Syntheses and crystal structures of the quaternary thiogermanates Cu~4~FeGe~2~S~7~ and Cu~4~CoGe~2~S~7~
Craig, Andrew J.; Stoyko, Stanislav S.; Bonnoni, Allyson; Aitken, Jennifer A.; Acta Crystallographica Section E 76 (2020) 1117–1121; doi:10.1107/S2056989020007872

data_2243524
_publ_section_title
;
 Syntheses and crystal structures of the quaternary thiogermanates
 Cu~4~FeGe~2~S~7~ and Cu~4~CoGe~2~S~7~
;
_journal_coeditor_code           HB7920
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1117
_journal_page_last               1121
_journal_paper_doi               10.1107/S2056989020007872
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          'Cu4 Fe Ge2 S7'
_chemical_formula_moiety         'Cu4 Fe Ge2 S7'
_chemical_formula_sum            'Cu4 Fe Ge2 S7'
_chemical_formula_weight         679.61
_chemical_name_systematic
;
Tetracopper iron digermanium heptasulfide
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 98.661(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7405(6)
_cell_length_b                   5.3589(2)
_cell_length_c                   8.3420(4)
_cell_measurement_reflns_used    4891
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.3595
_cell_measurement_theta_min      4.1805
_cell_volume                     518.86(4)
_computing_cell_refinement
;
SAINT (Bruker, 1998)
;
_computing_data_collection
;
SMART (Bruker, 1998)
;
_computing_data_reduction
;
SAINT (Bruker, 1998)
;
_computing_molecular_graphics
;
CrystalMaker (Palmer, 2014)
;
_computing_publication_material
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       '\f and \w Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2258
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.453
_diffrn_reflns_theta_min         2.470
_exptl_absorpt_coefficient_mu    16.457
_exptl_absorpt_correction_T_max  0.4352
_exptl_absorpt_correction_T_min  0.2456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2002)
;
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    4.350
_exptl_crystal_description       irregular
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.082
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.889
_refine_ls_abs_structure_details
;
Flack (1983)
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_coef       0.0123(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2018/3 (Sheldrick 2018)
;
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1187
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0315P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0938
_reflns_number_gt                994
_reflns_number_total             1187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7920sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2243524
_shelx_estimated_absorpt_t_min   0.346
_shelx_estimated_absorpt_t_max   0.629
_shelx_hkl_checksum              20162
_shelx_res_checksum              6844