Exploring new horizons in mid-to-far infrared nonlinear optical crystals: the significant potential of trigonal pyramidal [TeS<sub>3</sub>]<sup>2-</sup> functional units.
Zhang, Bo; Zhou, Sheng-Hua; Li, Bing-Xuan; Wu, Xin-Tao; Lin, Hua; Zhu, Qi-Long; Chemical science 16 (2025) 3218–3227; doi:10.1039/d4sc07322c

data_1573678
_publ_section_title
;
 Exploring new horizons in mid-to-far infrared nonlinear optical crystals:
 the significant potential of trigonal pyramidal
 [TeS<sub>3</sub>]<sup>2-</sup> functional units.
;
_journal_issue                   7
_journal_name_full               'Chemical science'
_journal_page_first              3218
_journal_page_last               3227
_journal_paper_doi               10.1039/d4sc07322c
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'Cu10.002 S13 Te4'
_chemical_formula_sum            'Cu10 S13 Te4'
_chemical_formula_weight         1562.58
_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_Hall           'I -4 2 3'
_space_group_name_H-M_alt        'I -4 3 m'
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-10-16 deposited with the CCDC.	2025-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.26090(10)
_cell_length_b                   10.26090(10)
_cell_length_c                   10.26090(10)
_cell_measurement_reflns_used    8151
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.5750
_cell_measurement_theta_min      2.1540
_cell_volume                     1080.330(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -100.00  60.00   0.50   10.00    --  -28.00  45.00   0.00  320
  2  \w    -90.00  50.00   0.50   10.00    --  -28.00  45.00  90.00  280
  3  \w    -90.00  50.00   0.50   10.00    --  -28.00  45.00 180.00  280
  4  \w    -90.00   3.50   0.50   10.00    --  -28.00  45.00 180.00  187
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0043812000
_diffrn_orient_matrix_UB_12      0.0539598000
_diffrn_orient_matrix_UB_13      -0.0429814000
_diffrn_orient_matrix_UB_21      -0.0522092000
_diffrn_orient_matrix_UB_22      -0.0308287000
_diffrn_orient_matrix_UB_23      -0.0332035000
_diffrn_orient_matrix_UB_31      -0.0450808000
_diffrn_orient_matrix_UB_32      0.0304155000
_diffrn_orient_matrix_UB_33      0.0426730000
_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  0.0524
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5620
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.329
_diffrn_reflns_theta_min         2.807
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    16.172
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic blackish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    4.804
_exptl_crystal_description       plate
_exptl_crystal_F_000             1412
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.166
_refine_ls_abs_structure_details
;
 Flack x determined using 97 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(16)
_refine_ls_extinction_coef       0.0333(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     18
_refine_ls_number_reflns         234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.0141
_refine_ls_R_factor_gt           0.0141
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0185P)^2^+0.9761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0306
_refine_ls_wR_factor_ref         0.0306
_reflns_Friedel_coverage         0.708
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                234
_reflns_number_total             234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc07322c2.cif
_cod_data_source_block           Cu10Te4S13
_cod_depositor_comments          'Adding full bibliography for 1573678.cif.'
_cod_original_cell_volume        1080.33(3)
_cod_database_code               1573678
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Cu Te S'
_olex2_refinement_description
;
1. Others
 Fixed Sof: Cu2(0.16675)
;
_shelx_res_checksum              9579
_shelx_hkl_checksum              34668
_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 1.751
_oxdiff_exptl_absorpt_empirical_full_min 0.529