Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_CAmbridge 182 loop_ _publ_author_name 'Cameron,T.' 'Decken, Andreas' 'Fing, Min' 'Passmore, Jack' _publ_contact_author_name 'Jack Passmore' _publ_contact_author_address ; Department of Chemistry University of New Brunswick #45222 Fredericton New Brunswick E3B 6E2 Canada ; _publ_contact_author_email passmore@unb.ca _publ_contact_author_fax '(506) 455-4981' _publ_contact_author_phone '(506) 453-4821' _publ_request_journal 'J. Chem. Soc., Chem. Comm. ' _publ_section_title ;The synthesis and characterization of the heteroaromatic SbF6- salts of the simple trithietanylium PhCSSS+ and the 1,2,4-trithiolanylium dication [PhCSSC(Ph)S]2+ ; #============================================================================== _audit_creation_date '1999-06-21' _audit_creation_method 'by teXsan for Windows v1.0' _audit_update_record ; ? ; #====================================================================== data_pass7 _database_code_CSD 156699 # This part was obtained from Dr. Cameron. #PhCSSC(Ph)S(SbF6)2 (25 C) #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows (MSC, 1997)' _computing_structure_solution ; SHELXS86 (Sheldrick, 1985) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' #------------------------------------------------------------------------------ _cell_length_a 9.359(5) _cell_length_b 15.148(2) _cell_length_c 15.762(2) _cell_angle_alpha 90 _cell_angle_beta 104.56(2) _cell_angle_gamma 90 _cell_volume 2162.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18.8 _cell_measurement_theta_max 19.9 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 2.291 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 745.89 _chemical_formula_analytical ? _chemical_formula_sum 'C14 H10 F12 S3 Sb2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1408.00 _exptl_absorpt_coefficient_mu 2.885 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.883 _exptl_special_details ; The scan width was (1.52+0.35tan\q)\% with an \w scan speed of 16\% per minute (up to 7 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.66 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 1 1 -1 2 0 -1 3 1 _diffrn_reflns_number 6923 _reflns_number_total 6564 _reflns_number_gt 2263 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.06174 _diffrn_reflns_av_sigmaI/netI 0.130 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 30.05 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00991 _diffrn_orient_matrix_UB_12 0.06211 _diffrn_orient_matrix_UB_13 0.02220 _diffrn_orient_matrix_UB_21 -0.01147 _diffrn_orient_matrix_UB_22 0.02212 _diffrn_orient_matrix_UB_23 -0.06113 _diffrn_orient_matrix_UB_31 -0.10935 _diffrn_orient_matrix_UB_32 0.00331 _diffrn_orient_matrix_UB_33 -0.00821 #------------------------------------------------------------------------------ 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 56 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 40 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) ; F 0 48 0.014 0.010 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Sb 0 8 -0.816 1.546 ;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 Sb(1) 0.12149(7) 0.36430(4) 0.12854(4) 0.0568(2) 1.000 . Uani d ? Sb(2) 0.22980(7) 0.39590(4) 0.50209(4) 0.0631(2) 1.000 . Uani d ? S(1) 0.3532(2) 0.1081(1) 0.1746(1) 0.0569(7) 1.000 . Uani d ? S(2) 0.1600(2) 0.0570(1) 0.1886(1) 0.0583(7) 1.000 . Uani d ? S(3) 0.3013(2) 0.1627(1) 0.3425(1) 0.0530(7) 1.000 . Uani d ? F(1) 0.212(1) 0.2866(5) 0.0680(5) 0.159(4) 1.000 . Uani d ? F(2) 0.0395(7) 0.4448(4) 0.1899(4) 0.112(3) 1.000 . Uani d ? F(3) 0.0721(6) 0.2702(4) 0.1901(4) 0.100(2) 1.000 . Uani d ? F(4) 0.1887(9) 0.4593(4) 0.0756(4) 0.135(3) 1.000 . Uani d ? F(5) 0.2989(5) 0.3707(4) 0.2132(4) 0.110(2) 1.000 . Uani d ? F(6) -0.0556(8) 0.3593(4) 0.0450(5) 0.170(3) 1.000 . Uani d ? F(7) 0.355(2) 0.3647(7) 0.450(1) 0.47(1) 1.000 . Uani d ? F(8) 0.092(1) 0.4196(9) 0.551(1) 0.385(9) 1.000 . Uani d ? F(9) 0.346(1) 0.3934(7) 0.6077(5) 0.225(5) 1.000 . Uani d ? F(10) 0.100(2) 0.409(1) 0.4008(6) 0.45(1) 1.000 . Uani d ? F(11) 0.2739(8) 0.5084(4) 0.4750(4) 0.135(3) 1.000 . Uani d ? F(12) 0.190(1) 0.2813(5) 0.5248(7) 0.273(6) 1.000 . Uani d ? C(1) 0.4077(8) 0.1661(5) 0.2693(5) 0.043(2) 1.000 . Uani d ? C(2) 0.5375(9) 0.2172(5) 0.2872(5) 0.051(3) 1.000 . Uani d ? C(3) 0.628(1) 0.2148(6) 0.2281(6) 0.080(4) 1.000 . Uani d ? C(4) 0.759(1) 0.2639(7) 0.2446(7) 0.095(4) 1.000 . Uani d ? C(5) 0.798(1) 0.3126(6) 0.3191(7) 0.081(4) 1.000 . Uani d ? C(6) 0.709(1) 0.3157(6) 0.3773(6) 0.076(3) 1.000 . Uani d ? C(7) 0.5807(9) 0.2668(6) 0.3612(6) 0.068(3) 1.000 . Uani d ? C(8) 0.1591(8) 0.0972(5) 0.2890(5) 0.048(2) 1.000 . Uani d ? C(9) 0.0420(9) 0.0786(5) 0.3279(5) 0.051(3) 1.000 . Uani d ? C(10) 0.0322(9) 0.1195(6) 0.4061(6) 0.075(3) 1.000 . Uani d ? C(11) -0.083(1) 0.1048(7) 0.4398(6) 0.088(4) 1.000 . Uani d ? C(12) -0.190(1) 0.0439(7) 0.4024(8) 0.077(4) 1.000 . Uani d ? C(13) -0.186(1) 0.0018(8) 0.3249(7) 0.093(5) 1.000 . Uani d ? C(14) -0.071(1) 0.0188(7) 0.2888(6) 0.079(4) 1.000 . Uani d ? H(1) 0.6000 0.1804 0.1762 0.093 1.000 . Uiso c ? H(2) 0.8186 0.2622 0.2038 0.118 1.000 . Uiso c ? H(3) 0.8885 0.3438 0.3304 0.093 1.000 . Uiso c ? H(4) 0.7382 0.3521 0.4274 0.093 1.000 . Uiso c ? H(5) 0.5219 0.2670 0.4026 0.083 1.000 . Uiso c ? H(6) 0.1089 0.1577 0.4373 0.091 1.000 . Uiso c ? H(7) -0.0934 0.1365 0.4886 0.107 1.000 . Uiso c ? H(8) -0.2709 0.0338 0.4281 0.092 1.000 . Uiso c ? H(9) -0.2562 -0.0418 0.3031 0.110 1.000 . Uiso c ? H(10) -0.0685 -0.0062 0.2343 0.096 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 Sb(1) 0.0725(4) 0.0485(3) 0.0546(4) -0.0019(3) 0.0254(3) 0.0006(3) Sb(2) 0.0758(5) 0.0666(4) 0.0463(3) -0.0123(4) 0.0142(3) -0.0045(3) S(1) 0.069(2) 0.061(1) 0.047(1) -0.007(1) 0.029(1) -0.009(1) S(2) 0.066(2) 0.062(1) 0.050(1) -0.010(1) 0.021(1) -0.010(1) S(3) 0.055(1) 0.062(1) 0.047(1) -0.004(1) 0.022(1) -0.009(1) F(1) 0.25(1) 0.120(6) 0.142(7) 0.047(6) 0.104(8) -0.020(5) F(2) 0.095(5) 0.114(5) 0.134(5) 0.027(4) 0.041(4) -0.040(4) F(3) 0.094(4) 0.083(4) 0.129(5) -0.009(3) 0.037(4) 0.045(4) F(4) 0.189(8) 0.095(5) 0.137(6) -0.010(5) 0.073(6) 0.035(5) F(5) 0.063(3) 0.097(4) 0.159(6) -0.003(3) 0.008(4) -0.005(5) F(6) 0.187(7) 0.099(5) 0.150(7) -0.004(5) -0.098(6) -0.005(5) F(7) 0.85(3) 0.26(1) 0.53(2) 0.28(2) 0.59(2) 0.11(2) F(8) 0.29(1) 0.51(2) 0.48(2) 0.30(1) 0.33(2) 0.38(2) F(9) 0.215(9) 0.28(1) 0.113(6) -0.117(9) -0.088(6) 0.083(7) F(10) 0.52(3) 0.61(3) 0.111(6) -0.42(3) -0.14(1) 0.10(1) F(11) 0.219(8) 0.083(4) 0.113(6) 0.002(5) 0.059(6) 0.027(4) F(12) 0.52(2) 0.109(7) 0.20(1) -0.16(1) 0.09(1) -0.026(7) C(1) 0.037(5) 0.053(5) 0.041(4) 0.006(4) 0.013(4) 0.002(4) C(2) 0.064(6) 0.045(5) 0.050(5) 0.010(4) 0.025(4) 0.006(4) C(3) 0.075(8) 0.102(7) 0.075(7) -0.021(6) 0.042(6) -0.018(6) C(4) 0.083(8) 0.099(8) 0.124(9) -0.015(7) 0.064(7) -0.002(7) C(5) 0.063(7) 0.085(7) 0.093(8) -0.008(5) 0.016(6) 0.001(6) C(6) 0.092(8) 0.076(7) 0.064(6) -0.025(6) 0.024(6) -0.025(5) C(7) 0.058(6) 0.086(7) 0.067(6) -0.010(5) 0.026(5) -0.008(5) C(8) 0.052(5) 0.046(5) 0.050(5) 0.010(4) 0.019(4) 0.000(4) C(9) 0.051(5) 0.044(5) 0.067(6) 0.002(4) 0.031(5) 0.002(4) C(10) 0.080(6) 0.068(6) 0.089(7) -0.017(5) 0.046(5) -0.015(5) C(11) 0.114(8) 0.081(8) 0.091(7) -0.025(7) 0.067(6) -0.019(6) C(12) 0.062(7) 0.083(7) 0.09(1) -0.005(6) 0.034(7) 0.015(7) C(13) 0.072(9) 0.12(1) 0.107(9) -0.023(7) 0.051(8) -0.011(8) C(14) 0.072(7) 0.094(8) 0.084(7) -0.000(6) 0.046(6) -0.012(6) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.00000024(2) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2263 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_all 0.2080 _refine_ls_wR_factor_ref 0.2020 _refine_ls_goodness_of_fit_all 2.910 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_shift/su_max 0.0006 _refine_ls_shift/su_mean 0.0004 _refine_diff_density_min -1.08 _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 Sb(1) F(1) 1.85(1) . . ? Sb(1) F(2) 1.845(9) . . ? Sb(1) F(3) 1.842(8) . . ? Sb(1) F(4) 1.86(1) . . ? Sb(1) F(5) 1.857(9) . . ? Sb(1) F(6) 1.82(1) . . ? Sb(2) F(7) 1.80(2) . . ? Sb(2) F(8) 1.68(1) . . ? Sb(2) F(9) 1.76(1) . . ? Sb(2) F(10) 1.68(1) . . ? Sb(2) F(11) 1.826(9) . . ? Sb(2) F(12) 1.82(1) . . ? S(1) S(2) 2.036(5) . . ? S(1) C(1) 1.70(1) . . ? S(2) C(8) 1.67(1) . . ? S(3) C(1) 1.70(1) . . ? S(3) C(8) 1.72(1) . . ? C(1) C(2) 1.41(2) . . ? C(2) C(3) 1.39(2) . . ? C(2) C(7) 1.35(2) . . ? C(3) C(4) 1.36(2) . . ? C(3) H(1) 0.97 . . no C(4) C(5) 1.35(2) . . ? C(4) H(2) 0.99 . . no C(5) C(6) 1.37(2) . . ? C(5) H(3) 0.98 . . no C(6) C(7) 1.36(2) . . ? C(6) H(4) 0.95 . . no C(7) H(5) 0.95 . . no C(8) C(9) 1.42(2) . . ? C(9) C(10) 1.39(2) . . ? C(9) C(14) 1.37(2) . . ? C(10) C(11) 1.39(2) . . ? C(10) H(6) 0.98 . . no C(11) C(12) 1.38(2) . . ? C(11) H(7) 0.93 . . no C(12) C(13) 1.36(2) . . ? C(12) H(8) 0.99 . . no C(13) C(14) 1.34(2) . . ? C(13) H(9) 0.96 . . no C(14) H(10) 0.93 . . 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 F(1) Sb(1) F(2) 176.7(6) . . . ? F(1) Sb(1) F(3) 88.0(5) . . . ? F(1) Sb(1) F(4) 90.6(6) . . . ? F(1) Sb(1) F(5) 86.2(6) . . . ? F(1) Sb(1) F(6) 94.0(7) . . . ? F(2) Sb(1) F(3) 93.0(5) . . . ? F(2) Sb(1) F(4) 88.1(5) . . . ? F(2) Sb(1) F(5) 90.6(4) . . . ? F(2) Sb(1) F(6) 89.2(6) . . . ? F(3) Sb(1) F(4) 173.1(5) . . . ? F(3) Sb(1) F(5) 88.2(4) . . . ? F(3) Sb(1) F(6) 91.7(5) . . . ? F(4) Sb(1) F(5) 85.0(5) . . . ? F(4) Sb(1) F(6) 95.1(6) . . . ? F(5) Sb(1) F(6) 179.8(6) . . . ? F(7) Sb(2) F(8) 172(1) . . . ? F(7) Sb(2) F(9) 86(1) . . . ? F(7) Sb(2) F(10) 92(2) . . . ? F(7) Sb(2) F(11) 81.7(7) . . . ? F(7) Sb(2) F(12) 95.4(9) . . . ? F(8) Sb(2) F(9) 86(1) . . . ? F(8) Sb(2) F(10) 96(2) . . . ? F(8) Sb(2) F(11) 98.3(8) . . . ? F(8) Sb(2) F(12) 84.6(9) . . . ? F(9) Sb(2) F(10) 178(1) . . . ? F(9) Sb(2) F(11) 94.7(7) . . . ? F(9) Sb(2) F(12) 85.3(8) . . . ? F(10) Sb(2) F(11) 84.1(9) . . . ? F(10) Sb(2) F(12) 96(1) . . . ? F(11) Sb(2) F(12) 177.1(8) . . . ? S(2) S(1) C(1) 100.4(5) . . . ? S(1) S(2) C(8) 100.5(5) . . . ? C(1) S(3) C(8) 101.6(6) . . . ? S(1) C(1) S(3) 118.4(8) . . . ? S(1) C(1) C(2) 120.8(9) . . . ? S(3) C(1) C(2) 121(1) . . . ? C(1) C(2) C(3) 119(1) . . . ? C(1) C(2) C(7) 122(1) . . . ? C(3) C(2) C(7) 119(1) . . . ? C(2) C(3) C(4) 121(2) . . . ? C(2) C(3) H(1) 120.5 . . . no C(4) C(3) H(1) 118.5 . . . no C(3) C(4) C(5) 119(2) . . . ? C(3) C(4) H(2) 121.2 . . . no C(5) C(4) H(2) 119.8 . . . no C(4) C(5) C(6) 121(2) . . . ? C(4) C(5) H(3) 117.5 . . . no C(6) C(5) H(3) 121.7 . . . no C(5) C(6) C(7) 120(2) . . . ? C(5) C(6) H(4) 117.2 . . . no C(7) C(6) H(4) 123.1 . . . no C(2) C(7) C(6) 121(1) . . . ? C(2) C(7) H(5) 119.5 . . . no C(6) C(7) H(5) 119.5 . . . no S(2) C(8) S(3) 119.0(8) . . . ? S(2) C(8) C(9) 122(1) . . . ? S(3) C(8) C(9) 119(1) . . . ? C(8) C(9) C(10) 121(1) . . . ? C(8) C(9) C(14) 121(1) . . . ? C(10) C(9) C(14) 119(1) . . . ? C(9) C(10) C(11) 121(1) . . . ? C(9) C(10) H(6) 123.2 . . . no C(11) C(10) H(6) 115.5 . . . no C(10) C(11) C(12) 117(2) . . . ? C(10) C(11) H(7) 118.2 . . . no C(12) C(11) H(7) 124.0 . . . no C(11) C(12) C(13) 122(2) . . . ? C(11) C(12) H(8) 113.4 . . . no C(13) C(12) H(8) 124.5 . . . no C(12) C(13) C(14) 120(2) . . . ? C(12) C(13) H(9) 113.8 . . . no C(14) C(13) H(9) 125.6 . . . no C(9) C(14) C(13) 121(2) . . . ? C(9) C(14) H(10) 119.8 . . . no C(13) C(14) H(10) 118.8 . . . 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 Sb(1) F(6) 1.82(1) . . no Sb(1) F(3) 1.842(8) . . no Sb(1) F(2) 1.845(9) . . no Sb(1) F(1) 1.85(1) . . no Sb(1) F(4) 1.86(1) . . no Sb(1) F(5) 1.857(9) . . no Sb(2) F(10) 1.68(1) . . no Sb(2) F(8) 1.68(1) . . no Sb(2) F(9) 1.76(1) . . no Sb(2) F(7) 1.80(2) . . no Sb(2) F(12) 1.82(1) . . no Sb(2) F(11) 1.826(9) . . no S(1) F(11) 2.83(1) . 2_545 no S(1) F(2) 3.24(1) . 2_545 no S(1) F(1) 3.26(1) . . no S(1) F(8) 3.36(1) . 4_554 no S(1) F(10) 3.44(3) . 2_545 no S(2) F(11) 2.92(1) . 2_545 no S(2) F(9) 2.99(1) . 4_454 no S(2) F(5) 3.22(1) . 2_545 no S(2) F(3) 3.32(1) . . no S(2) F(2) 3.41(1) . 2_545 no S(3) F(6) 3.20(1) . 4 no S(3) F(3) 3.22(1) . . no S(3) F(4) 3.35(1) . 2_545 no F(1) H(7) 2.7391 . 4_554 no F(1) H(5) 2.8864 . 4_454 no F(1) C(7) 3.31(2) . 4_454 no F(1) C(6) 3.37(2) . 4_454 no F(1) C(11) 3.54(2) . 4_554 no F(2) H(9) 2.7055 . 2_455 no F(2) F(10) 3.24(2) . . no F(2) C(13) 3.44(2) . 2_455 no F(2) C(1) 3.45(2) . 2 no F(2) C(12) 3.57(2) . 2_455 no F(2) C(8) 3.58(2) . 2 no F(3) H(2) 2.4594 . 1_455 no F(3) C(8) 3.04(1) . . no F(3) C(4) 3.32(2) . 1_455 no F(3) F(9) 3.36(2) . 4_454 no F(3) C(1) 3.41(2) . . no F(4) H(8) 2.4371 . 4_554 no F(4) C(8) 3.08(2) . 2 no F(4) C(9) 3.15(2) . 2 no F(4) C(12) 3.24(2) . 4_554 no F(4) F(6) 3.44(2) . 3_565 no F(4) C(11) 3.44(2) . 4_554 no F(4) C(10) 3.50(2) . 2 no F(5) C(2) 3.21(2) . . no F(5) C(1) 3.28(2) . . no F(5) C(14) 3.33(2) . 2 no F(5) C(7) 3.42(2) . . no F(5) C(8) 3.45(2) . 2 no F(5) C(9) 3.57(2) . 2 no F(6) F(12) 3.12(2) . 4_454 no F(7) H(5) 2.3816 . . no F(7) C(7) 3.14(2) . . no F(7) F(11) 3.47(3) . 3_666 no F(8) H(1) 2.5101 . 4_455 no F(8) F(8) 3.13(3) . 3_566 no F(8) C(3) 3.47(2) . 4_455 no F(8) F(11) 3.51(2) . 3_566 no F(9) H(10) 2.5363 . 4 no F(9) H(2) 2.8720 . 4_455 no F(9) H(1) 2.9761 . 4_455 no F(9) C(14) 3.02(2) . 4 no F(9) C(4) 3.47(2) . 4_455 no F(9) C(9) 3.48(2) . 4 no F(9) C(8) 3.51(2) . 4 no F(9) C(3) 3.54(2) . 4_455 no F(10) H(3) 2.3560 . 1_455 no F(10) C(5) 3.30(3) . 1_455 no F(11) H(4) 2.6104 . 3_666 no F(11) C(6) 3.50(2) . 3_666 no F(12) H(6) 2.3432 . . no F(12) H(1) 2.7943 . 4_455 no F(12) H(2) 2.8456 . 4_455 no F(12) C(10) 3.25(2) . . no F(12) C(3) 3.43(2) . 4_455 no F(12) C(4) 3.44(3) . 4_455 no C(4) H(9) 3.0559 . 2 no C(5) H(9) 2.9030 . 2 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag S(1) S(2) C(8) S(3) . . . . 0.7(8) no S(1) S(2) C(8) C(9) . . . . -179(1) no S(1) C(1) S(3) C(8) . . . . -3.6(9) no S(1) C(1) C(2) C(3) . . . . -2(2) no S(1) C(1) C(2) C(7) . . . . 178(1) no S(2) S(1) C(1) S(3) . . . . 3.9(8) no S(2) S(1) C(1) C(2) . . . . -179(1) no S(2) C(8) S(3) C(1) . . . . 1.4(9) no S(2) C(8) C(9) C(10) . . . . -172(1) no S(2) C(8) C(9) C(14) . . . . 6(2) no S(3) C(1) C(2) C(3) . . . . 176(1) no S(3) C(1) C(2) C(7) . . . . -5(2) no S(3) C(8) C(9) C(10) . . . . 8(2) no S(3) C(8) C(9) C(14) . . . . -174(1) no C(1) S(1) S(2) C(8) . . . . -2.5(6) no C(1) S(3) C(8) C(9) . . . . -179(1) no C(1) C(2) C(3) C(4) . . . . -180(2) no C(1) C(2) C(7) C(6) . . . . 180(1) no C(2) C(1) S(3) C(8) . . . . 179(1) no C(2) C(3) C(4) C(5) . . . . -0(3) no C(2) C(7) C(6) C(5) . . . . -0(3) no C(3) C(2) C(7) C(6) . . . . -1(2) no C(3) C(4) C(5) C(6) . . . . -0(3) no C(4) C(3) C(2) C(7) . . . . 1(3) no C(4) C(5) C(6) C(7) . . . . 1(3) no C(8) C(9) C(10) C(11) . . . . 179(1) no C(8) C(9) C(14) C(13) . . . . -177(2) no C(9) C(10) C(11) C(12) . . . . -1(3) no C(9) C(14) C(13) C(12) . . . . -2(3) no C(10) C(9) C(14) C(13) . . . . 1(3) no C(10) C(11) C(12) C(13) . . . . -0(3) no C(11) C(10) C(9) C(14) . . . . 0(2) no C(11) C(12) C(13) C(14) . . . . 2(3) no #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== #===END data_LT7 _database_code_CSD 156700 #This part was obtained from Dr. Decken. #PhCSSC(Ph)S(SbF6)2 (-60 C) _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H10 F12 S3 Sb2' _chemical_formula_weight 745.90 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.345(4) _cell_length_b 15.005(5) _cell_length_c 15.745(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.71(3) _cell_angle_gamma 90.00 _cell_volume 2135.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 213 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.320 _exptl_crystal_density_method ? _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 2.926 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6683 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.1289 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 30.34 _reflns_number_total 6334 _reflns_number_observed 2260 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6330 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1982 _refine_ls_R_factor_obs 0.0391 _refine_ls_wR_factor_all 0.1487 _refine_ls_wR_factor_obs 0.0946 _refine_ls_goodness_of_fit_all 1.016 _refine_ls_goodness_of_fit_obs 1.148 _refine_ls_restrained_S_all 1.034 _refine_ls_restrained_S_obs 1.148 _refine_ls_shift/esd_max 0.006 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C1 C 0.4062(8) 0.6663(5) -0.2312(5) 0.043(2) Uani 1 d . . S2 S 0.3012(2) 0.66269(14) -0.15761(13) 0.0526(5) Uani 1 d . . C3 C 0.1595(8) 0.5973(5) -0.2118(5) 0.046(2) Uani 1 d . . S4 S 0.1602(3) 0.55694(15) -0.31119(14) 0.0576(5) Uani 1 d . . S5 S 0.3532(3) 0.60810(15) -0.32537(13) 0.0568(5) Uani 1 d . . C6 C 0.5382(9) 0.7167(5) -0.2132(5) 0.051(2) Uani 1 d . . C7 C 0.6275(10) 0.7153(7) -0.2726(6) 0.077(3) Uani 1 d . . H7A H 0.5963(10) 0.6810(7) -0.3256(6) 0.099(11) Uiso 1 d R . C8 C 0.7582(12) 0.7623(8) -0.2548(8) 0.089(3) Uani 1 d . . H8A H 0.8153(12) 0.7645(8) -0.2976(8) 0.099(11) Uiso 1 d R . C9 C 0.7982(11) 0.8123(7) -0.1808(7) 0.078(3) Uani 1 d . . H9A H 0.8923(11) 0.8420(7) -0.1664(7) 0.099(11) Uiso 1 d R . C10 C 0.7109(11) 0.8148(7) -0.1224(6) 0.076(3) Uani 1 d . . H10A H 0.7367(11) 0.8519(7) -0.0711(6) 0.099(11) Uiso 1 d R . C11 C 0.5811(10) 0.7668(6) -0.1387(6) 0.067(2) Uani 1 d . . H11A H 0.5177(10) 0.7692(6) -0.0993(6) 0.099(11) Uiso 1 d R . C12 C 0.0423(9) 0.5786(5) -0.1717(6) 0.051(2) Uani 1 d . . C13 C 0.0316(10) 0.6208(6) -0.0948(6) 0.071(3) Uani 1 d . . H13A H 0.1138(10) 0.6570(6) -0.0651(6) 0.099(11) Uiso 1 d R . C14 C -0.0821(12) 0.6033(7) -0.0589(7) 0.083(3) Uani 1 d . . H14A H -0.0907(12) 0.6352(7) -0.0075(7) 0.099(11) Uiso 1 d R . C15 C -0.1891(11) 0.5443(7) -0.0976(8) 0.081(3) Uani 1 d . . H15A H -0.2701(11) 0.5320(7) -0.0721(8) 0.099(11) Uiso 1 d R . C16 C -0.1848(12) 0.5022(8) -0.1737(8) 0.091(3) Uani 1 d . . H16A H -0.2628(12) 0.4625(8) -0.2021(8) 0.099(11) Uiso 1 d R . C17 C -0.0706(11) 0.5195(7) -0.2108(6) 0.076(3) Uani 1 d . . H17A H -0.0593(11) 0.4862(7) -0.2608(6) 0.099(11) Uiso 1 d R . Sb1 Sb 0.37862(7) 0.36428(4) -0.12847(4) 0.0564(2) Uani 1 d . . F1 F 0.2897(12) 0.2858(5) -0.0681(6) 0.164(4) Uani 1 d . . F2 F 0.1998(6) 0.3704(4) -0.2118(5) 0.115(2) Uani 1 d . . F3 F 0.4272(7) 0.2702(4) -0.1901(4) 0.101(2) Uani 1 d . . F4 F 0.5550(11) 0.3586(5) -0.0467(6) 0.178(4) Uani 1 d . . F5 F 0.3126(10) 0.4600(5) -0.0755(5) 0.137(3) Uani 1 d . . F6 F 0.4584(7) 0.4457(4) -0.1904(5) 0.111(2) Uani 1 d . . Sb2 Sb -0.27019(7) 0.60407(4) -0.49794(4) 0.0627(2) Uani 1 d . . F7 F -0.0737(16) 0.6199(12) -0.5131(15) 0.147(7) Uani 0.50 d P . F8 F -0.3425(31) 0.6345(24) -0.6121(11) 0.199(13) Uani 0.50 d P . F9 F -0.4460(12) 0.6074(10) -0.4799(10) 0.103(4) Uani 0.50 d P . F10 F -0.1861(22) 0.5824(12) -0.3829(8) 0.114(6) Uani 0.50 d P . F11 F -0.3136(20) 0.7176(7) -0.4764(8) 0.289(8) Uani 1 d . . F12 F -0.2285(10) 0.4917(4) -0.5245(5) 0.139(3) Uani 1 d . . F7A F -0.1295(20) 0.6291(13) -0.4077(13) 0.145(8) Uani 0.50 d P . F8A F -0.2149(38) 0.6522(15) -0.5813(16) 0.189(11) Uani 0.50 d P . F9A F -0.4429(20) 0.5625(10) -0.5860(11) 0.131(6) Uani 0.50 d P . F10A F -0.3665(18) 0.5443(11) -0.4168(10) 0.117(5) Uani 0.50 d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.042(4) 0.047(4) 0.044(4) 0.002(3) 0.016(3) 0.008(3) S2 0.0554(12) 0.0605(12) 0.0471(11) -0.0079(9) 0.0225(10) -0.0037(10) C3 0.049(4) 0.045(4) 0.048(4) 0.003(3) 0.019(3) 0.008(3) S4 0.0658(14) 0.0594(13) 0.0512(11) -0.0106(10) 0.0215(10) -0.0098(10) S5 0.0685(14) 0.0608(13) 0.0481(11) -0.0085(10) 0.0276(10) -0.0068(11) C6 0.058(5) 0.050(5) 0.048(4) 0.004(4) 0.022(4) 0.009(4) C7 0.067(6) 0.098(8) 0.077(6) -0.017(6) 0.039(5) -0.018(6) C8 0.075(7) 0.100(8) 0.109(9) 0.002(7) 0.054(7) -0.016(6) C9 0.059(6) 0.081(7) 0.092(8) 0.004(6) 0.018(6) -0.008(5) C10 0.088(7) 0.078(7) 0.062(6) -0.018(5) 0.019(5) -0.017(6) C11 0.066(6) 0.076(6) 0.065(6) -0.008(5) 0.027(5) -0.013(5) C12 0.047(5) 0.047(4) 0.067(5) 0.003(4) 0.028(4) 0.006(4) C13 0.070(6) 0.071(6) 0.085(7) -0.013(5) 0.042(5) -0.013(5) C14 0.092(8) 0.087(7) 0.089(7) -0.016(6) 0.057(6) -0.016(6) C15 0.066(7) 0.085(7) 0.103(8) 0.016(6) 0.039(6) -0.003(6) C16 0.068(7) 0.116(9) 0.102(8) -0.016(7) 0.046(7) -0.019(6) C17 0.069(6) 0.092(7) 0.079(7) -0.017(6) 0.039(6) -0.009(6) Sb1 0.0719(4) 0.0476(3) 0.0548(3) -0.0007(3) 0.0253(3) 0.0019(3) F1 0.262(11) 0.115(6) 0.149(7) 0.030(5) 0.116(8) -0.038(6) F2 0.058(4) 0.098(5) 0.175(7) 0.007(5) 0.003(4) 0.003(3) F3 0.095(4) 0.085(4) 0.127(5) -0.047(4) 0.033(4) 0.010(3) F4 0.196(9) 0.098(5) 0.159(8) -0.001(5) -0.105(7) 0.009(5) F5 0.196(8) 0.092(5) 0.137(6) -0.029(5) 0.071(6) 0.023(5) F6 0.096(5) 0.109(5) 0.134(6) 0.037(4) 0.043(4) -0.026(4) Sb2 0.0762(4) 0.0650(4) 0.0466(3) 0.0048(3) 0.0148(3) 0.0121(3) F7 0.069(9) 0.179(16) 0.217(20) 0.058(15) 0.083(11) -0.003(10) F8 0.201(24) 0.340(39) 0.049(8) 0.062(15) 0.017(12) 0.092(25) F9 0.049(7) 0.124(11) 0.144(12) 0.001(10) 0.040(7) 0.000(7) F10 0.171(18) 0.131(14) 0.031(5) 0.011(7) 0.010(8) 0.061(12) F11 0.544(24) 0.118(8) 0.207(11) 0.028(7) 0.101(13) 0.178(12) F12 0.225(9) 0.079(5) 0.124(6) -0.027(4) 0.065(6) 0.003(5) F7A 0.107(12) 0.156(17) 0.122(15) 0.005(12) -0.061(11) -0.056(11) F8A 0.284(33) 0.156(17) 0.155(21) 0.080(15) 0.110(22) -0.060(22) F9A 0.158(15) 0.106(11) 0.097(11) 0.010(9) -0.028(10) -0.002(10) F10A 0.113(12) 0.149(13) 0.104(10) -0.021(10) 0.059(9) -0.031(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.412(11) . ? C1 S5 1.683(7) . ? C1 S2 1.699(7) . ? S2 C3 1.694(8) . ? C3 C12 1.424(10) . ? C3 S4 1.680(8) . ? S4 S5 2.024(3) . ? C6 C11 1.366(11) . ? C6 C7 1.403(10) . ? C7 C8 1.377(13) . ? C8 C9 1.356(14) . ? C9 C10 1.376(13) . ? C10 C11 1.378(12) . ? C12 C13 1.392(11) . ? C12 C17 1.397(12) . ? C13 C14 1.351(12) . ? C14 C15 1.359(14) . ? C15 C16 1.363(14) . ? C16 C17 1.365(12) . ? Sb1 F4 1.818(7) . ? Sb1 F6 1.835(5) . ? Sb1 F3 1.835(5) . ? Sb1 F1 1.839(7) . ? Sb1 F5 1.844(6) . ? Sb1 F2 1.846(6) . ? Sb2 F8A 1.690(15) . ? Sb2 F7A 1.715(14) . ? Sb2 F9 1.738(10) . ? Sb2 F11 1.803(8) . ? Sb2 F12 1.803(7) . ? Sb2 F8 1.81(2) . ? Sb2 F10 1.812(12) . ? Sb2 F7 1.925(11) . ? Sb2 F9A 1.944(14) . ? Sb2 F10A 1.958(13) . ? F7 F8A 1.55(3) . ? F8 F8A 1.20(3) . ? F8 F9A 1.55(3) . ? F9 F10A 1.44(2) . ? F10 F7A 1.01(2) . ? F10 F10A 1.73(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 S5 120.0(5) . . ? C6 C1 S2 120.4(6) . . ? S5 C1 S2 119.5(4) . . ? C3 S2 C1 100.8(4) . . ? C12 C3 S4 121.8(6) . . ? C12 C3 S2 118.8(6) . . ? S4 C3 S2 119.4(4) . . ? C3 S4 S5 100.4(3) . . ? C1 S5 S4 99.8(3) . . ? C11 C6 C7 119.1(8) . . ? C11 C6 C1 121.2(7) . . ? C7 C6 C1 119.7(8) . . ? C8 C7 C6 120.3(9) . . ? C9 C8 C7 119.7(9) . . ? C8 C9 C10 120.5(10) . . ? C9 C10 C11 120.4(9) . . ? C6 C11 C10 120.0(8) . . ? C13 C12 C17 117.4(8) . . ? C13 C12 C3 121.9(8) . . ? C17 C12 C3 120.7(8) . . ? C14 C13 C12 120.9(9) . . ? C13 C14 C15 120.4(10) . . ? C14 C15 C16 120.9(10) . . ? C15 C16 C17 119.2(10) . . ? C16 C17 C12 121.1(9) . . ? F4 Sb1 F6 89.4(4) . . ? F4 Sb1 F3 92.1(4) . . ? F6 Sb1 F3 92.4(3) . . ? F4 Sb1 F1 93.0(5) . . ? F6 Sb1 F1 177.1(4) . . ? F3 Sb1 F1 89.2(4) . . ? F4 Sb1 F5 93.6(4) . . ? F6 Sb1 F5 87.1(3) . . ? F3 Sb1 F5 174.2(3) . . ? F1 Sb1 F5 91.1(4) . . ? F4 Sb1 F2 179.7(4) . . ? F6 Sb1 F2 90.3(3) . . ? F3 Sb1 F2 87.9(3) . . ? F1 Sb1 F2 87.3(4) . . ? F5 Sb1 F2 86.4(4) . . ? F8A Sb2 F7A 103.2(13) . . ? F8A Sb2 F9 127.1(13) . . ? F7A Sb2 F9 114.6(10) . . ? F8A Sb2 F11 82.5(10) . . ? F7A Sb2 F11 78.4(9) . . ? F9 Sb2 F11 71.0(7) . . ? F8A Sb2 F12 95.3(9) . . ? F7A Sb2 F12 103.4(8) . . ? F9 Sb2 F12 109.5(6) . . ? F11 Sb2 F12 177.5(4) . . ? F8A Sb2 F8 39.8(10) . . ? F7A Sb2 F8 141.4(13) . . ? F9 Sb2 F8 91.4(10) . . ? F11 Sb2 F8 84.4(11) . . ? F12 Sb2 F8 93.1(11) . . ? F8A Sb2 F10 135.5(13) . . ? F7A Sb2 F10 33.3(7) . . ? F9 Sb2 F10 91.7(8) . . ? F11 Sb2 F10 92.5(6) . . ? F12 Sb2 F10 90.0(6) . . ? F8 Sb2 F10 174.6(14) . . ? F8A Sb2 F7 50.4(11) . . ? F7A Sb2 F7 61.4(10) . . ? F9 Sb2 F7 171.0(7) . . ? F11 Sb2 F7 100.0(8) . . ? F12 Sb2 F7 79.5(6) . . ? F8 Sb2 F7 88.5(10) . . ? F10 Sb2 F7 87.8(9) . . ? F8A Sb2 F9A 86.8(11) . . ? F7A Sb2 F9A 169.9(9) . . ? F9 Sb2 F9A 58.5(7) . . ? F11 Sb2 F9A 104.6(7) . . ? F12 Sb2 F9A 73.9(5) . . ? F8 Sb2 F9A 48.7(10) . . ? F10 Sb2 F9A 136.6(9) . . ? F7 Sb2 F9A 126.6(9) . . ? F8A Sb2 F10A 170.0(12) . . ? F7A Sb2 F10A 86.7(8) . . ? F9 Sb2 F10A 45.3(6) . . ? F11 Sb2 F10A 98.5(7) . . ? F12 Sb2 F10A 83.4(5) . . ? F8 Sb2 F10A 130.2(12) . . ? F10 Sb2 F10A 54.5(8) . . ? F7 Sb2 F10A 138.5(8) . . ? F9A Sb2 F10A 83.3(8) . . ? F8A F7 Sb2 57.0(7) . . ? F8A F8 F9A 130.9(20) . . ? F8A F8 Sb2 64.7(11) . . ? F9A F8 Sb2 70.2(10) . . ? F10A F9 Sb2 75.5(7) . . ? F7A F10 F10A 132.2(17) . . ? F7A F10 Sb2 68.1(11) . . ? F10A F10 Sb2 67.0(8) . . ? F10 F7A Sb2 78.6(13) . . ? F8 F8A F7 142.6(21) . . ? F8 F8A Sb2 75.5(13) . . ? F7 F8A Sb2 72.7(10) . . ? F8 F9A Sb2 61.2(8) . . ? F9 F10A F10 106.7(11) . . ? F9 F10A Sb2 59.2(7) . . ? F10 F10A Sb2 58.4(6) . . ? _refine_diff_density_max 0.918 _refine_diff_density_min -0.927 _refine_diff_density_rms 0.126 #===End data_AsSSS _database_code_CSD 156701 # PhCSSC(Ph)S(AsF6)2 (-100 C) #This part of data was obtained from Dr. Cameron. #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H10 As2 F12 S3' _chemical_formula_weight 652.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.1371(9) _cell_length_b 14.8501(15) _cell_length_c 15.4273(17) _cell_angle_alpha 90.00 _cell_angle_beta 107.747(7) _cell_angle_gamma 90.00 _cell_volume 1993.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 3.776 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5041 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1187 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 30.42 _reflns_number_total 5041 _reflns_number_gt 2765 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5041 _refine_ls_number_parameters 316 _refine_ls_number_restraints 125 _refine_ls_R_factor_all 0.1356 _refine_ls_R_factor_gt 0.0757 _refine_ls_wR_factor_ref 0.2136 _refine_ls_wR_factor_gt 0.1908 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.02027(9) 0.36727(6) 0.13153(5) 0.0337(2) Uani 1 d . . . As2 As 0.25620(12) 0.10193(7) -0.00107(5) 0.0477(3) Uani 1 d DU . . S1 S 1.0408(2) 0.16357(14) 0.35195(11) 0.0315(4) Uani 1 d . . . S2 S 1.0472(2) 0.05628(14) 0.19334(12) 0.0364(4) Uani 1 d . . . S3 S 0.8353(2) 0.11060(15) 0.17320(12) 0.0373(5) Uani 1 d . . . F1 F 0.1435(8) 0.3649(4) 0.0673(4) 0.0613(15) Uani 1 d . . . F2 F -0.1010(6) 0.3698(4) 0.1981(4) 0.0585(15) Uani 1 d . . . F3 F -0.0673(8) 0.4619(4) 0.0769(4) 0.0691(17) Uani 1 d . . . F4 F 0.1052(6) 0.2734(4) 0.1891(3) 0.0455(12) Uani 1 d . . . F5 F 0.1489(6) 0.4335(4) 0.2085(3) 0.0508(13) Uani 1 d . . . F6 F -0.1085(7) 0.3018(4) 0.0540(4) 0.078(2) Uani 1 d . . . F7 F 0.1703(5) 0.1433(3) -0.10807(15) 0.0837(19) Uani 1 d DU . . F8 F 0.3419(5) 0.0605(3) 0.10589(15) 0.140(3) Uani 1 d DU . . F9 F 0.1294(6) 0.0139(3) -0.0231(3) 0.076(3) Uani 0.50 d PDU . . F10 F 0.3829(6) 0.1900(3) 0.0209(3) 0.136(4) Uani 0.50 d PDU . . F11 F 0.3795(6) 0.0403(4) -0.0416(4) 0.138(4) Uani 0.50 d PDU . . F12 F 0.1328(7) 0.1636(4) 0.0393(3) 0.144(4) Uani 0.50 d PDU . . F13 F 0.4276(3) 0.0954(5) -0.0240(4) 0.149(4) Uani 0.50 d PDU . . F14 F 0.0847(4) 0.1085(5) 0.0218(4) 0.122(3) Uani 0.50 d PDU . . F15 F 0.2997(8) 0.20927(14) 0.0388(3) 0.138(4) Uani 0.50 d PDU . . F16 F 0.2126(8) -0.00538(14) -0.0409(3) 0.084(3) Uani 0.50 d PDU . . C1 C 0.8645(8) 0.1678(5) 0.2712(5) 0.0316(15) Uani 1 d . . . C2 C 1.1374(8) 0.0984(6) 0.2975(5) 0.0331(16) Uani 1 d . . . C3 C 0.7422(8) 0.2189(5) 0.2876(5) 0.0337(16) Uani 1 d . . . C4 C 0.7730(8) 0.2798(6) 0.3611(5) 0.0361(17) Uani 1 d . . . C5 C 0.6536(10) 0.3276(6) 0.3733(6) 0.0421(19) Uani 1 d . . . C6 C 0.5033(10) 0.3168(7) 0.3158(6) 0.045(2) Uani 1 d . . . C7 C 0.4749(9) 0.2565(7) 0.2433(6) 0.048(2) Uani 1 d . . . C8 C 0.5932(9) 0.2087(6) 0.2289(5) 0.0425(19) Uani 1 d . . . C9 C 1.2988(9) 0.0789(5) 0.3401(5) 0.0348(17) Uani 1 d . . . C10 C 1.3742(9) 0.0127(6) 0.3041(6) 0.0425(19) Uani 1 d . . . C11 C 1.5307(10) -0.0002(7) 0.3433(6) 0.048(2) Uani 1 d . . . C12 C 1.6119(10) 0.0489(7) 0.4187(6) 0.045(2) Uani 1 d . . . C13 C 1.5389(9) 0.1132(6) 0.4566(6) 0.045(2) Uani 1 d . . . C14 C 1.3819(9) 0.1264(6) 0.4168(5) 0.0388(17) Uani 1 d . . . H1 H 0.8726 0.2859 0.4002 0.038 Uiso 1 d . . . H2 H 0.6714 0.3689 0.4229 0.047 Uiso 1 d . . . H3 H 0.4212 0.3506 0.3266 0.052 Uiso 1 d . . . H4 H 0.3734 0.2506 0.2034 0.057 Uiso 1 d . . . H5 H 0.5712 0.1672 0.1791 0.046 Uiso 1 d . . . H6 H 1.3194 -0.0225 0.2533 0.049 Uiso 1 d . . . H7 H 1.5822 -0.0439 0.3184 0.057 Uiso 1 d . . . H8 H 1.7170 0.0395 0.4435 0.050 Uiso 1 d . . . H9 H 1.5951 0.1470 0.5070 0.048 Uiso 1 d . . . H10 H 1.3313 0.1701 0.4427 0.045 Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0346(4) 0.0299(4) 0.0340(4) -0.0023(3) 0.0065(3) 0.0014(3) As2 0.0679(6) 0.0415(6) 0.0315(4) 0.0056(4) 0.0119(4) -0.0027(5) S1 0.0286(8) 0.0350(10) 0.0280(8) -0.0030(7) 0.0045(7) 0.0012(7) S2 0.0424(10) 0.0351(11) 0.0318(8) -0.0026(7) 0.0114(8) 0.0011(8) S3 0.0396(10) 0.0378(12) 0.0293(8) -0.0037(7) 0.0026(7) -0.0009(8) F1 0.097(4) 0.050(3) 0.055(3) 0.003(3) 0.049(3) 0.002(3) F2 0.043(3) 0.053(3) 0.091(4) -0.014(3) 0.038(3) -0.003(3) F3 0.085(4) 0.050(4) 0.062(3) 0.007(3) 0.007(3) 0.019(3) F4 0.045(3) 0.042(3) 0.050(3) 0.011(2) 0.016(2) 0.009(2) F5 0.041(3) 0.057(4) 0.055(3) -0.016(3) 0.016(2) -0.014(2) F6 0.061(4) 0.058(4) 0.083(4) -0.035(3) -0.023(3) 0.004(3) F7 0.110(5) 0.084(4) 0.0473(19) 0.028(3) 0.010(2) 0.028(4) F8 0.192(7) 0.104(6) 0.063(3) 0.048(3) -0.052(3) -0.079(5) F9 0.107(6) 0.085(5) 0.036(4) -0.022(4) 0.024(4) -0.045(4) F10 0.206(8) 0.125(6) 0.064(6) 0.014(5) 0.023(6) -0.110(6) F11 0.142(8) 0.081(7) 0.244(9) 0.089(8) 0.138(8) 0.075(5) F12 0.281(10) 0.057(6) 0.173(7) 0.018(7) 0.188(9) 0.034(6) F13 0.080(3) 0.102(8) 0.287(11) 0.141(9) 0.089(5) 0.053(5) F14 0.148(5) 0.099(10) 0.171(10) 0.022(10) 0.125(7) 0.029(6) F15 0.258(14) 0.051(2) 0.089(6) -0.006(3) 0.029(10) -0.052(6) F16 0.119(9) 0.042(2) 0.082(5) -0.011(2) 0.017(7) 0.010(4) C1 0.033(4) 0.028(4) 0.033(3) 0.002(3) 0.008(3) -0.005(3) C2 0.032(4) 0.033(4) 0.035(3) 0.004(3) 0.011(3) -0.002(3) C3 0.029(4) 0.030(4) 0.042(4) 0.006(3) 0.011(3) 0.001(3) C4 0.028(4) 0.039(5) 0.039(4) 0.002(3) 0.008(3) 0.000(3) C5 0.044(4) 0.040(5) 0.043(4) -0.002(4) 0.014(4) 0.000(4) C6 0.038(4) 0.049(6) 0.055(5) 0.015(4) 0.025(4) 0.012(4) C7 0.031(4) 0.061(6) 0.045(4) 0.009(4) 0.001(3) 0.002(4) C8 0.035(4) 0.049(5) 0.039(4) 0.009(4) 0.005(3) 0.004(4) C9 0.039(4) 0.031(4) 0.033(4) 0.006(3) 0.010(3) -0.005(3) C10 0.034(4) 0.040(5) 0.053(5) -0.008(4) 0.013(4) -0.001(4) C11 0.036(4) 0.049(6) 0.061(5) -0.005(4) 0.019(4) 0.002(4) C12 0.037(4) 0.047(6) 0.052(5) 0.004(4) 0.016(4) 0.003(4) C13 0.030(4) 0.048(6) 0.050(5) 0.002(4) 0.001(3) 0.004(4) C14 0.040(4) 0.036(5) 0.037(4) 0.000(3) 0.007(3) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 F6 1.704(5) . ? As1 F5 1.705(5) . ? As1 F3 1.707(6) . ? As1 F4 1.707(5) . ? As1 F1 1.712(5) . ? As1 F2 1.726(5) . ? As2 F8 1.7106(8) . ? As2 F13 1.7105(8) . ? As2 F10 1.7108(8) . ? As2 F16 1.7107(8) . ? As2 F12 1.7110(8) . ? As2 F11 1.7108(8) . ? As2 F15 1.7111(8) . ? As2 F9 1.7112(8) . ? As2 F14 1.7114(8) . ? As2 F7 1.7115(8) . ? S1 C2 1.695(8) . ? S1 C1 1.711(7) . ? S2 C2 1.687(8) . ? S2 S3 2.032(3) . ? S3 C1 1.683(8) . ? F9 F16 0.9290(9) . ? F9 F14 1.6720(11) . ? F10 F15 0.9300(9) . ? F10 F13 1.6709(11) . ? F11 F13 0.9297(9) . ? F11 F16 1.6715(11) . ? F12 F14 0.9293(9) . ? F12 F15 1.6713(11) . ? C1 C3 1.436(11) . ? C2 C9 1.449(11) . ? C3 C8 1.395(10) . ? C3 C4 1.409(11) . ? C4 C5 1.363(11) . ? C5 C6 1.399(12) . ? C6 C7 1.394(13) . ? C7 C8 1.367(13) . ? C9 C14 1.388(11) . ? C9 C10 1.408(12) . ? C10 C11 1.386(12) . ? C11 C12 1.382(13) . ? C12 C13 1.392(13) . ? C13 C14 1.392(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F6 As1 F5 179.5(3) . . ? F6 As1 F3 90.2(3) . . ? F5 As1 F3 89.4(3) . . ? F6 As1 F4 90.4(3) . . ? F5 As1 F4 90.1(3) . . ? F3 As1 F4 178.0(3) . . ? F6 As1 F1 91.0(3) . . ? F5 As1 F1 88.9(3) . . ? F3 As1 F1 91.3(3) . . ? F4 As1 F1 90.6(3) . . ? F6 As1 F2 89.9(3) . . ? F5 As1 F2 90.2(3) . . ? F3 As1 F2 89.2(3) . . ? F4 As1 F2 88.9(3) . . ? F1 As1 F2 178.9(3) . . ? F8 As2 F13 90.03(5) . . ? F8 As2 F10 90.04(5) . . ? F13 As2 F10 58.47(4) . . ? F8 As2 F16 90.00(5) . . ? F13 As2 F16 90.02(4) . . ? F10 As2 F16 148.49(5) . . ? F8 As2 F12 89.99(5) . . ? F13 As2 F12 148.48(5) . . ? F10 As2 F12 90.01(4) . . ? F16 As2 F12 121.50(5) . . ? F8 As2 F11 90.06(5) . . ? F13 As2 F11 31.53(3) . . ? F10 As2 F11 90.00(4) . . ? F16 As2 F11 58.49(4) . . ? F12 As2 F11 179.95(12) . . ? F8 As2 F15 90.02(5) . . ? F13 As2 F15 90.01(4) . . ? F10 As2 F15 31.54(3) . . ? F16 As2 F15 179.97(14) . . ? F12 As2 F15 58.47(4) . . ? F11 As2 F15 121.54(5) . . ? F8 As2 F9 90.01(5) . . ? F13 As2 F9 121.52(5) . . ? F10 As2 F9 179.96(13) . . ? F16 As2 F9 31.50(3) . . ? F12 As2 F9 90.00(4) . . ? F11 As2 F9 89.99(4) . . ? F15 As2 F9 148.47(5) . . ? F8 As2 F14 90.01(5) . . ? F13 As2 F14 179.96(14) . . ? F10 As2 F14 121.52(5) . . ? F16 As2 F14 89.99(4) . . ? F12 As2 F14 31.51(3) . . ? F11 As2 F14 148.48(5) . . ? F15 As2 F14 89.98(4) . . ? F9 As2 F14 58.49(4) . . ? F8 As2 F7 179.96(14) . . ? F13 As2 F7 90.01(5) . . ? F10 As2 F7 89.98(5) . . ? F16 As2 F7 90.00(5) . . ? F12 As2 F7 89.98(5) . . ? F11 As2 F7 89.98(5) . . ? F15 As2 F7 89.98(5) . . ? F9 As2 F7 89.97(5) . . ? F14 As2 F7 89.95(5) . . ? C2 S1 C1 100.2(4) . . ? C2 S2 S3 99.5(3) . . ? C1 S3 S2 100.4(3) . . ? F16 F9 F14 134.99(7) . . ? F16 F9 As2 74.22(6) . . ? F14 F9 As2 60.76(4) . . ? F15 F10 F13 135.00(7) . . ? F15 F10 As2 74.25(6) . . ? F13 F10 As2 60.76(4) . . ? F13 F11 F16 134.97(7) . . ? F13 F11 As2 74.21(6) . . ? F16 F11 As2 60.75(4) . . ? F14 F12 F15 135.04(7) . . ? F14 F12 As2 74.27(6) . . ? F15 F12 As2 60.77(4) . . ? F11 F13 F10 135.03(7) . . ? F11 F13 As2 74.25(6) . . ? F10 F13 As2 60.77(4) . . ? F12 F14 F9 134.97(7) . . ? F12 F14 As2 74.22(6) . . ? F9 F14 As2 60.75(4) . . ? F10 F15 F12 134.98(7) . . ? F10 F15 As2 74.21(6) . . ? F12 F15 As2 60.76(4) . . ? F9 F16 F11 135.03(7) . . ? F9 F16 As2 74.27(6) . . ? F11 F16 As2 60.76(4) . . ? C3 C1 S3 120.4(5) . . ? C3 C1 S1 120.1(6) . . ? S3 C1 S1 119.5(5) . . ? C9 C2 S2 119.5(6) . . ? C9 C2 S1 120.1(6) . . ? S2 C2 S1 120.4(4) . . ? C8 C3 C4 120.6(7) . . ? C8 C3 C1 119.1(7) . . ? C4 C3 C1 120.3(6) . . ? C5 C4 C3 118.3(7) . . ? C4 C5 C6 121.7(8) . . ? C7 C6 C5 119.3(8) . . ? C8 C7 C6 120.1(7) . . ? C7 C8 C3 120.1(8) . . ? C14 C9 C10 119.0(7) . . ? C14 C9 C2 120.1(8) . . ? C10 C9 C2 120.9(7) . . ? C11 C10 C9 119.3(8) . . ? C12 C11 C10 120.8(8) . . ? C11 C12 C13 120.9(8) . . ? C12 C13 C14 118.2(8) . . ? C9 C14 C13 121.8(8) . . ? _diffrn_measured_fraction_theta_max 0.807 _diffrn_reflns_theta_full 30.42 _diffrn_measured_fraction_theta_full 0.807 _refine_diff_density_max 1.994 _refine_diff_density_min -1.839 _refine_diff_density_rms 0.186 #------------------------------------------------------------------------------ #===End