Synthesis and characterization of In(III) <i>S</i>-thiobenzoylthioglycolate complexes and their catalytic applications in CO<sub>2</sub> fixation and multicomponent synthetic reactions.
Pratap, Rajesh; Sahani, Raj Kumar; Maddeshiya, Tarkeshwar; Tripathi, Himanshu Shekhar; Pandey, Mrituanjay D.; Bhattacharya, Subrato; Dalton transactions (Cambridge, England : 2003) 54 (2025) 4518–4529; doi:10.1039/d4dt03382e

data_1573813
_publ_section_title
;
 Synthesis and characterization of In(III)
 <i>S</i>-thiobenzoylthioglycolate complexes and their catalytic
 applications in CO<sub>2</sub> fixation and multicomponent synthetic
 reactions.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4518
_journal_page_last               4529
_journal_paper_doi               10.1039/d4dt03382e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C37 H29 In N2 O6 S6'
_chemical_formula_sum            'C37 H29 In N2 O6 S6'
_chemical_formula_weight         904.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-26 deposited with the CCDC.	2025-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.2437(6)
_cell_length_b                   17.5038(3)
_cell_length_c                   14.8073(3)
_cell_measurement_reflns_used    20825
_cell_measurement_temperature    99.98(18)
_cell_measurement_theta_max      26.8590
_cell_measurement_theta_min      2.4370
_cell_volume                     7320.3(2)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(18)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.963
_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    -29.00   3.00   0.50    4.56    --  -11.14 -17.00   0.00   64
  2  \w      0.00  51.00   0.50    4.56    --   11.77-110.00-128.00  102
  3  \w    -53.00  -5.00   0.50    4.56    --   11.77 -17.00   0.00   96
  4  \w     16.00  49.00   0.50    4.56    --   11.77-128.00 151.00   66
  5  \w    -26.00  13.00   0.50    4.56    --  -11.14 -99.00 -90.00   78
  6  \w    -73.00 -29.00   0.50    4.56    --  -11.14 -38.00 150.00   88
  7  \w    -26.00  23.00   0.50    4.56    --  -11.14 -99.00  30.00   98
  8  \w    -57.00 -21.00   0.50    4.56    --   11.77 -77.00 -90.00   72
  9  \w     47.00  72.00   0.50    4.56    --   11.77  38.00  30.00   50
 10  \w      1.00  28.00   0.50    4.56    --   11.77  38.00  30.00   54
 11  \w    -19.00  41.00   0.50    4.56    --   11.77 -99.00 150.00  120
 12  \w     -1.00  24.00   0.50    4.56    --   11.77  77.00 -60.00   50
 13  \w    -52.00 -23.00   0.50    4.56    --   11.77 -19.00-150.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0009794000
_diffrn_orient_matrix_UB_12      0.0247807000
_diffrn_orient_matrix_UB_13      0.0075903000
_diffrn_orient_matrix_UB_21      0.0086150000
_diffrn_orient_matrix_UB_22      0.0037710000
_diffrn_orient_matrix_UB_23      -0.0462572000
_diffrn_orient_matrix_UB_31      -0.0395930000
_diffrn_orient_matrix_UB_32      0.0014506000
_diffrn_orient_matrix_UB_33      -0.0098648000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            54672
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.064
_diffrn_reflns_theta_min         2.308
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic reddish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       block
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.024
_exptl_crystal_size_mid          0.024
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.900
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Flack x determined using 3449 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.317(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     937
_refine_ls_number_reflns         14672
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0541P)^2^+14.1861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1436
_reflns_Friedel_coverage         0.821
_reflns_Friedel_fraction_full    0.935
_reflns_Friedel_fraction_max     0.857
_reflns_number_gt                9988
_reflns_number_total             14672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03382e2.cif
_cod_data_source_block           in-3_autored
_cod_depositor_comments
;

2025-06-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 1573811--1573813.cif.
;
_cod_original_formula_moiety     '2(C37 H29 In N2 O6 S6)'
_cod_original_formula_sum        'C74 H58 In2 N4 O12 S12'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1809.60
_cod_database_code               1573813
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H O N Sn'
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.976
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C2(H2A,H2B), C48(H48A,H48B), C20(H20A,H20B), C57(H57A,H57B),
 C39(H39A,H39B)
2.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C28(H28), C67(H67), C44(H44), C37(H37), C72(H72), C27(H27),
 C14(H14), C71(H71), C46(H46), C64(H64), C31(H31), C36(H36), C42(H42), C51(H51),
  C73(H73), C68(H68), C23(H23), C53(H53), C45(H45), C43(H43), C54(H54), C8(H8),
 C34(H34), C15(H15), C17(H17), C26(H26), C74(H74), C9(H9), C6(H6), C52(H52),
 C55(H55), C30(H30), C63(H63), C16(H16), C18(H18), C5(H5), C65(H65), C35(H35),
 C60(H60), C66(H66), C25(H25), C24(H24), C62(H62), C7(H7), C61(H61)
;
_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 1.289
_oxdiff_exptl_absorpt_empirical_full_min 0.774