Solvothermal syntheses, crystal structures, and properties of new mercury(II)‒thioantimonates(III) and a mixed-valent thioantimonate(III,V)
Tang, Weiwei; Tang, Chunying; Wang, Fang; Chen, Ruihong; Zhang, Yong; Jia, Dingxian; Journal of Solid State Chemistry 199 (2013) 287–294; doi:10.1016/j.jssc.2012.12.035

data_1562723
_publ_section_title
;
 Solvothermal syntheses, crystal structures, and properties of new
 mercury(II)--thioantimonates(III) and a mixed-valent
 thioantimonate(III,V)
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              287
_journal_page_last               294
_journal_paper_doi               10.1016/j.jssc.2012.12.035
_journal_volume                  199
_journal_year                    2013
_chemical_formula_moiety         'C4 H15 N3, Hg S14 Sb8'
_chemical_formula_sum            'C4 H15 Hg N3 S14 Sb8'
_chemical_formula_weight         1728.62
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.424(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.0893(16)
_cell_length_b                   28.258(6)
_cell_length_c                   7.9381(18)
_cell_measurement_reflns_used    7183
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.2
_cell_volume                     1573.1(6)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12472
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    12.551
_exptl_absorpt_correction_T_max  0.3667
_exptl_absorpt_correction_T_min  0.0550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.649
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.441
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.330
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    .
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2876
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1436P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                2442
_reflns_number_total             2876
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2013-199-287.cif
_cod_data_source_block           complex_3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1562723