Mild Solvothermal Syntheses of Thioargentates A-Ag-S (A = K, Rb, Cs) and A-Ag-Ge-S (A = Na, Rb): Crucial Role of Excess Sulfur
Chi Zhang; Kai-Ni Wang; Min Ji; Yong-Lin An; Inorganic Chemistry 52 (2013) 12367–12371; doi:10.1021/ic402092r

data_4336646
_publ_section_title
;
 Mild Solvothermal Syntheses of Thioargentates A-Ag-S (A = K, Rb, Cs) and
 A-Ag-Ge-S (A = Na, Rb): Crucial Role of Excess Sulfur
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12367
_journal_page_last               12371
_journal_paper_doi               10.1021/ic402092r
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'Ag5 K S3'
_chemical_formula_weight         674.66
_chemical_name_common            Compound-1
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           190
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P -6c -2c'
_symmetry_space_group_name_H-M   'P -6 2 c'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.2208(12)
_cell_length_b                   13.2208(12)
_cell_length_c                   7.9479(14)
_cell_measurement_temperature    296
_cell_volume                     1203.1(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5096
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    13.189
_exptl_absorpt_correction_T_max  0.2596
_exptl_absorpt_correction_T_min  0.1195
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark red-black'
_exptl_crystal_density_diffrn    5.587
_exptl_crystal_description       block
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.367
_refine_diff_density_min         -3.253
_refine_diff_density_rms         0.763
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.41(13)
_refine_ls_extinction_coef       0.0116(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.333
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.333
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0395P)^2^+2.1661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0797
_reflns_number_gt                751
_reflns_number_total             771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402092r_si_001_1.cif
_cod_data_source_block           1
_cod_database_code               4336646