Accurate X-ray diffraction data required for proper evaluation of bond valence sums and global instability indexes: redetermination of the crystal structures of diamond-like Cu<sub>2</sub>CdSiS<sub>4</sub> and Cu<sub>2</sub>HgSnS<sub>4</sub> as a case study.
Treece, Megan M.; Kelly, Jordan C.; Rosello, Kate E.; Craig, Andrew J.; Aitken, Jennifer A.; Acta crystallographica. Section C, Structural chemistry 79 (2023) –; doi:10.1107/S2053229623006848

data_2312275
_publ_section_title
;
 Accurate X-ray diffraction data required for proper evaluation of bond
 valence sums and global instability indexes: redetermination of the
 crystal structures of diamond-like Cu<sub>2</sub>CdSiS<sub>4</sub> and
 Cu<sub>2</sub>HgSnS<sub>4</sub> as a case study.
;
_journal_coeditor_code           VX3001
_journal_issue                   9
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi               10.1107/S2053229623006848
_journal_volume                  79
_journal_year                    2023
_chemical_absolute_configuration inapplicable
_chemical_formula_iupac          'Cu2 Cd Si S4'
_chemical_formula_moiety         'Cd Cu2 S4 Si'
_chemical_formula_sum            'Cd Cu2 S4 Si'
_chemical_formula_weight         395.81
_chemical_name_common            'Copper cadmium silicon sulfide'
_chemical_name_systematic        'Copper cadmium silicon sulfide'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.60853(11)
_cell_length_b                   6.48071(9)
_cell_length_c                   6.24923(10)
_cell_measurement_reflns_used    5413
_cell_measurement_temperature    296
_cell_measurement_theta_max      32.755
_cell_measurement_theta_min      3.140
_cell_volume                     308.141(8)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
SMART (Bruker, 2001)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_molecular_graphics
;
ShelXle (H\"ubschle <i>et al.</i>,  2011)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0326
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3842
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.143
_diffrn_source                   'fine focus sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    11.669
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.3569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2002)
;
_exptl_crystal_colour            green-yellow
_exptl_crystal_density_diffrn    4.266
_exptl_crystal_description       polyhedra
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.330
_refine_diff_density_min         -2.257
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 305 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.006(10)
_refine_ls_extinction_coef       0.446(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015<>i>b</i>)
;
_refine_ls_goodness_of_fit_ref   1.269
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         723
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.268
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+0.0278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0470
_reflns_number_gt                719
_reflns_number_total             723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vx3001sup1.cif
_cod_data_source_block           Cu2CdSiS4
_cod_database_code               2312275
_shelx_estimated_absorpt_t_min   0.158
_shelx_estimated_absorpt_t_max   0.420
_shelx_hkl_checksum              97105
_shelx_res_checksum              21236
_cod_database_fobs_code 2312275