Exploratory Synthesis in Molten Salts: Role of Flux Basicity in the Stabilization of the Complex Thiogermanates Cs4Pb4Ge5S16, K2PbGe2S6, and K4Sn3Ge3S14
Palchik, Oleg; Marking, Gregory M.; Kanatzidis, Mercouri G.; Inorganic Chemistry 44 (2005) 4151–4153; doi:10.1021/ic050087v

data_4331486
_publ_section_title
;
 Exploratory Synthesis in Molten Salts:&#x00A0; Role of Flux Basicity in
 the Stabilization of the Complex Thiogermanates Cs4Pb4Ge5S16, K2PbGe2S6,
 and K4Sn3Ge3S14
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4151
_journal_page_last               4153
_journal_paper_doi               10.1021/ic050087v
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'Cs4 Ge5 Pb4 S16'
_chemical_formula_weight         2236.31
_chemical_name_common            Cs4Pb4Ge5S16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           64
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_atom_sites_solution_hydrogens   geom
_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            8
_cell_length_a                   38.3020(19)
_cell_length_b                   9.0770(5)
_cell_length_c                   19.4421(1)
_cell_measurement_temperature    293(2)
_cell_volume                     6759.4(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38801
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    29.462
_exptl_crystal_density_diffrn    4.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7712
_refine_diff_density_max         2.012
_refine_diff_density_min         -1.593
_refine_diff_density_rms         0.255
_refine_ls_extinction_coef       0.000037(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   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         4215
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+14.5462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0636
_reflns_number_gt                3325
_reflns_number_total             4215
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050087vsup1.cif
_cod_data_source_block           52at
_cod_original_cell_volume        6759(6)
_cod_database_code               4331486