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_4336650
_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
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_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            'Ag2 Ge Rb2 S4'
_chemical_formula_weight         587.51
_chemical_name_common            Compound-5
_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                 115.664(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4774(3)
_cell_length_b                   22.1120(7)
_cell_length_c                   6.2963(2)
_cell_measurement_temperature    296
_cell_volume                     938.33(6)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296
_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  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2650
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    18.428
_exptl_absorpt_correction_T_max  0.1565
_exptl_absorpt_correction_T_min  0.0789
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    4.159
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.302
_refine_diff_density_min         -1.468
_refine_diff_density_rms         0.336
_refine_ls_extinction_coef       0.0014(3)
_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   0.887
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0375
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                781
_reflns_number_total             830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402092r_si_001_5.cif
_cod_data_source_block           5
_cod_database_code               4336650