Copper-Rich Framework Sulfides: A4Cu8Ge3S12 (A = K, Rb) with Cubic Perovskite Structure
Ren-Chun Zhang; Hua-Gang Yao; Shou-Hua Ji; Mei-Chen Liu; Min Ji; Yong-Lin An; Inorganic Chemistry 49 (2010) 6372–6374; doi:10.1021/ic100690q

data_4316064
_publ_section_title
;
 Copper-Rich Framework Sulfides: A4Cu8Ge3S12 (A = K, Rb) with Cubic
 Perovskite Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6372
_journal_page_last               6374
_journal_paper_doi               10.1021/ic100690q
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'Cu32 Ge12 K16 S48'
_chemical_formula_weight         5068.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           226
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4a 2 3'
_symmetry_space_group_name_H-M   'F m -3 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                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.6753(17)
_cell_length_b                   17.6753(17)
_cell_length_c                   17.6753(17)
_cell_measurement_reflns_used    1853
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.394
_cell_measurement_theta_min      2.304
_cell_volume                     5522.1(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Smart Apex II CCD'
_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  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6143
_diffrn_reflns_theta_full        28.19
_diffrn_reflns_theta_max         28.19
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    10.744
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4768
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.20
_refine_diff_density_min         -2.087
_refine_diff_density_rms         0.315
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     15
_refine_ls_number_reflns         322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0426
_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^)+(0.1900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1597
_reflns_number_gt                262
_reflns_number_total             322
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100690q_si_001_1.cif
_cod_data_source_block           K4Cu8Ge3S12
_cod_database_code               4316064