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_7718870
_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_absolute_configuration ad
_chemical_formula_moiety         'Ga3 Ge2 La3 O10 S3'
_chemical_formula_sum            'Ga3 Ge2 La3 O10 S3'
_chemical_formula_weight         1027.25
_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             2025-04-25
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, 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                   10.1701(4)
_cell_length_b                   10.1701(4)
_cell_length_c                   7.5198(3)
_cell_measurement_reflns_used    6837
_cell_measurement_temperature    297.15
_cell_measurement_theta_max      30.5300
_cell_measurement_theta_min      3.5340
_cell_volume                     673.58(5)
_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-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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      6.00 110.00   0.50   15.00    --   20.00  54.00 -90.00  208
  2  \w    -71.00 -39.00   0.50   15.00    --   20.00  54.00 120.00   64
  3  \w    -22.00  98.00   0.50   15.00    --   20.00  54.00 120.00  240
  4  \w    -72.00 110.00   0.50   15.00    --   20.00  54.00  60.00  364
  5  \w    -20.00  54.00   0.50   15.00    --   20.00  54.00-180.00  148
  6  \w     70.00  95.00   0.50   15.00    --   20.00  54.00-180.00   50
  7  \w    -73.00 -44.00   0.50   15.00    --   20.00  54.00 -30.00   58
  8  \w     20.00  45.00   0.50   15.00    --   20.00  54.00 -30.00   50
  9  \w     75.00 100.00   0.50   15.00    --   20.00  54.00 -30.00   50
 10  \w    -73.00 -38.00   0.50   15.00    --   20.00  54.00-150.00   70
 11  \w     -6.00  26.00   0.50   15.00    --   20.00  54.00-150.00   64
 12  \w     57.00  82.00   0.50   15.00    --   20.00  54.00-150.00   50
 13  \w    -59.00 -33.00   0.50   15.00    --   20.00  54.00 150.00   52
 14  \w     62.00  87.00   0.50   15.00    --   20.00  54.00  30.00   50
 15  \w    -68.00 -21.00   0.50   15.00    --   20.00  54.00 -90.00   94
;
_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      0.0802620000
_diffrn_orient_matrix_UB_12      0.0341800000
_diffrn_orient_matrix_UB_13      0.0007492000
_diffrn_orient_matrix_UB_21      0.0019588000
_diffrn_orient_matrix_UB_22      0.0264976000
_diffrn_orient_matrix_UB_23      0.0877307000
_diffrn_orient_matrix_UB_31      -0.0065540000
_diffrn_orient_matrix_UB_32      -0.0678998000
_diffrn_orient_matrix_UB_33      0.0346150000
_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  0.0417
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9330
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         2.312
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    20.096
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62103
_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 whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    5.065
_exptl_crystal_description       irregular
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.0848
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 300 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(13)
_refine_ls_extinction_coef       0.0049(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0114
_refine_ls_R_factor_gt           0.0109
_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^)+(0.0100P)^2^+0.3488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0251
_refine_ls_wR_factor_ref         0.0252
_reflns_Friedel_coverage         0.723
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                719
_reflns_number_total             734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01100k2.cif
_cod_data_source_block           La3Ga3Ge2S3O10
_cod_depositor_comments
'Adding full bibliography for 7718868--7718871.cif.'
_cod_original_cell_volume        673.58(6)
_cod_database_code               7718870
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'La Ga Ge S O'
_shelx_estimated_absorpt_t_max   0.427
_shelx_estimated_absorpt_t_min   0.259
_olex2_refinement_description
;
;
_shelx_res_checksum              44835
_shelx_hkl_checksum              32322
_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 1.354
_oxdiff_exptl_absorpt_empirical_full_min 0.748