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_4336648
_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            'Ag7 Cs S4'
_chemical_formula_weight         1016.24
_chemical_name_common            Compound-3
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1002(13)
_cell_length_b                   11.1002(13)
_cell_length_c                   8.531(2)
_cell_measurement_temperature    296
_cell_volume                     1051.1(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5021
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    16.907
_exptl_absorpt_correction_T_max  0.1330
_exptl_absorpt_correction_T_min  0.0879
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    6.422
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.481
_refine_diff_density_min         -1.585
_refine_diff_density_rms         0.204
_refine_ls_extinction_coef       0.00067(7)
_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   1.075
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0204P)^2^+17.3187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                853
_reflns_number_total             936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402092r_si_001_3.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               4336648