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_1573811
_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         'C39 H29 In N2 O6 S6'
_chemical_formula_sum            'C39 H29 In N2 O6 S6'
_chemical_formula_weight         928.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-23
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-22 deposited with the CCDC.	2025-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.401(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9278(2)
_cell_length_b                   9.4920(2)
_cell_length_c                   19.0268(4)
_cell_measurement_reflns_used    12150
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.4860
_cell_measurement_theta_min      2.8400
_cell_volume                     1957.14(7)
_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_temperature      293
_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 0.961
_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    -79.00 -28.00   0.50    2.96    --  -11.14 -62.00   1.00  102
  2  \w      7.00  50.00   0.50    2.96    --  -11.14  62.00 139.00   86
  3  \w     -6.00  65.00   0.50    2.96    --   11.77  62.00 139.00  142
  4  \w    -50.00 -11.00   0.50    2.96    --   11.77 -62.00   1.00   78
  5  \w    -26.00  16.00   0.50    2.96    --  -11.14 -99.00 150.00   84
  6  \w     -8.00  18.00   0.50    2.96    --  -11.14 -99.00-120.00   52
  7  \w    -26.00  35.00   0.50    2.96    --  -11.14  38.00 150.00  122
  8  \w    -22.00  12.00   0.50    2.96    --  -11.14 -99.00  60.00   68
  9  \w     -7.00  23.00   0.50    2.96    --  -11.14 -99.00 -30.00   60
 10  \w    -24.00   1.00   0.50    2.96    --  -11.14 -62.00   1.00   50
 11  \w      9.00  59.00   0.50    2.96    --   11.77-125.00  30.00  100
 12  \w     14.00  59.00   0.50    2.96    --   11.77-125.00-120.00   90
 13  \w    -17.00  13.00   0.50    2.96    --   11.77 -99.00 -30.00   60
 14  \w    -54.00 -28.00   0.50    2.96    --   11.77 -19.00 150.00   52
 15  \w    -20.00   5.00   0.50    2.96    --   11.77 -19.00 150.00   50
 16  \w     14.00  40.00   0.50    2.96    --   11.77-125.00  60.00   52
 17  \w    -49.00 -23.00   0.50    2.96    --   11.77 -38.00  90.00   52
 18  \w      1.00  26.00   0.50    2.96    --   11.77  19.00 -90.00   50
 19  \w    -27.00   3.00   0.50    2.96    --   11.77 -19.00-150.00   60
 20  \w     41.00  76.00   0.50    2.96    --   11.77  19.00 -90.00   70
 21  \w     -9.00  34.00   0.50    2.96    --   11.77 -99.00-120.00   86
;
_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      0.0391154000
_diffrn_orient_matrix_UB_12      -0.0179472000
_diffrn_orient_matrix_UB_13      0.0314170000
_diffrn_orient_matrix_UB_21      0.0299910000
_diffrn_orient_matrix_UB_22      -0.0508521000
_diffrn_orient_matrix_UB_23      -0.0190872000
_diffrn_orient_matrix_UB_31      0.0430647000
_diffrn_orient_matrix_UB_32      0.0517299000
_diffrn_orient_matrix_UB_33      -0.0078684000
_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  0.0460
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23670
_diffrn_reflns_point_group_measured_fraction_full 0.918
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.068
_diffrn_reflns_theta_min         2.402
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71107
_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 light red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_description       block
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.028
_exptl_crystal_size_mid          0.026
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         7385
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0159P)^2^+0.7170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0604
_refine_ls_wR_factor_ref         0.0663
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_full    0.838
_reflns_Friedel_fraction_max     0.757
_reflns_number_gt                6371
_reflns_number_total             7385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03382e2.cif
_cod_data_source_block           in-2nonheating_autored
_cod_depositor_comments
'Adding full bibliography for 1573811--1573813.cif.'
_cod_database_code               1573811
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'In C H O N S'
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.973
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.97(2)
 0.03(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Rigid body (RIGU) restrains
 C28, C27, C29, C30, C25, C26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C32(H32A,H32B), C14(H14A,H14B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C30(H30), C8(H8), C39(H39), C37(H37), C35(H35),
 C26(H26), C9(H9), C28(H28), C10(H10), C1(H1), C21(H21), C5(H5), C38(H38),
 C27(H27), C36(H36), C20(H20), C18(H18), C29(H29), C19(H19), C17(H17)
;
_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 1.136
_oxdiff_exptl_absorpt_empirical_full_min 0.841