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_4336649
_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            'Ag Ge2 Na5 S7'
_chemical_formula_weight         592.42
_chemical_name_common            compound-4
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 104.315(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1456(18)
_cell_length_b                   10.2611(19)
_cell_length_c                   14.863(3)
_cell_measurement_reflns_used    2468
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.59
_cell_measurement_theta_min      2.83
_cell_volume                     1351.5(5)
_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(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3700
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    7.051
_exptl_absorpt_correction_T_max  0.6023
_exptl_absorpt_correction_T_min  0.3329
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.912
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.590
_refine_diff_density_min         -1.783
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.00084(17)
_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   1.136
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0331P)^2^+13.0139P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0767
_reflns_number_gt                1114
_reflns_number_total             1189
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402092r_si_001_4.cif
_cod_data_source_block           4
_cod_original_cell_volume        1351.5(4)
_cod_original_formula_sum        ' Ag Ge2  Na5 S7'
_cod_database_code               4336649