S2 C3 H9 109.5 . . . no H7 C3 H8 109.5 . . . no H7 C3 H9 109.5 . . . no H8 C3 H9 109.5 . . . no S2 C4 H10 109.5 . . . no S2 C4 H11 109.5 . . . no S2 C4 H12 109.5 . . . no H10 C4 H11 109.5 . . . no H10 C4 H12 109.5 . . . no H11 C4 H12 109.5 . . . no #------------------------------------------------------------------------------ #============================================================================== # End of CIF