# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_521_auto
_database_code_depnum_ccdc_archive 'CCDC 2449159'
loop_
_audit_author_name
_audit_author_address
'Yoshihiro Tsujimoto'
;National Institute for Materials Science
Japan
;
_audit_update_record             
;
2025-05-07 deposited with the CCDC.	2025-06-12 downloaded from the CCDC.
;
_audit_creation_date             2025-05-02
_audit_creation_method           
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Ce3 Ga3 Ge2 O10 S3'
_chemical_formula_sum            'Ce3 Ga3 Ge2 O10 S3'
_chemical_formula_weight         1030.88
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ce3 Ga3 Ge2 S3 O10'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_H-M_alt        'P -6 2 c'
_space_group_name_Hall           'P -6c -2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z+1/2'
'-y, x-y, -z+1/2'
'-x+y, -x, -z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'

_cell_length_a                   10.0993(4)
_cell_length_b                   10.0993(4)
_cell_length_c                   7.4738(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     660.17(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5693
_cell_measurement_temperature    297
_cell_measurement_theta_max      30.7070
_cell_measurement_theta_min      3.5450
_shelx_estimated_absorpt_T_max   0.570
_shelx_estimated_absorpt_T_min   0.300
_exptl_absorpt_coefficient_mu    21.140
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_correction_T_min  0.544
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    5.186
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             918
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 3 0 0.0049
5 3 0 0.0223
1 -1 0 0.0205
-2 -5 0 0.0187
0 1 0 0.0131
2 -1 -5 0.0279
-2 1 5 0.0345

_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5.0000 3.0000 -0.0000 -0.3320 -0.1172 0.0313
5.0000 3.0000 0.0000 0.3251 0.0971 0.4546
1.0000 -1.0000 0.0000 0.0669 0.0248 -0.0387
-2.0000 -5.0000 -0.0000 -0.1257 -0.0262 -0.4896
-0.0000 1.0000 0.0000 -0.0012 -0.0033 0.0810
2.0000 -1.0000 -5.0000 -0.0240 0.4941 0.0200
-2.0000 1.0000 5.0000 0.0240 -0.4941 -0.0200

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9529
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.644
_diffrn_reflns_theta_min         2.329
_diffrn_ambient_temperature      297.00
_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 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -37.00   9.00   0.50   14.54    --   20.00  54.00 -30.00   92
  2  ω    -74.00  49.00   0.50   14.54    --   20.00  54.00-150.00  246
  3  ω     63.00 110.00   0.50   14.54    --   20.00  54.00-150.00   94
  4  ω    -73.00 -47.00   0.50   14.54    --   20.00  54.00  30.00   52
  5  ω    -11.00  54.00   0.50   14.54    --   20.00  54.00  30.00  130
  6  ω     57.00  83.00   0.50   14.54    --   20.00  54.00  30.00   52
  7  ω    -74.00 104.00   0.50   14.54    --   20.00  54.00 120.00  356
  8  ω    -66.00 -40.00   0.50   14.54    --   20.00  54.00 -90.00   52
  9  ω     67.00  92.00   0.50   14.54    --   20.00  54.00 -90.00   50
 10  ω    -71.00 -46.00   0.50   14.54    --   20.00  54.00   0.00   50
 11  ω     -5.00  35.00   0.50   14.54    --   20.00  54.00   0.00   80
 12  ω    -23.00  51.00   0.50   14.54    --   20.00  54.00-120.00  148
 13  ω    -65.00   1.00   0.50   14.54    --   20.00  54.00 -60.00  132
 14  ω     44.00  71.00   0.50   14.54    --   20.00  54.00 -60.00   54
 15  ω    -67.00 -18.00   0.50   14.54    --   20.00  54.00  90.00   98
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0657126000
_diffrn_orient_matrix_UB_12      -0.0011512000
_diffrn_orient_matrix_UB_13      0.0313116000
_diffrn_orient_matrix_UB_21      0.0214318000
_diffrn_orient_matrix_UB_22      -0.0033415000
_diffrn_orient_matrix_UB_23      -0.0895856000
_diffrn_orient_matrix_UB_31      0.0423337000
_diffrn_orient_matrix_UB_32      0.0809878000
_diffrn_orient_matrix_UB_33      -0.0032679000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.730
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                698
_reflns_number_total             723
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_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)'
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 
;
 Flack x determined using 293 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(12)
_refine_ls_extinction_coef       0.00142(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         723
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0126
_refine_ls_R_factor_gt           0.0109
_refine_ls_restrained_S_all      1.083
_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/[σ²(Fo²)+(0.0062P)²+0.1781P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0208
_refine_ls_wR_factor_ref         0.0210
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce Ce 0.35730(3) 0.38047(3) 0.250000 0.00888(7) Uani 1 2 d S T P . .
Ge Ge 0.666667 0.333333 0.51309(7) 0.00542(13) Uani 1 3 d S T P . .
Ga Ga 0.000000 0.19034(6) 0.000000 0.00761(11) Uani 1 2 d S T P . .
S S 0.01396(15) 0.32373(15) 0.250000 0.0120(3) Uani 1 2 d S T P . .
O1 O 0.1770(3) 0.1770(3) 0.000000 0.0111(7) Uani 1 2 d S T P . .
O2 O 0.5038(3) 0.3439(3) 0.4663(3) 0.0115(5) Uani 1 1 d . . . . .
O3 O 0.666667 0.333333 0.750000 0.032(2) Uani 1 6 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce Ce 3.7588(2) 7 ?
Ce Ce 3.7588(2) 7_556 ?
Ce Ge 3.4997(3) 10_554 ?
Ce Ge 3.4997(3) 7_556 ?
Ce S 3.2195(13) . ?
Ce S 3.1758(13) 2_665 ?
Ce O1 2.700(2) . ?
Ce O1 2.700(2) 4 ?
Ce O2 2.497(2) 7_556 ?
Ce O2 2.497(2) 10_554 ?
Ce O2 2.342(2) 4 ?
Ce O2 2.342(2) . ?
Ge O2 1.737(2) 2_655 ?
Ge O2 1.737(2) 3_665 ?
Ge O2 1.737(2) . ?
Ge O3 1.7706(5) . ?
Ga S 2.2662(8) 9 ?
Ga S 2.2662(8) . ?
Ga O1 1.8587(15) 2 ?
Ga O1 1.8587(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Ce Ce Ce 167.622(15) 7 7_556 ?
Ge Ce Ce 65.202(8) 7_556 7_556 ?
Ge Ce Ce 125.913(12) 7_556 7 ?
Ge Ce Ce 125.913(12) 10_554 7_556 ?
Ge Ce Ce 65.202(9) 10_554 7 ?
Ge Ce Ge 60.787(16) 7_556 10_554 ?
S Ce Ce 94.815(6) . 7_556 ?
S Ce Ce 89.843(3) 2_665 7 ?
S Ce Ce 94.815(6) . 7 ?
S Ce Ce 89.843(3) 2_665 7_556 ?
S Ce Ge 68.99(2) 2_665 10_554 ?
S Ce Ge 68.99(2) 2_665 7_556 ?
S Ce Ge 68.52(2) . 7_556 ?
S Ce Ge 68.52(2) . 10_554 ?
S Ce S 130.32(4) 2_665 . ?
O1 Ce Ce 45.88(5) . 7 ?
O1 Ce Ce 45.88(5) 4 7_556 ?
O1 Ce Ce 132.85(5) . 7_556 ?
O1 Ce Ce 132.85(5) 4 7 ?
O1 Ce Ge 88.83(3) 4 7_556 ?
O1 Ce Ge 132.841(14) . 7_556 ?
O1 Ce Ge 132.841(14) 4 10_554 ?
O1 Ce Ge 88.83(3) . 10_554 ?
O1 Ce S 66.92(3) 4 . ?
O1 Ce S 66.92(3) . . ?
O1 Ce S 135.70(5) 4 2_665 ?
O1 Ce S 135.70(5) . 2_665 ?
O1 Ce O1 87.60(10) . 4 ?
O2 Ce Ce 37.56(5) 7_556 7_556 ?
O2 Ce Ce 127.78(6) 4 7_556 ?
O2 Ce Ce 127.78(6) . 7 ?
O2 Ce Ce 153.64(5) 10_554 7_556 ?
O2 Ce Ce 40.53(6) 4 7 ?
O2 Ce Ce 37.56(5) 10_554 7 ?
O2 Ce Ce 153.64(5) 7_556 7 ?
O2 Ce Ce 40.54(6) . 7_556 ?
O2 Ce Ge 95.22(6) . 7_556 ?
O2 Ce Ge 88.54(5) 7_556 10_554 ?
O2 Ce Ge 142.14(6) 4 7_556 ?
O2 Ce Ge 142.14(6) . 10_554 ?
O2 Ce Ge 88.54(5) 10_554 7_556 ?
O2 Ce Ge 27.76(5) 10_554 10_554 ?
O2 Ce Ge 27.76(5) 7_556 7_556 ?
O2 Ce Ge 95.22(6) 4 10_554 ?
O2 Ce S 75.27(6) . 2_665 ?
O2 Ce S 77.87(6) 10_554 2_665 ?
O2 Ce S 75.27(6) 4 2_665 ?
O2 Ce S 132.92(6) . . ?
O2 Ce S 132.92(6) 4 . ?
O2 Ce S 76.51(6) 10_554 . ?
O2 Ce S 76.51(6) 7_556 . ?
O2 Ce S 77.87(6) 7_556 2_665 ?
O2 Ce O1 141.57(7) 7_556 . ?
O2 Ce O1 126.63(6) 4 4 ?
O2 Ce O1 68.96(7) 4 . ?
O2 Ce O1 66.90(7) 7_556 4 ?
O2 Ce O1 68.96(7) . 4 ?
O2 Ce O1 66.90(7) 10_554 . ?
O2 Ce O1 126.63(6) . . ?
O2 Ce O1 141.57(7) 10_554 4 ?
O2 Ce O2 87.31(11) 4 . ?
O2 Ce O2 71.84(9) 4 10_554 ?
O2 Ce O2 116.28(10) 7_556 10_554 ?
O2 Ce O2 149.42(11) 4 7_556 ?
O2 Ce O2 71.84(9) . 7_556 ?
O2 Ce O2 149.42(11) . 10_554 ?
Ce Ge Ce 96.662(11) 8_666 7_556 ?
Ce Ge Ce 96.664(10) 9_656 8_666 ?
Ce Ge Ce 96.663(11) 9_656 7_556 ?
O2 Ge Ce 120.88(8) 2_655 8_666 ?
O2 Ge Ce 122.36(8) . 8_666 ?
O2 Ge Ce 120.88(8) . 9_656 ?
O2 Ge Ce 120.88(8) 3_665 7_556 ?
O2 Ge Ce 122.37(8) 3_665 9_656 ?
O2 Ge Ce 42.02(8) . 7_556 ?
O2 Ge Ce 122.37(8) 2_655 7_556 ?
O2 Ge Ce 42.02(8) 2_655 9_656 ?
O2 Ge Ce 42.02(8) 3_665 8_666 ?
O2 Ge O2 116.05(5) 2_655 3_665 ?
O2 Ge O2 116.05(5) 3_665 . ?
O2 Ge O2 116.05(5) 2_655 . ?
O2 Ge O3 101.62(8) . . ?
O2 Ge O3 101.62(8) 3_665 . ?
O2 Ge O3 101.62(8) 2_655 . ?
O3 Ge Ce 59.606(8) . 7_556 ?
O3 Ge Ce 59.606(8) . 9_656 ?
O3 Ge Ce 59.606(8) . 8_666 ?
S Ga S 111.43(6) . 9 ?
O1 Ga S 105.48(6) . . ?
O1 Ga S 110.89(5) . 9 ?
O1 Ga S 105.48(6) 2 9 ?
O1 Ga S 110.89(5) 2 . ?
O1 Ga O1 112.81(18) 2 . ?
Ce S Ce 109.68(4) 3_565 . ?
Ga S Ce 124.37(3) . 3_565 ?
Ga S Ce 81.21(3) 4 . ?
Ga S Ce 81.21(3) . . ?
Ga S Ce 124.37(3) 4 3_565 ?
Ga S Ga 111.07(6) . 4 ?
Ce O1 Ce 88.25(10) . 7 ?
Ga O1 Ce 104.59(5) . . ?
Ga O1 Ce 112.73(5) 3 . ?
Ga O1 Ce 104.60(5) 3 7 ?
Ga O1 Ce 112.73(5) . 7 ?
Ga O1 Ga 127.19(18) 3 . ?
Ce O2 Ce 101.91(9) . 7_556 ?
Ge O2 Ce 110.22(11) . 7_556 ?
Ge O2 Ce 147.27(13) . . ?
Ge O3 Ge 180.0 4_556 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ce Ge O2 Ce -129.0(2) 9_656 . . . ?
Ce Ge O2 Ce 62.50(12) 9_656 . . 7_556 ?
Ce Ge O2 Ce -60.12(13) 8_666 . . 7_556 ?
Ce Ge O2 Ce 168.5(3) 7_556 . . . ?
Ce Ge O2 Ce 108.4(2) 8_666 . . . ?
S Ga O1 Ce 107.61(5) 9 . . . ?
S Ga O1 Ce 13.32(11) 9 . . 7 ?
S Ga O1 Ce -13.15(9) . . . . ?
S Ga O1 Ce -107.44(7) . . . 7 ?
S Ga O1 Ga 121.19(4) . . . 3 ?
S Ga O1 Ga -118.06(4) 9 . . 3 ?
O1 Ga O1 Ce 131.37(8) 2 . . 7 ?
O1 Ga O1 Ce -134.34(6) 2 . . . ?
O1 Ga O1 Ga 0.0 2 . . 3 ?
O2 Ge O2 Ce 110.34(16) 2_655 . . 7_556 ?
O2 Ge O2 Ce -108.12(16) 3_665 . . 7_556 ?
O2 Ge O2 Ce 60.4(3) 3_665 . . . ?
O2 Ge O2 Ce -81.2(2) 2_655 . . . ?
O3 Ge O2 Ce 169.6(2) . . . . ?
O3 Ge O2 Ce 1.11(11) . . . 7_556 ?

_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 1.350
_oxdiff_exptl_absorpt_empirical_full_min 0.862
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_306
_database_code_depnum_ccdc_archive 'CCDC 2449160'
loop_
_audit_author_name
_audit_author_address
'Yoshihiro Tsujimoto'
;National Institute for Materials Science
Japan
;
_audit_update_record             
;
2025-05-07 deposited with the CCDC.	2025-06-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT213_exp_306             
;
PROBLEM: Atom O3              has ADP max/min Ratio .....        4.2 oblate
RESPONSE: O3 atoms are strongly bound to two Ga atoms along the c axis but not to Pr atoms in the ab plane. Therefore, the displacement ellipsoid of O3 become significantly oblate.
;
# Added during the CSD deposition process: Wednesday 07 May 2025 05:12 AM
# end Validation Reply Form

_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)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Ga3 Ge2 O10 Pr3 S3'
_chemical_formula_sum            'Ga3 Ge2 O10 Pr3 S3'
_chemical_formula_weight         1033.25
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pr3 Ga3 Ge2 S3 O10'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_H-M_alt        'P -6 2 c'
_space_group_name_Hall           'P -6c -2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z+1/2'
'-y, x-y, -z+1/2'
'-x+y, -x, -z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'

_cell_length_a                   10.0921(7)
_cell_length_b                   10.0921(7)
_cell_length_c                   7.4251(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     654.93(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1991
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.3800
_cell_measurement_theta_min      3.5840
_shelx_estimated_absorpt_T_max   0.250
_shelx_estimated_absorpt_T_min   0.158
_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_absorpt_special_details   ?
_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_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -52.00 -26.00   0.50    4.08    --   20.00  54.00 150.00   52
  2  ω      9.00  47.00   0.50    4.08    --   20.00  54.00 150.00   76
  3  ω     76.00 102.00   0.50    4.08    --   20.00  54.00 150.00   52
  4  ω     80.00 105.00   0.50    4.08    --   20.00  54.00-180.00   50
  5  ω    -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       'ω 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_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_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_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_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+0.001xFc²λ³/sin(2θ)]^-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_R_factor_all          0.0136
_refine_ls_R_factor_gt           0.0128
_refine_ls_restrained_S_all      0.977
_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/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0234
_refine_ls_wR_factor_ref         0.0236
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr Pr 0.35754(5) 0.38139(6) 0.250000 0.00797(13) Uani 1 2 d S T P . .
Ge Ge 0.666667 0.333333 0.51145(11) 0.0039(2) Uani 1 3 d S T P . .
Ga Ga 0.000000 0.19057(10) 0.000000 0.0070(2) Uani 1 2 d S T P . .
S S 0.0163(2) 0.3260(2) 0.250000 0.0118(5) Uani 1 2 d S T P . .
O1 O 0.1764(6) 0.1764(6) 0.000000 0.0135(15) Uani 1 2 d S T P . .
O2 O 0.5033(4) 0.3433(4) 0.4658(5) 0.0106(9) Uani 1 1 d . . . . .
O3 O 0.666667 0.333333 0.750000 0.036(4) Uani 1 6 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr Pr 3.7359(3) 7 ?
Pr Pr 3.7359(3) 7_556 ?
Pr Ge 3.4913(6) 7_556 ?
Pr Ge 3.4913(6) 10_554 ?
Pr S 3.201(2) . ?
Pr S 3.156(2) 2_665 ?
Pr O1 2.699(4) 4 ?
Pr O1 2.699(4) . ?
Pr O2 2.333(4) . ?
Pr O2 2.333(4) 4 ?
Pr O2 2.483(4) 10_554 ?
Pr O2 2.483(4) 7_556 ?
Ge O2 1.735(4) 2_655 ?
Ge O2 1.735(4) . ?
Ge O2 1.735(4) 3_665 ?
Ge O3 1.7712(8) . ?
Ga S 2.2618(13) . ?
Ga S 2.2618(13) 9 ?
Ga O1 1.856(3) . ?
Ga O1 1.856(3) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Pr Pr Pr 167.18(3) 7 7_556 ?
Ge Pr Pr 126.20(2) 10_554 7_556 ?
Ge Pr Pr 65.311(14) 7_556 7_556 ?
Ge Pr Pr 126.20(2) 7_556 7 ?
Ge Pr Pr 65.311(13) 10_554 7 ?
Ge Pr Ge 60.97(3) 7_556 10_554 ?
S Pr Pr 94.997(10) . 7 ?
S Pr Pr 94.997(10) . 7_556 ?
S Pr Pr 89.866(4) 2_665 7_556 ?
S Pr Pr 89.866(4) 2_665 7 ?
S Pr Ge 68.84(3) 2_665 10_554 ?
S Pr Ge 68.36(3) . 7_556 ?
S Pr Ge 68.84(3) 2_665 7_556 ?
S Pr Ge 68.36(3) . 10_554 ?
S Pr S 129.90(6) 2_665 . ?
O1 Pr Pr 46.21(9) 4 7_556 ?
O1 Pr Pr 132.44(8) 4 7 ?
O1 Pr Pr 46.21(9) . 7 ?
O1 Pr Pr 132.44(8) . 7_556 ?
O1 Pr Ge 132.93(2) . 7_556 ?
O1 Pr Ge 89.05(5) . 10_554 ?
O1 Pr Ge 89.05(5) 4 7_556 ?
O1 Pr Ge 132.93(2) 4 10_554 ?
O1 Pr S 66.98(5) . . ?
O1 Pr S 136.06(9) . 2_665 ?
O1 Pr S 66.98(5) 4 . ?
O1 Pr S 136.06(9) 4 2_665 ?
O1 Pr O1 86.89(17) 4 . ?
O2 Pr Pr 40.60(10) 4 7 ?
O2 Pr Pr 127.27(10) 4 7_556 ?
O2 Pr Pr 127.27(10) . 7 ?
O2 Pr Pr 153.92(9) 7_556 7 ?
O2 Pr Pr 37.70(9) 7_556 7_556 ?
O2 Pr Pr 153.92(9) 10_554 7_556 ?
O2 Pr Pr 40.60(10) . 7_556 ?
O2 Pr Pr 37.70(9) 10_554 7 ?
O2 Pr Ge 142.56(10) 4 7_556 ?
O2 Pr Ge 95.58(10) 4 10_554 ?
O2 Pr Ge 27.74(9) 10_554 10_554 ?
O2 Pr Ge 27.74(9) 7_556 7_556 ?
O2 Pr Ge 88.70(9) 7_556 10_554 ?
O2 Pr Ge 88.70(9) 10_554 7_556 ?
O2 Pr Ge 95.58(10) . 7_556 ?
O2 Pr Ge 142.56(10) . 10_554 ?
O2 Pr S 75.69(10) 4 2_665 ?
O2 Pr S 133.08(10) 4 . ?
O2 Pr S 76.28(9) 10_554 . ?
O2 Pr S 77.95(9) 7_556 2_665 ?
O2 Pr S 76.28(9) 7_556 . ?
O2 Pr S 77.95(9) 10_554 2_665 ?
O2 Pr S 133.08(10) . . ?
O2 Pr S 75.69(10) . 2_665 ?
O2 Pr O1 67.07(12) 7_556 4 ?
O2 Pr O1 141.22(12) 7_556 . ?
O2 Pr O1 67.07(12) 10_554 . ?
O2 Pr O1 141.22(11) 10_554 4 ?
O2 Pr O1 125.96(10) 4 4 ?
O2 Pr O1 125.96(10) . . ?
O2 Pr O1 69.07(12) 4 . ?
O2 Pr O1 69.07(12) . 4 ?
O2 Pr O2 86.7(2) . 4 ?
O2 Pr O2 72.26(16) . 7_556 ?
O2 Pr O2 149.62(16) 4 7_556 ?
O2 Pr O2 72.26(16) 4 10_554 ?
O2 Pr O2 116.42(18) 7_556 10_554 ?
O2 Pr O2 149.62(16) . 10_554 ?
Pr Ge Pr 96.542(17) 8_666 7_556 ?
Pr Ge Pr 96.542(17) 9_656 8_666 ?
Pr Ge Pr 96.542(17) 9_656 7_556 ?
O2 Ge Pr 120.51(13) 2_655 8_666 ?
O2 Ge Pr 120.51(13) 3_665 7_556 ?
O2 Ge Pr 41.78(12) . 7_556 ?
O2 Ge Pr 41.78(12) 3_665 8_666 ?
O2 Ge Pr 41.78(12) 2_655 9_656 ?
O2 Ge Pr 122.39(13) . 8_666 ?
O2 Ge Pr 122.39(13) 3_665 9_656 ?
O2 Ge Pr 120.51(13) . 9_656 ?
O2 Ge Pr 122.39(13) 2_655 7_556 ?
O2 Ge O2 116.27(8) 2_655 3_665 ?
O2 Ge O2 116.27(8) 3_665 . ?
O2 Ge O2 116.27(8) 2_655 . ?
O2 Ge O3 101.28(12) 2_655 . ?
O2 Ge O3 101.28(12) . . ?
O2 Ge O3 101.28(12) 3_665 . ?
O3 Ge Pr 59.514(13) . 8_666 ?
O3 Ge Pr 59.514(13) . 7_556 ?
O3 Ge Pr 59.514(13) . 9_656 ?
S Ga S 110.80(10) 9 . ?
O1 Ga S 105.30(10) . . ?
O1 Ga S 105.30(10) 2 9 ?
O1 Ga S 111.62(9) 2 . ?
O1 Ga S 111.62(9) . 9 ?
O1 Ga O1 112.3(3) . 2 ?
Pr S Pr 110.10(6) 3_565 . ?
Ga S Pr 81.51(5) . . ?
Ga S Pr 81.51(5) 4 . ?
Ga S Pr 124.69(5) . 3_565 ?
Ga S Pr 124.69(5) 4 3_565 ?
Ga S Ga 110.31(10) . 4 ?
Pr O1 Pr 87.58(17) . 7 ?
Ga O1 Pr 104.42(9) 3 7 ?
Ga O1 Pr 112.81(9) 3 . ?
Ga O1 Pr 104.42(9) . . ?
Ga O1 Pr 112.81(9) . 7 ?
Ga O1 Ga 127.7(3) 3 . ?
Pr O2 Pr 101.70(15) . 7_556 ?
Ge O2 Pr 147.1(2) . . ?
Ge O2 Pr 110.48(17) . 7_556 ?
Ge O3 Ge 180.0 4_556 . ?

_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

_vrf_PLAT213_ALERT_2_B           
;
Atom O3 has ADP max/min Ratio .....        4.2 oblate

RESPONSE:O3 atoms are strongly bound to two Ga atoms along the c axis
but not to Pr atoms in the ab plane. Therefore, the displacement
ellipsoid of O3 become significantly oblate.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_La3Ga3Ge2S3O10
_database_code_depnum_ccdc_archive 'CCDC 2449238'
loop_
_audit_author_name
_audit_author_address
'Yoshihiro Tsujimoto'
;National Institute for Materials Science
Japan
;
_audit_update_record             
;
2025-05-07 deposited with the CCDC.	2025-06-12 downloaded from the CCDC.
;
_audit_creation_date             2025-04-25
_audit_creation_method           
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Ga3 Ge2 La3 O10 S3'
_chemical_formula_sum            'Ga3 Ge2 La3 O10 S3'
_chemical_formula_weight         1027.25
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'La Ga Ge S O'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_H-M_alt        'P -6 2 c'
_space_group_name_Hall           'P -6c -2c'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z+1/2'
'-y, x-y, -z+1/2'
'-x+y, -x, -z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'

_cell_length_a                   10.1701(4)
_cell_length_b                   10.1701(4)
_cell_length_c                   7.5198(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     673.58(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6837
_cell_measurement_temperature    297.15
_cell_measurement_theta_max      30.5300
_cell_measurement_theta_min      3.5340
_shelx_estimated_absorpt_T_max   0.427
_shelx_estimated_absorpt_T_min   0.259
_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_absorpt_special_details   ?
_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_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      6.00 110.00   0.50   15.00    --   20.00  54.00 -90.00  208
  2  ω    -71.00 -39.00   0.50   15.00    --   20.00  54.00 120.00   64
  3  ω    -22.00  98.00   0.50   15.00    --   20.00  54.00 120.00  240
  4  ω    -72.00 110.00   0.50   15.00    --   20.00  54.00  60.00  364
  5  ω    -20.00  54.00   0.50   15.00    --   20.00  54.00-180.00  148
  6  ω     70.00  95.00   0.50   15.00    --   20.00  54.00-180.00   50
  7  ω    -73.00 -44.00   0.50   15.00    --   20.00  54.00 -30.00   58
  8  ω     20.00  45.00   0.50   15.00    --   20.00  54.00 -30.00   50
  9  ω     75.00 100.00   0.50   15.00    --   20.00  54.00 -30.00   50
 10  ω    -73.00 -38.00   0.50   15.00    --   20.00  54.00-150.00   70
 11  ω     -6.00  26.00   0.50   15.00    --   20.00  54.00-150.00   64
 12  ω     57.00  82.00   0.50   15.00    --   20.00  54.00-150.00   50
 13  ω    -59.00 -33.00   0.50   15.00    --   20.00  54.00 150.00   52
 14  ω     62.00  87.00   0.50   15.00    --   20.00  54.00  30.00   50
 15  ω    -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       'ω 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_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_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_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_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+0.001xFc²λ³/sin(2θ)]^-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_R_factor_all          0.0114
_refine_ls_R_factor_gt           0.0109
_refine_ls_restrained_S_all      1.107
_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/[σ²(Fo²)+(0.0100P)²+0.3488P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0251
_refine_ls_wR_factor_ref         0.0252
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La01 La 0.35751(3) 0.38034(3) 0.250000 0.00771(8) Uani 1 2 d S T P . .
Ge02 Ge 0.666667 0.333333 0.51367(7) 0.00446(13) Uani 1 3 d S T P . .
Ga03 Ga 0.000000 0.18935(5) 0.000000 0.00652(12) Uani 1 2 d S T P . .
S004 S 0.01248(14) 0.32093(14) 0.250000 0.0106(2) Uani 1 2 d S T P . .
O003 O 0.666667 0.333333 0.750000 0.033(2) Uani 1 6 d S T P . .
O001 O 0.1757(3) 0.1757(3) 0.000000 0.0089(7) Uani 1 2 d S T P . .
O002 O 0.5052(3) 0.3439(3) 0.4667(3) 0.0111(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La01 La01 3.78134(16) 7 ?
La01 La01 3.78134(17) 7_556 ?
La01 Ge02 3.5235(4) 7_556 ?
La01 Ge02 3.5235(4) 10_554 ?
La01 S004 3.2190(13) 2_665 ?
La01 S004 3.2493(12) . ?
La01 O001 2.727(2) . ?
La01 O001 2.727(2) 4 ?
La01 O002 2.368(2) 4 ?
La01 O002 2.368(2) . ?
La01 O002 2.519(3) 10_554 ?
La01 O002 2.519(3) 7_556 ?
Ge02 O003 1.7772(5) . ?
Ge02 O002 1.735(2) 2_655 ?
Ge02 O002 1.735(2) . ?
Ge02 O002 1.735(2) 3_665 ?
Ga03 S004 2.2740(7) 9 ?
Ga03 S004 2.2740(7) . ?
Ga03 O001 1.8602(15) . ?
Ga03 O001 1.8602(15) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
La01 La01 La01 167.792(16) 7 7_556 ?
Ge02 La01 La01 125.737(12) 7_556 7 ?
Ge02 La01 La01 125.737(12) 10_554 7_556 ?
Ge02 La01 La01 65.229(9) 7_556 7_556 ?
Ge02 La01 La01 65.229(9) 10_554 7 ?
Ge02 La01 Ge02 60.582(16) 7_556 10_554 ?
S004 La01 La01 89.827(3) 2_665 7 ?
S004 La01 La01 89.827(2) 2_665 7_556 ?
S004 La01 La01 94.722(6) . 7_556 ?
S004 La01 La01 94.722(6) . 7 ?
S004 La01 Ge02 69.133(19) 2_665 10_554 ?
S004 La01 Ge02 68.81(2) . 7_556 ?
S004 La01 Ge02 69.133(19) 2_665 7_556 ?
S004 La01 Ge02 68.81(2) . 10_554 ?
S004 La01 S004 130.89(4) 2_665 . ?
O001 La01 La01 46.10(5) 4 7_556 ?
O001 La01 La01 132.66(5) 4 7 ?
O001 La01 La01 46.10(5) . 7 ?
O001 La01 La01 132.66(5) . 7_556 ?
O001 La01 Ge02 88.98(3) 4 7_556 ?
O001 La01 Ge02 132.655(14) 4 10_554 ?
O001 La01 Ge02 132.655(14) . 7_556 ?
O001 La01 Ge02 88.98(3) . 10_554 ?
O001 La01 S004 66.48(3) 4 . ?
O001 La01 S004 135.91(5) . 2_665 ?
O001 La01 S004 66.48(3) . . ?
O001 La01 S004 135.91(5) 4 2_665 ?
O001 La01 O001 87.17(10) . 4 ?
O002 La01 La01 127.71(6) . 7 ?
O002 La01 La01 153.17(6) 7_556 7 ?
O002 La01 La01 37.87(6) 7_556 7_556 ?
O002 La01 La01 37.87(6) 10_554 7 ?
O002 La01 La01 40.77(6) 4 7 ?
O002 La01 La01 127.71(6) 4 7_556 ?
O002 La01 La01 153.17(5) 10_554 7_556 ?
O002 La01 La01 40.77(6) . 7_556 ?
O002 La01 Ge02 142.03(6) 4 7_556 ?
O002 La01 Ge02 88.04(6) 10_554 7_556 ?
O002 La01 Ge02 27.47(6) 7_556 7_556 ?
O002 La01 Ge02 88.04(6) 7_556 10_554 ?
O002 La01 Ge02 27.47(6) 10_554 10_554 ?
O002 La01 Ge02 95.39(6) . 7_556 ?
O002 La01 Ge02 95.39(6) 4 10_554 ?
O002 La01 Ge02 142.03(7) . 10_554 ?
O002 La01 S004 75.03(7) . 2_665 ?
O002 La01 S004 76.55(6) 10_554 . ?
O002 La01 S004 77.83(6) 7_556 2_665 ?
O002 La01 S004 77.83(6) 10_554 2_665 ?
O002 La01 S004 76.55(6) 7_556 . ?
O002 La01 S004 75.03(7) 4 2_665 ?
O002 La01 S004 132.96(6) . . ?
O002 La01 S004 132.96(6) 4 . ?
O002 La01 O001 67.33(7) 10_554 . ?
O002 La01 O001 69.34(7) . 4 ?
O002 La01 O001 141.32(7) 10_554 4 ?
O002 La01 O001 126.61(7) 4 4 ?
O002 La01 O001 126.61(7) . . ?
O002 La01 O001 69.34(7) 4 . ?
O002 La01 O001 67.33(7) 7_556 4 ?
O002 La01 O001 141.32(7) 7_556 . ?
O002 La01 O002 115.49(11) 7_556 10_554 ?
O002 La01 O002 149.32(11) 4 7_556 ?
O002 La01 O002 72.28(10) 4 10_554 ?
O002 La01 O002 87.01(12) . 4 ?
O002 La01 O002 149.32(11) . 10_554 ?
O002 La01 O002 72.28(10) . 7_556 ?
La01 Ge02 La01 96.799(11) 8_666 7_556 ?
La01 Ge02 La01 96.799(11) 9_656 8_666 ?
La01 Ge02 La01 96.799(11) 9_656 7_556 ?
O003 Ge02 La01 59.709(8) . 8_666 ?
O003 Ge02 La01 59.709(8) . 7_556 ?
O003 Ge02 La01 59.709(8) . 9_656 ?
O002 Ge02 La01 120.94(9) 2_655 8_666 ?
O002 Ge02 La01 122.43(9) 3_665 9_656 ?
O002 Ge02 La01 42.04(8) 3_665 8_666 ?
O002 Ge02 La01 42.04(8) 2_655 9_656 ?
O002 Ge02 La01 122.43(9) 2_655 7_556 ?
O002 Ge02 La01 120.94(9) 3_665 7_556 ?
O002 Ge02 La01 120.95(9) . 9_656 ?
O002 Ge02 La01 122.43(9) . 8_666 ?
O002 Ge02 La01 42.04(8) . 7_556 ?
O002 Ge02 O003 101.74(9) 2_655 . ?
O002 Ge02 O003 101.74(9) 3_665 . ?
O002 Ge02 O003 101.74(9) . . ?
O002 Ge02 O002 115.97(6) 2_655 . ?
O002 Ge02 O002 115.97(6) 2_655 3_665 ?
O002 Ge02 O002 115.97(6) 3_665 . ?
S004 Ga03 S004 111.81(5) 9 . ?
O001 Ga03 S004 110.56(5) 2 . ?
O001 Ga03 S004 105.71(6) . . ?
O001 Ga03 S004 110.56(5) . 9 ?
O001 Ga03 S004 105.71(6) 2 9 ?
O001 Ga03 O001 112.60(19) . 2 ?
La01 S004 La01 109.11(4) 3_565 . ?
Ga03 S004 La01 81.18(3) 4 . ?
Ga03 S004 La01 124.17(3) 4 3_565 ?
Ga03 S004 La01 81.18(3) . . ?
Ga03 S004 La01 124.17(3) . 3_565 ?
Ga03 S004 Ga03 111.52(5) . 4 ?
Ge02 O003 Ge02 180.0 . 4_556 ?
La01 O001 La01 87.79(10) . 7 ?
Ga03 O001 La01 112.67(5) 3 . ?
Ga03 O001 La01 104.66(5) . . ?
Ga03 O001 La01 104.67(5) 3 7 ?
Ga03 O001 La01 112.67(5) . 7 ?
Ga03 O001 Ga03 127.40(19) 3 . ?
La01 O002 La01 101.36(9) . 7_556 ?
Ge02 O002 La01 110.50(12) . 7_556 ?
Ge02 O002 La01 147.56(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
La01 Ge02 O002 La01 -128.7(2) 9_656 . . . ?
La01 Ge02 O002 La01 -60.31(13) 8_666 . . 7_556 ?
La01 Ge02 O002 La01 168.6(4) 7_556 . . . ?
La01 Ge02 O002 La01 62.68(13) 9_656 . . 7_556 ?
La01 Ge02 O002 La01 108.3(2) 8_666 . . . ?
S004 Ga03 O001 La01 -13.73(9) . . . . ?
S004 Ga03 O001 La01 13.66(11) 9 . . 7 ?
S004 Ga03 O001 La01 107.45(5) 9 . . . ?
S004 Ga03 O001 La01 -107.52(7) . . . 7 ?
S004 Ga03 O001 Ga03 -118.00(4) 9 . . 3 ?
S004 Ga03 O001 Ga03 120.82(4) . . . 3 ?
O003 Ge02 O002 La01 1.11(12) . . . 7_556 ?
O003 Ge02 O002 La01 169.7(2) . . . . ?
O001 Ga03 O001 La01 -134.55(6) 2 . . . ?
O001 Ga03 O001 La01 131.66(8) 2 . . 7 ?
O001 Ga03 O001 Ga03 0.0 2 . . 3 ?
O002 Ge02 O002 La01 -108.29(17) 3_665 . . 7_556 ?
O002 Ge02 O002 La01 -80.9(3) 2_655 . . . ?
O002 Ge02 O002 La01 60.3(3) 3_665 . . . ?
O002 Ge02 O002 La01 110.52(17) 2_655 . . 7_556 ?

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_357_auto
_audit_block_doi                 10.25505/fiz.icsd.cc2n6mq7
_database_code_depnum_ccdc_archive 'CCDC 2449239'
loop_
_audit_author_name
_audit_author_address
'Yoshihiro Tsujimoto'
;National Institute for Materials Science
Japan
;
_audit_update_record             
;
2025-05-07 deposited with the CCDC.	2025-06-12 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT213_exp_357_auto        
;
PROBLEM: Atom O3              has ADP max/min Ratio .....        4.1 oblate
RESPONSE: O3 atoms are strongly bound to two Ga atoms along the c axis  but not to Nd atoms in the ab plane. Therefore, the displacement  ellipsoid of O3 become significantly oblate.
;
# Added during the CSD deposition process: Wednesday 07 May 2025 05:07 AM
# end Validation Reply Form

_audit_creation_date             2025-05-01
_audit_creation_method           
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Ga3 Ge2 Nd3 O10 S3'
_chemical_formula_sum            'Ga3 Ge2 Nd3 O10 S3'
_chemical_formula_weight         1043.24
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Nd3 Ga3 Ge2 S3 O10'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_H-M_alt        'P -6 2 c'
_space_group_name_Hall           'P -6c -2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z+1/2'
'-y, x-y, -z+1/2'
'-x+y, -x, -z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'

_cell_length_a                   10.0682(5)
_cell_length_b                   10.0682(5)
_cell_length_c                   7.3802(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     647.89(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1637
_cell_measurement_temperature    294
_cell_measurement_theta_max      30.2070
_cell_measurement_theta_min      3.5950
_shelx_estimated_absorpt_T_max   0.517
_shelx_estimated_absorpt_T_min   0.174
_exptl_absorpt_coefficient_mu    23.023
_exptl_absorpt_correction_T_max  0.569
_exptl_absorpt_correction_T_min  0.246
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear pinkish pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    5.348
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             930
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -3 -5 0.0446
-2 -3 0 0.0131
2 3 0 0.0213
-1 2 5 0.0451
2 -5 -1 0.0206
-9 4 0 0.0165
7 -5 0 0.0108

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.117
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.033
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0021 -2.9997 -4.9990 0.3720 0.2224 0.2990
-1.9971 -3.0030 0.0009 -0.0988 -0.0374 0.3387
1.9971 3.0030 -0.0009 0.0988 0.0374 -0.3387
-1.0009 1.9989 4.9988 -0.4001 -0.1987 -0.2263
2.0063 -5.0031 -1.0018 -0.0356 0.2458 0.2711
-9.0078 4.0007 0.0069 0.0459 -0.5816 0.2520
7.0083 -5.0021 -0.0056 -0.0886 0.4969 -0.0587

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2520
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.607
_diffrn_reflns_theta_min         2.336
_diffrn_ambient_temperature      294
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     21.00 106.00   0.50   11.46    --   20.00  54.00 -60.00  170
  2  ω    -49.00  32.00   0.50   11.46    --   20.00  54.00   0.00  162
  3  ω     66.00  91.00   0.50   11.46    --   20.00  54.00   0.00   50
  4  ω    -74.00 -35.00   0.50   11.46    --   20.00  54.00 -60.00   78
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0072849000
_diffrn_orient_matrix_UB_12      0.0280219000
_diffrn_orient_matrix_UB_13      -0.0897784000
_diffrn_orient_matrix_UB_21      0.0540916000
_diffrn_orient_matrix_UB_22      -0.0235378000
_diffrn_orient_matrix_UB_23      -0.0195132000
_diffrn_orient_matrix_UB_31      -0.0602869000
_diffrn_orient_matrix_UB_32      -0.0727003000
_diffrn_orient_matrix_UB_33      -0.0282795000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.632
_reflns_Friedel_fraction_full    0.937
_reflns_Friedel_fraction_max     0.833
_reflns_number_gt                622
_reflns_number_total             656
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_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  (Sheldrick, 2015)'
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details 
;
 Flack x determined using 239 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_extinction_coef       0.0117(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         656
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0190
_refine_ls_restrained_S_all      1.119
_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/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0328
_refine_ls_wR_factor_ref         0.0334
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd Nd 0.35688(5) 0.38212(6) 0.250000 0.00931(13) Uani 1 2 d S T P . .
Ge Ge 0.666667 0.333333 0.51012(12) 0.0056(2) Uani 1 3 d S T P . .
Ga Ga 0.000000 0.19118(10) 0.000000 0.0077(2) Uani 1 2 d S T P . .
S S 0.0183(3) 0.3287(3) 0.250000 0.0122(5) Uani 1 2 d S T P . .
O1 O 0.1777(6) 0.1777(6) 0.000000 0.0120(14) Uani 1 2 d S T P . .
O2 O 0.5030(5) 0.3436(5) 0.4640(5) 0.0115(9) Uani 1 1 d . . . . .
O3 O 0.666667 0.333333 0.750000 0.034(4) Uani 1 6 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd Nd 3.7162(3) 7 ?
Nd Nd 3.7162(3) 7_556 ?
Nd Ge 3.4753(6) 10_554 ?
Nd Ge 3.4753(6) 7_556 ?
Nd S 3.175(2) . ?
Nd S 3.131(2) 2_665 ?
Nd O1 2.680(5) . ?
Nd O1 2.680(5) 4 ?
Nd O2 2.473(4) 7_556 ?
Nd O2 2.473(4) 10_554 ?
Nd O2 2.320(4) 4 ?
Nd O2 2.320(4) . ?
Ge O2 1.735(4) 2_655 ?
Ge O2 1.735(4) 3_665 ?
Ge O2 1.735(4) . ?
Ge O3 1.7704(9) . ?
Ga S 2.2585(14) 9 ?
Ga S 2.2585(14) . ?
Ga O1 1.861(3) 2 ?
Ga O1 1.861(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Nd Nd Nd 166.40(3) 7 7_556 ?
Ge Nd Nd 65.525(15) 7_556 7_556 ?
Ge Nd Nd 126.68(2) 7_556 7 ?
Ge Nd Nd 126.68(2) 10_554 7_556 ?
Ge Nd Nd 65.525(15) 10_554 7 ?
Ge Nd Ge 61.25(3) 7_556 10_554 ?
S Nd Nd 95.322(11) . 7_556 ?
S Nd Nd 89.869(5) 2_665 7 ?
S Nd Nd 95.322(11) . 7 ?
S Nd Nd 89.869(5) 2_665 7_556 ?
S Nd Ge 68.71(4) 2_665 10_554 ?
S Nd Ge 68.71(4) 2_665 7_556 ?
S Nd Ge 68.25(4) . 7_556 ?
S Nd Ge 68.25(4) . 10_554 ?
S Nd S 129.54(7) 2_665 . ?
O1 Nd Nd 46.10(9) . 7 ?
O1 Nd Nd 46.10(9) 4 7_556 ?
O1 Nd Nd 132.38(9) . 7_556 ?
O1 Nd Nd 132.38(9) 4 7 ?
O1 Nd Ge 89.15(5) 4 7_556 ?
O1 Nd Ge 133.37(3) . 7_556 ?
O1 Nd Ge 133.37(3) 4 10_554 ?
O1 Nd Ge 89.15(5) . 10_554 ?
O1 Nd S 67.45(6) 4 . ?
O1 Nd S 67.45(6) . . ?
O1 Nd S 135.95(9) 4 2_665 ?
O1 Nd S 135.95(9) . 2_665 ?
O1 Nd O1 87.03(19) . 4 ?
O2 Nd Nd 37.69(10) 7_556 7_556 ?
O2 Nd Nd 126.44(11) 4 7_556 ?
O2 Nd Nd 126.44(11) . 7 ?
O2 Nd Nd 154.60(10) 10_554 7_556 ?
O2 Nd Nd 40.68(10) 4 7 ?
O2 Nd Nd 37.69(10) 10_554 7 ?
O2 Nd Nd 154.60(10) 7_556 7 ?
O2 Nd Nd 40.68(10) . 7_556 ?
O2 Nd Ge 95.82(11) . 7_556 ?
O2 Nd Ge 89.21(10) 7_556 10_554 ?
O2 Nd Ge 142.67(11) 4 7_556 ?
O2 Nd Ge 142.67(11) . 10_554 ?
O2 Nd Ge 89.21(10) 10_554 7_556 ?
O2 Nd Ge 27.96(10) 10_554 10_554 ?
O2 Nd Ge 27.96(10) 7_556 7_556 ?
O2 Nd Ge 95.82(11) 4 10_554 ?
O2 Nd S 75.70(11) . 2_665 ?
O2 Nd S 77.89(10) 10_554 2_665 ?
O2 Nd S 75.70(11) 4 2_665 ?
O2 Nd S 133.54(10) . . ?
O2 Nd S 133.54(10) 4 . ?
O2 Nd S 76.44(10) 10_554 . ?
O2 Nd S 76.44(10) 7_556 . ?
O2 Nd S 77.89(10) 7_556 2_665 ?
O2 Nd O1 141.65(13) 7_556 . ?
O2 Nd O1 125.46(11) 4 4 ?
O2 Nd O1 69.05(13) 4 . ?
O2 Nd O1 66.99(13) 7_556 4 ?
O2 Nd O1 69.05(13) . 4 ?
O2 Nd O1 66.99(13) 10_554 . ?
O2 Nd O1 125.46(11) . . ?
O2 Nd O1 141.65(13) 10_554 4 ?
O2 Nd O2 85.8(2) 4 . ?
O2 Nd O2 72.31(18) 4 10_554 ?
O2 Nd O2 117.15(19) 7_556 10_554 ?
O2 Nd O2 149.12(18) 4 7_556 ?
O2 Nd O2 72.31(18) . 7_556 ?
O2 Nd O2 149.12(18) . 10_554 ?
Nd Ge Nd 96.358(19) 8_666 7_556 ?
Nd Ge Nd 96.358(19) 9_656 8_666 ?
Nd Ge Nd 96.358(19) 9_656 7_556 ?
O2 Ge Nd 120.66(14) 2_655 8_666 ?
O2 Ge Nd 122.24(14) . 8_666 ?
O2 Ge Nd 120.66(14) . 9_656 ?
O2 Ge Nd 120.66(14) 3_665 7_556 ?
O2 Ge Nd 122.24(14) 3_665 9_656 ?
O2 Ge Nd 41.94(13) . 7_556 ?
O2 Ge Nd 122.24(14) 2_655 7_556 ?
O2 Ge Nd 41.94(13) 2_655 9_656 ?
O2 Ge Nd 41.94(13) 3_665 8_666 ?
O2 Ge O2 116.26(9) 2_655 3_665 ?
O2 Ge O2 116.26(9) 3_665 . ?
O2 Ge O2 116.26(9) 2_655 . ?
O2 Ge O3 101.30(13) . . ?
O2 Ge O3 101.30(13) 3_665 . ?
O2 Ge O3 101.30(13) 2_655 . ?
O3 Ge Nd 59.375(14) . 7_556 ?
O3 Ge Nd 59.375(14) . 9_656 ?
O3 Ge Nd 59.375(14) . 8_666 ?
S Ga S 110.16(10) . 9 ?
O1 Ga S 104.96(11) . . ?
O1 Ga S 112.06(10) . 9 ?
O1 Ga S 104.96(11) 2 9 ?
O1 Ga S 112.06(10) 2 . ?
O1 Ga O1 112.8(4) 2 . ?
Nd S Nd 110.46(7) 3_565 . ?
Ga S Nd 125.01(5) . 3_565 ?
Ga S Nd 81.67(6) 4 . ?
Ga S Nd 81.67(6) . . ?
Ga S Nd 125.01(5) 4 3_565 ?
Ga S Ga 109.56(10) . 4 ?
Nd O1 Nd 87.81(19) 7 . ?
Ga O1 Nd 113.19(9) . 7 ?
Ga O1 Nd 104.28(9) 3 7 ?
Ga O1 Nd 113.19(9) 3 . ?
Ga O1 Nd 104.28(9) . . ?
Ga O1 Ga 127.2(4) 3 . ?
Nd O2 Nd 101.63(17) . 7_556 ?
Ge O2 Nd 110.10(18) . 7_556 ?
Ge O2 Nd 147.6(2) . . ?
Ge O3 Ge 180.0 . 4_556 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Nd Ge O2 Nd -130.5(4) 9_656 . . . ?
Nd Ge O2 Nd 62.1(2) 9_656 . . 7_556 ?
Nd Ge O2 Nd -59.6(2) 8_666 . . 7_556 ?
Nd Ge O2 Nd 167.3(6) 7_556 . . . ?
Nd Ge O2 Nd 107.7(4) 8_666 . . . ?
S Ga O1 Nd 13.3(2) 9 . . 7 ?
S Ga O1 Nd 107.10(8) 9 . . . ?
S Ga O1 Nd -106.25(13) . . . 7 ?
S Ga O1 Nd -12.46(17) . . . . ?
S Ga O1 Ga 122.27(7) . . . 3 ?
S Ga O1 Ga -118.18(9) 9 . . 3 ?
O1 Ga O1 Nd -134.72(12) 2 . . . ?
O1 Ga O1 Nd 131.49(15) 2 . . 7 ?
O1 Ga O1 Ga 0.0 2 . . 3 ?
O2 Ge O2 Nd 109.9(3) 2_655 . . 7_556 ?
O2 Ge O2 Nd -107.6(3) 3_665 . . 7_556 ?
O2 Ge O2 Nd 59.8(5) 3_665 . . . ?
O2 Ge O2 Nd -82.7(4) 2_655 . . . ?
O3 Ge O2 Nd 168.5(4) . . . . ?
O3 Ge O2 Nd 1.18(19) . . . 7_556 ?

_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 1.218
_oxdiff_exptl_absorpt_empirical_full_min 0.762

_vrf_PLAT213_ALERT_2_B           
;
Atom O3 has ADP max/min Ratio .....        4.1 oblate

RESPONSE:O3 atoms are strongly bound to two Ga atoms along the c axis 
but not to Nd atoms in the ab plane. Therefore, the displacement 
ellipsoid of O3 become significantly oblate.
;
