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_4331488
_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            'Ge3 K4 S14 Sn3'
_chemical_formula_weight         1179.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 100.508(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.9442(16)
_cell_length_b                   15.118(4)
_cell_length_c                   12.071(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1246.0(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 0.957
_diffrn_measured_fraction_theta_max 0.957
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13054
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    8.366
_exptl_crystal_density_diffrn    3.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1092
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       0.00000(10)
_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   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         2960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+0.3130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0589
_reflns_number_gt                2329
_reflns_number_total             2960
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050087vsup3.cif
_cod_data_source_block           73am
_cod_database_code               4331488