#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003788.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003788 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1547 _journal_page_last 1549 _publ_section_title ; Hexakis(dimethyl sulfoxide)mercury(II) Trifluoromethanesulfonate, a Standard for Solid-State ^199^Hg NMR ; _chemical_formula_moiety 'C12 H36 Hg O6 S6,2(C F3 S O3)' _chemical_formula_sum 'C14 H36 F6 Hg O12 S8' _chemical_formula_weight 967.49 _symmetry_cell_setting trigonal loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -y, +x-y, +z' ' -x+y, -x, +z' ' -x, -y, -z' ' +y, -x+y, -z' ' +x-y, +x, -z' _symmetry_space_group_name_H-M 'P -3' _cell_length_a 12.195(1) _cell_length_b 12.1952 _cell_length_c 6.713(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 864.6(2) _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 1.858 _exptl_crystal_density_meas 0.000 _diffrn_radiation_type CuKalpha _diffrn_radiation_wavelength 1.5418 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 48.8 _cell_measurement_theta_max 50.0 _exptl_absorpt_coefficient_mu 12.76 _cell_measurement_temperature 293 _exptl_crystal_description 'block' _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.100 _exptl_crystal_colour 'colourless' _chemical_compound_source ; The literature synthesis (Peringer, 1980) produced (1) in crystalline form ; _diffrn_measurement_device 'Rigaku AFC6R' _diffrn_measurement_method '\w/2\q scans' _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.157 _exptl_absorpt_correction_T_max 0.354 _diffrn_reflns_number 1498 _reflns_number_total 869 _reflns_number_observed 859 _reflns_observed_criterion >3\s(I) _diffrn_reflns_av_R_equivalents 8.12 _diffrn_reflns_theta_max 60.12 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -10.79 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.0360 _refine_ls_wR_factor_obs 0.0460 _refine_ls_wR_factor_all ? _refine_ls_goodness_of_fit_obs 2.69 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 859 _refine_ls_number_parameters 64 _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme ; w=4F~o~^2^/[\s^2^(F~o~^2^)+(0.009F~o~^2^)^2^] ; _refine_ls_shift/esd_max 0.0030 _refine_diff_density_max 1.04 _refine_diff_density_min -1.20 _refine_ls_extinction_method 'Zachariasen (1968) type 2 Gaussian isotropic' _refine_ls_extinction_coef 2E-6(2) loop_ _atom_type_symbol _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C 'International Tables' 0.018 0.009 H 'International Tables' 0.000 0.000 F 'International Tables' 0.073 0.053 Hg 'International Tables' -4.292 7.685 O 'International Tables' 0.049 0.032 S 'International Tables' 0.333 0.557 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? ;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1989) ; ; TEXSAN (Molecular Structure Corporation, 1993) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Hg(1) 0.0 0.0 0.0 0.0376(3) S(1) 0.2141(2) -0.0540(2) 0.2176(3) 0.042(1) S(2) 0.6667 0.3333 -0.3568(5) 0.051(1) F(1) 0.6628(7) 0.2316(6) -0.7020(9) 0.098(4) O(1) 0.1832(5) 0.0528(5) 0.1848(7) 0.050(3) O(2) 0.5516(6) 0.2214(6) -0.3095(9) 0.078(4) C(1) 0.2999(9) -0.0130(8) 0.443(1) 0.059(5) C(2) 0.3391(9) -0.0235(10) 0.053(1) 0.069(5) C(3) 0.6667 0.3333 -0.626(2) 0.061(6) H(1a) 0.3221 -0.0753 0.4756 0.0702 H(1b) 0.3747 0.0670 0.4292 0.0702 H(1c) 0.2491 -0.0085 0.5470 0.0702 H(2a) 0.3612 -0.0876 0.0679 0.0821 H(2b) 0.3130 -0.0232 -0.0799 0.0821 H(2c) 0.4105 0.0566 0.0836 0.0821 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Hg(1) 0.0338(4) 0.0169 0.0000 0.0338 0.0000 0.0452(5) S(1) 0.043(1) 0.0206(9) -0.0045(8) 0.041(1) -0.0011(8) 0.042(1) S(2) 0.046(1) 0.0231 0.0000 0.0461 0.0000 0.059(2) F(1) 0.141(6) 0.070(5) -0.012(4) 0.091(5) -0.027(3) 0.079(4) O(1) 0.051(3) 0.025(3) -0.012(3) 0.046(3) -0.006(3) 0.054(3) O(2) 0.063(4) 0.011(3) 0.006(3) 0.061(4) 0.016(3) 0.083(5) C(1) 0.074(6) 0.037(5) -0.017(4) 0.057(5) -0.008(4) 0.048(5) C(2) 0.069(6) 0.051(6) 0.016(5) 0.087(7) 0.014(5) 0.065(6) C(3) 0.058(6) 0.0291 0.0000 0.0583 0.0000 0.07(1)