The crystal structure of Cu~2~GeSe~3~ and the structure-types of the I~2~-IV-VI~3~ family of semiconducting compounds
Dugarte-Dugarte, Analio; Ramírez Pineda, Nahum; Nieves, Luis; Henao, José Antonio; Díaz de Delgado, Graciela; Delgado, José Miguel; Acta Crystallographica Section B 77 (2021) 158–167; doi:10.1107/S2052520620016571

data_2108771
_publ_section_title
;
 The crystal structure of Cu~2~GeSe~3~ and the structure-types of the
 I~2~-IV-VI~3~ family of semiconducting compounds
;
_journal_coeditor_code           RA5092SUP1
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              158
_journal_page_last               167
_journal_paper_doi               10.1107/S2052520620016571
_journal_volume                  77
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Cu2 Ge Se3'
_chemical_formula_sum            'Cu2 Ge Se3'
_chemical_formula_weight         436.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-08 # Formatted by IUCr publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 108.512(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.7703(4)
_cell_length_b                   11.8624(5)
_cell_length_c                   6.7705(4)
_cell_measurement_reflns_used    2471
_cell_measurement_temperature    293
_cell_measurement_theta_max      34.7790
_cell_measurement_theta_min      3.1330
_cell_volume                     515.62(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material
'Olex2 (Dolomanov et al., 2009) and enCIFer (Allen et al., 2004)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'PILATUS 200'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -114.00  66.00   0.50   30.00    --  -24.00  24.00 108.00  360
  2  \w    -90.00  47.00   0.50   30.00    --  -24.00  36.00 -72.00  274
  3  \w    -86.50  43.50   0.50   30.00    --  -24.00  60.00 108.00  260
  4  \w   -100.50 -24.00   0.50   30.00    --  -24.00  12.00  72.00  153
  5  \w   -114.00 -69.00   0.50   30.00    --  -24.00  24.00-180.00   90
;
_diffrn_measurement_device       'AFC11 (Right): Eulerian 3 circle'
_diffrn_measurement_device_type  'Rigaku XtaLab Pro'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0954395000
_diffrn_orient_matrix_UB_12      -0.0202830000
_diffrn_orient_matrix_UB_13      -0.0693203000
_diffrn_orient_matrix_UB_21      -0.0557223000
_diffrn_orient_matrix_UB_22      0.0347576000
_diffrn_orient_matrix_UB_23      0.0492467000
_diffrn_orient_matrix_UB_31      0.0000708000
_diffrn_orient_matrix_UB_32      0.0442099000
_diffrn_orient_matrix_UB_33      -0.0704742000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4227
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.829
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.632
_diffrn_reflns_theta_min         3.435
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    34.964
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28e (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            grey
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    grey
_exptl_crystal_density_diffrn    5.624
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.533
_refine_diff_density_min         -1.830
_refine_diff_density_rms         0.410
_refine_ls_abs_structure_details
;
 Flack x determined using 626 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.043(18)
_refine_ls_extinction_coef       0.0158(8)
_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   1.163
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         1824
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0266P)^2^+0.1027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0770
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    0.938
_reflns_Friedel_fraction_max     0.718
_reflns_number_gt                1605
_reflns_number_total             1824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ra5092sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2108771.cif.'
_cod_database_code               2108771
_cod_database_fobs_code          2108771
_publcif_datablock.id            {5770b306-16e6-459e-8418-7e60a4a1a42c}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu2 Ge Se3'
_shelx_estimated_absorpt_t_max   0.048
_shelx_estimated_absorpt_t_min   0.044
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop with grease'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.543
_oxdiff_exptl_absorpt_empirical_full_min 0.669
_publcif_info_exptl_table_max_cols 5
_publcif_info_exptl_table_use_headnotes n
_publcif_funding_html
;
;