Flux crystal growth, structure, and optical properties of non-centrosymmetric oxysulfides Ln<sub>3</sub>Ga<sub>3</sub>Ge<sub>2</sub>S<sub>3</sub>O<sub>10</sub> (Ln = La, Ce, Pr, Nd).
Yan, Hong; Fujii, Kotaro; Matsushita, Yoshitaka; Yashima, Masatomo; Yamaura, Kazunari; Tsujimoto, Yoshihiro; Dalton transactions (Cambridge, England : 2003) 54 (2025) 10433–10440; doi:10.1039/d5dt01100k

data_7718869
_publ_section_title
;
 Flux crystal growth, structure, and optical properties of
 non-centrosymmetric oxysulfides
 Ln<sub>3</sub>Ga<sub>3</sub>Ge<sub>2</sub>S<sub>3</sub>O<sub>10</sub> (Ln
 = La, Ce, Pr, Nd).
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10433
_journal_page_last               10440
_journal_paper_doi               10.1039/d5dt01100k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'Ga3 Ge2 O10 Pr3 S3'
_chemical_formula_sum            'Ga3 Ge2 O10 Pr3 S3'
_chemical_formula_weight         1033.25
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_space_group_name_H-M_alt        'P -6 2 c'
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-30
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2025-05-07 deposited with the CCDC.	2025-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.0921(7)
_cell_length_b                   10.0921(7)
_cell_length_c                   7.4251(5)
_cell_measurement_reflns_used    1991
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.3800
_cell_measurement_theta_min      3.5840
_cell_volume                     654.93(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      297.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.979
_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    -52.00 -26.00   0.50    4.08    --   20.00  54.00 150.00   52
  2  \w      9.00  47.00   0.50    4.08    --   20.00  54.00 150.00   76
  3  \w     76.00 102.00   0.50    4.08    --   20.00  54.00 150.00   52
  4  \w     80.00 105.00   0.50    4.08    --   20.00  54.00-180.00   50
  5  \w    -74.00  65.00   0.50    4.08    --   20.00  54.00-120.00  278
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0148315000
_diffrn_orient_matrix_UB_12      0.0405795000
_diffrn_orient_matrix_UB_13      0.0675565000
_diffrn_orient_matrix_UB_21      -0.0494789000
_diffrn_orient_matrix_UB_22      -0.0699289000
_diffrn_orient_matrix_UB_23      0.0442740000
_diffrn_orient_matrix_UB_31      0.0626281000
_diffrn_orient_matrix_UB_32      0.0069560000
_diffrn_orient_matrix_UB_33      0.0509604000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2246
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.357
_diffrn_reflns_theta_min         2.330
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    22.042
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.60a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear greenish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    5.240
_exptl_crystal_description       block
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 180 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_coef       0.00504(17)
_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   0.977
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0136
_refine_ls_R_factor_gt           0.0128
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0234
_refine_ls_wR_factor_ref         0.0236
_reflns_Friedel_coverage         0.656
_reflns_Friedel_fraction_full    0.904
_reflns_Friedel_fraction_max     0.907
_reflns_number_gt                457
_reflns_number_total             467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01100k2.cif
_cod_data_source_block           exp_306
_cod_depositor_comments
'Adding full bibliography for 7718868--7718871.cif.'
_cod_original_cell_volume        654.93(9)
_cod_database_code               7718869
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pr3 Ga3 Ge2 S3 O10'
_shelx_estimated_absorpt_t_max   0.250
_shelx_estimated_absorpt_t_min   0.158
_olex2_refinement_description
;
;
_shelx_res_checksum              87327
_shelx_hkl_checksum              3329
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.317
_oxdiff_exptl_absorpt_empirical_full_min 0.744