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_1562722
_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         'C8 H26 N6 Ni, Hg S5 Sb2'
_chemical_formula_sum            'C8 H26 Hg N6 Ni S5 Sb2'
_chemical_formula_weight         869.45
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.015(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5862(11)
_cell_length_b                   20.6190(18)
_cell_length_c                   10.7610(11)
_cell_measurement_reflns_used    9390
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2145.6(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10704
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    10.980
_exptl_absorpt_correction_T_max  0.3525
_exptl_absorpt_correction_T_min  0.0730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orang
_exptl_crystal_density_diffrn    2.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.894
_refine_diff_density_min         -1.298
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3911
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+1.1724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0795
_reflns_number_gt                3455
_reflns_number_total             3911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2013-199-287.cif
_cod_data_source_block           complex_2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1562722