#Copyright The Royal Society of Chemistry, 1998 data_CIF_for_cmpnd_Zr1S2C28H48 #------------------------------------------------------------------------------ _audit_creation_date 'Fri Feb 13 09:18:08 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 14.847(3) _cell_length_b 13.234(5) _cell_length_c 16.394(3) _cell_angle_alpha 90 _cell_angle_beta 115.96(1) _cell_angle_gamma 90 _cell_volume 2896(1) _cell_formula_units_Z 4 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 39.4 _cell_measurement_theta_max 42.7 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' +x, +y, +z' ' -x, +y,1/2-z' ' -x, +y,1/2-z' ' -x, -y, -z' ' -x, -y, -z' ' +x, -y,1/2+z' ' +x, -y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 540.03 _chemical_formula_analytical ? _chemical_formula_sum 'C28 H48 S2 Zr ' _chemical_formula_moiety 'C28 H48 S2 Zr ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1152.00 _exptl_absorpt_coefficient_mu 0.536 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.981 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% -3.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 2777 _reflns_number_total 2666 _reflns_number_observed 2147 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 1.16 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 24.99 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.00919 _diffrn_orient_matrix_UB_12 -0.07499 _diffrn_orient_matrix_UB_13 -0.00365 _diffrn_orient_matrix_UB_21 -0.07421 _diffrn_orient_matrix_UB_22 0.00925 _diffrn_orient_matrix_UB_23 -0.02577 _diffrn_orient_matrix_UB_31 -0.00445 _diffrn_orient_matrix_UB_32 0.00057 _diffrn_orient_matrix_UB_33 -0.06265 #------------------------------------------------------------------------------ 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 Zr 0 4 -2.967 0.560 'International Tables' C 0 112 0.003 0.002 'International Tables' H 0 192 0.000 0.000 'International Tables' S 0 8 0.125 0.123 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Zr(1) 0.5000 -0.11314(3) 0.2500 0.0428 Uij ? ? S(1) 0.44746(6) 0.01303(7) 0.33418(6) 0.0709 Uij ? ? C(1) 0.3884(2) -0.2313(2) 0.1237(2) 0.0531 Uij ? ? C(2) 0.3476(2) -0.1347(2) 0.0931(2) 0.0538 Uij ? ? C(3) 0.3073(2) -0.0984(2) 0.1512(2) 0.0583 Uij ? ? C(4) 0.3230(2) -0.1734(3) 0.2176(2) 0.0614 Uij ? ? C(5) 0.3704(2) -0.2567(2) 0.1991(2) 0.0604 Uij ? ? C(6) 0.4227(3) -0.2998(2) 0.0694(2) 0.0714 Uij ? ? C(7) 0.3346(3) -0.0917(2) 0.0037(2) 0.0692 Uij ? ? C(8) 0.2438(2) -0.0054(3) 0.1365(2) 0.0839 Uij ? ? C(9) 0.2805(3) -0.1726(3) 0.2863(3) 0.0939 Uij ? ? C(10) 0.3748(3) -0.3612(3) 0.2372(3) 0.0901 Uij ? ? C(11) 0.5423(3) 0.1096(3) 0.3879(3) 0.0906 Uij ? ? C(12) 0.5003(3) 0.2132(3) 0.3723(2) 0.0777 Uij ? ? C(13) 0.5816(3) 0.2938(3) 0.4162(3) 0.1062 Uij ? ? C(14) 0.5445(5) 0.3958(4) 0.3962(5) 0.1661 Uij ? ? H(1) 0.4481 -0.3608 0.1020 0.0862 Uij ? ? H(2) 0.3678 -0.3146 0.0128 0.0862 Uij ? ? H(3) 0.4740 -0.2672 0.0593 0.0862 Uij ? ? H(4) 0.3980 -0.0878 0.0026 0.0836 Uij ? ? H(5) 0.2914 -0.1341 -0.0442 0.0836 Uij ? ? H(6) 0.3063 -0.0260 -0.0038 0.0836 Uij ? ? H(7) 0.2692 0.0340 0.1904 0.1013 Uij ? ? H(8) 0.2452 0.0333 0.0883 0.1013 Uij ? ? H(9) 0.1767 -0.0248 0.1215 0.1013 Uij ? ? H(10) 0.2526 -0.1080 0.2865 0.1131 Uij ? ? H(11) 0.2299 -0.2227 0.2707 0.1131 Uij ? ? H(12) 0.3324 -0.1865 0.3449 0.1131 Uij ? ? H(13) 0.3086 -0.3860 0.2186 0.1086 Uij ? ? H(14) 0.4102 -0.4049 0.2154 0.1086 Uij ? ? H(15) 0.4082 -0.3586 0.3016 0.1086 Uij ? ? H(16) 0.5744 0.0972 0.4513 0.1092 Uij ? ? H(17) 0.5902 0.1053 0.3641 0.1092 Uij ? ? H(18) 0.4668 0.2252 0.3089 0.0939 Uij ? ? H(19) 0.4537 0.2182 0.3975 0.0939 Uij ? ? H(20) 0.6115 0.2845 0.4800 0.1281 Uij ? ? H(21) 0.6310 0.2848 0.3945 0.1281 Uij ? ? H(22) 0.5981 0.4422 0.4251 0.2006 Uij ? ? H(23) 0.5148 0.4068 0.3326 0.2006 Uij ? ? H(24) 0.4955 0.4066 0.4183 0.2006 Uij ? ? 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) 0.0414(2) 0.0477(2) 0.0394(2) 0.0000 0.0177(2) 0.0000 S(1) 0.0563(5) 0.0762(6) 0.0773(6) 0.0003(4) 0.0266(4) -0.0279(4) C(1) 0.057(2) 0.054(2) 0.045(2) -0.008(1) 0.019(1) -0.005(1) C(2) 0.048(2) 0.067(2) 0.041(1) -0.006(1) 0.014(1) -0.004(1) C(3) 0.040(1) 0.076(2) 0.053(2) -0.003(1) 0.014(1) -0.011(1) C(4) 0.051(2) 0.085(2) 0.051(2) -0.021(2) 0.025(1) -0.013(2) C(5) 0.061(2) 0.068(2) 0.049(2) -0.024(2) 0.021(1) -0.003(1) C(6) 0.090(2) 0.063(2) 0.058(2) -0.003(2) 0.029(2) -0.014(2) C(7) 0.074(2) 0.080(2) 0.044(2) -0.002(2) 0.017(2) 0.003(1) C(8) 0.054(2) 0.111(3) 0.076(2) 0.019(2) 0.019(2) -0.014(2) C(9) 0.075(2) 0.145(4) 0.079(2) -0.033(2) 0.049(2) -0.021(2) C(10) 0.104(3) 0.083(2) 0.071(2) -0.036(2) 0.027(2) 0.010(2) C(11) 0.069(2) 0.073(2) 0.107(3) 0.003(2) 0.017(2) -0.031(2) C(12) 0.080(2) 0.077(2) 0.078(2) 0.000(2) 0.037(2) -0.006(2) C(13) 0.114(3) 0.071(3) 0.119(4) -0.010(2) 0.038(3) -0.009(2) C(14) 0.181(6) 0.095(4) 0.166(6) -0.030(4) 0.024(5) 0.008(4) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2147 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0307 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0395 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.647 _refine_ls_shift/esd_max 0.0010 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.29 _refine_diff_density_max 0.35 #------------------------------------------------------------------------------ _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 Zr(1) S(1) 2.4987(8) ? ? yes Zr(1) S(1) 2.4987(8) ? ? yes Zr(1) C(1) 2.545(3) ? ? yes Zr(1) C(1) 2.545(3) ? ? yes Zr(1) C(2) 2.593(3) ? ? yes Zr(1) C(2) 2.593(3) ? ? yes Zr(1) C(3) 2.606(3) ? ? yes Zr(1) C(3) 2.606(3) ? ? yes Zr(1) C(4) 2.569(3) ? ? yes Zr(1) C(4) 2.569(3) ? ? yes Zr(1) C(5) 2.570(3) ? ? yes Zr(1) C(5) 2.570(3) ? ? yes S(1) C(11) 1.818(4) ? ? yes C(1) C(2) 1.410(4) ? ? yes C(1) C(5) 1.416(4) ? ? yes C(1) C(6) 1.506(4) ? ? yes C(2) C(3) 1.412(4) ? ? yes C(2) C(7) 1.505(4) ? ? yes C(3) C(4) 1.414(4) ? ? yes C(3) C(8) 1.505(4) ? ? yes C(4) C(5) 1.410(4) ? ? yes C(4) C(9) 1.514(4) ? ? yes C(5) C(10) 1.507(4) ? ? yes C(11) C(12) 1.481(5) ? ? yes C(12) C(13) 1.534(5) ? ? yes C(13) C(14) 1.441(6) ? ? yes #------------------------------------------------------------------------------ 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 S(1) Zr(1) S(1) 96.14(5) ? ? ? yes S(1) Zr(1) C(1) 127.66(7) ? ? ? yes S(1) Zr(1) C(1) 102.15(7) ? ? ? yes S(1) Zr(1) C(2) 105.88(7) ? ? ? yes S(1) Zr(1) C(2) 82.75(7) ? ? ? yes S(1) Zr(1) C(3) 76.71(7) ? ? ? yes S(1) Zr(1) C(3) 97.47(7) ? ? ? yes S(1) Zr(1) C(4) 77.48(7) ? ? ? yes S(1) Zr(1) C(4) 129.15(8) ? ? ? yes S(1) Zr(1) C(5) 107.62(8) ? ? ? yes S(1) Zr(1) C(5) 133.25(7) ? ? ? yes S(1) Zr(1) C(1) 102.15(7) ? ? ? yes S(1) Zr(1) C(1) 127.66(7) ? ? ? yes S(1) Zr(1) C(2) 82.75(7) ? ? ? yes S(1) Zr(1) C(2) 105.88(7) ? ? ? yes S(1) Zr(1) C(3) 97.47(7) ? ? ? yes S(1) Zr(1) C(3) 76.71(7) ? ? ? yes S(1) Zr(1) C(4) 129.15(8) ? ? ? yes S(1) Zr(1) C(4) 77.48(7) ? ? ? yes S(1) Zr(1) C(5) 133.25(7) ? ? ? yes S(1) Zr(1) C(5) 107.62(8) ? ? ? yes C(1) Zr(1) C(1) 104.1(1) ? ? ? yes C(1) Zr(1) C(2) 31.83(9) ? ? ? yes C(1) Zr(1) C(2) 135.56(10) ? ? ? yes C(1) Zr(1) C(3) 52.67(9) ? ? ? yes C(1) Zr(1) C(3) 134.28(10) ? ? ? yes C(1) Zr(1) C(4) 53.03(9) ? ? ? yes C(1) Zr(1) C(4) 102.7(1) ? ? ? yes C(1) Zr(1) C(5) 32.14(8) ? ? ? yes C(1) Zr(1) C(5) 86.44(9) ? ? ? yes C(1) Zr(1) C(2) 135.56(10) ? ? ? yes C(1) Zr(1) C(2) 31.83(9) ? ? ? yes C(1) Zr(1) C(3) 134.28(10) ? ? ? yes C(1) Zr(1) C(3) 52.67(9) ? ? ? yes C(1) Zr(1) C(4) 102.7(1) ? ? ? yes C(1) Zr(1) C(4) 53.03(9) ? ? ? yes C(1) Zr(1) C(5) 86.44(9) ? ? ? yes C(1) Zr(1) C(5) 32.14(8) ? ? ? yes C(2) Zr(1) C(2) 167.3(1) ? ? ? yes C(2) Zr(1) C(3) 31.51(9) ? ? ? yes C(2) Zr(1) C(3) 150.35(9) ? ? ? yes C(2) Zr(1) C(4) 52.48(9) ? ? ? yes C(2) Zr(1) C(4) 122.73(9) ? ? ? yes C(2) Zr(1) C(5) 52.55(9) ? ? ? yes C(2) Zr(1) C(5) 116.42(9) ? ? ? yes C(2) Zr(1) C(3) 150.35(9) ? ? ? yes C(2) Zr(1) C(3) 31.51(9) ? ? ? yes C(2) Zr(1) C(4) 122.73(9) ? ? ? yes C(2) Zr(1) C(4) 52.48(9) ? ? ? yes C(2) Zr(1) C(5) 116.42(9) ? ? ? yes C(2) Zr(1) C(5) 52.55(9) ? ? ? yes C(3) Zr(1) C(3) 171.4(1) ? ? ? yes C(3) Zr(1) C(4) 31.71(9) ? ? ? yes C(3) Zr(1) C(4) 153.77(9) ? ? ? yes C(3) Zr(1) C(5) 52.48(10) ? ? ? yes C(3) Zr(1) C(5) 136.02(10) ? ? ? yes C(3) Zr(1) C(4) 153.77(9) ? ? ? yes C(3) Zr(1) C(4) 31.71(9) ? ? ? yes C(3) Zr(1) C(5) 136.02(10) ? ? ? yes C(3) Zr(1) C(5) 52.48(10) ? ? ? yes C(4) Zr(1) C(4) 143.8(2) ? ? ? yes C(4) Zr(1) C(5) 31.85(10) ? ? ? yes C(4) Zr(1) C(5) 113.0(1) ? ? ? yes C(4) Zr(1) C(5) 113.0(1) ? ? ? yes C(4) Zr(1) C(5) 31.85(10) ? ? ? yes C(5) Zr(1) C(5) 84.7(1) ? ? ? yes Zr(1) S(1) C(11) 112.0(1) ? ? ? yes Zr(1) C(1) C(2) 76.0(2) ? ? ? yes Zr(1) C(1) C(5) 74.9(2) ? ? ? yes Zr(1) C(1) C(6) 125.6(2) ? ? ? yes C(2) C(1) C(5) 108.0(3) ? ? ? yes C(2) C(1) C(6) 122.7(3) ? ? ? yes C(5) C(1) C(6) 128.0(3) ? ? ? yes Zr(1) C(2) C(1) 72.2(1) ? ? ? yes Zr(1) C(2) C(3) 74.8(2) ? ? ? yes Zr(1) C(2) C(7) 127.5(2) ? ? ? yes C(1) C(2) C(3) 108.2(3) ? ? ? yes C(1) C(2) C(7) 122.7(3) ? ? ? yes C(3) C(2) C(7) 128.1(3) ? ? ? yes Zr(1) C(3) C(2) 73.7(2) ? ? ? yes Zr(1) C(3) C(4) 72.7(2) ? ? ? yes Zr(1) C(3) C(8) 127.0(2) ? ? ? yes C(2) C(3) C(4) 107.7(3) ? ? ? yes C(2) C(3) C(8) 126.2(3) ? ? ? yes C(4) C(3) C(8) 125.3(3) ? ? ? yes Zr(1) C(4) C(3) 75.6(2) ? ? ? yes Zr(1) C(4) C(5) 74.1(2) ? ? ? yes Zr(1) C(4) C(9) 124.5(2) ? ? ? yes C(3) C(4) C(5) 108.2(3) ? ? ? yes C(3) C(4) C(9) 125.9(3) ? ? ? yes C(5) C(4) C(9) 125.1(3) ? ? ? yes Zr(1) C(5) C(1) 73.0(2) ? ? ? yes Zr(1) C(5) C(4) 74.0(2) ? ? ? yes Zr(1) C(5) C(10) 130.8(2) ? ? ? yes C(1) C(5) C(4) 107.8(3) ? ? ? yes C(1) C(5) C(10) 126.1(3) ? ? ? yes C(4) C(5) C(10) 124.3(3) ? ? ? yes S(1) C(11) C(12) 112.9(3) ? ? ? yes C(11) C(12) C(13) 112.2(3) ? ? ? yes C(12) C(13) C(14) 113.6(4) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;