Synthesis and Structural Features of Indium(III) furan-2-thiocarboxylates: Efficient Catalytic Activity Toward Multicomponent Reactions via Knoevenagel Condensation
Kumar, Krishna; Sahani, Raj Kumar; Garai, Somenath; Bhattacharya, Subrato; Dalton Transactions  (2023) –; doi:10.1039/D3DT02681G

data_7714342
_publ_section_title
;
 Synthesis and Structural Features of Indium(III)
 furan-2-thiocarboxylates: Efficient Catalytic Activity Toward
 Multicomponent Reactions via Knoevenagel Condensation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02681G
_journal_year                    2023
_chemical_formula_moiety         'C56 H38 Ag In O8 P2 S4'
_chemical_formula_sum            'C56 H38 Ag In O8 P2 S4'
_chemical_formula_weight         1251.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-24
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.06.10 svn.r3fa896fb for OlexSys, GUI svn.r6535)
;
_audit_update_record
;
2022-10-04 deposited with the CCDC.	2023-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.664(2)
_cell_length_b                   16.4106(19)
_cell_length_c                   21.309(2)
_cell_measurement_reflns_used    2870
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.8630
_cell_measurement_theta_min      3.7050
_cell_volume                     5477.6(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0938
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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    -18.00  23.00   1.00    6.57    --  -18.59 -99.00  90.00   41
  2  \w    -94.00 -67.00   1.00    6.57    --  -18.59-178.00   0.00   27
  3  \w    -25.00  13.00   1.00    6.57    --  -18.59  38.00-150.00   38
  4  \w    -49.00  18.00   1.00    6.57    --   19.84 -57.00-150.00   67
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0166196000
_diffrn_orient_matrix_UB_12      -0.0164431000
_diffrn_orient_matrix_UB_13      0.0282837000
_diffrn_orient_matrix_UB_21      0.0201324000
_diffrn_orient_matrix_UB_22      -0.0315354000
_diffrn_orient_matrix_UB_23      -0.0172636000
_diffrn_orient_matrix_UB_31      0.0369537000
_diffrn_orient_matrix_UB_32      0.0245918000
_diffrn_orient_matrix_UB_33      -0.0033123000
_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  0.0854
_diffrn_reflns_av_unetI/netI     0.0829
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7329
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         3.721
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.042
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block-shape
_exptl_crystal_F_000             2512
_refine_diff_density_max         0.891
_refine_diff_density_min         -1.242
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         2550
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1421
_refine_ls_R_factor_gt           0.0994
_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^)+111.2431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1783
_refine_ls_wR_factor_ref         0.2061
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1597
_reflns_number_total             2550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02681g2.cif
_cod_data_source_block           fk9
_cod_original_cell_volume        5477.5(11)
_cod_database_code               7714342
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H40 S8 O8 N4 Ag1 In1'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C10) \\sim
Ueq, Uanis(C12) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C20) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C15) \\sim Ueq,
Uanis(C22) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(S2) \\sim Ueq, Uanis(S1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 S2, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: O1(0.5) C1(0.5) C4(0.5) O4(0.5) C6(0.5) C8(0.5) C10(0.5) H10(0.5)
 C12(0.5) O2(0.5) O3(0.5) C14(0.5) H14(0.5) C16(0.5) H16(0.5) C18(0.5) H18(0.5)
 C20(0.5) P2(0.5) C22(0.5) C24(0.5) H24(0.5) C26(0.5) H26(0.5) C28(0.5)
 H28(0.5) C7(0.5) H7(0.5) C15(0.5) H15(0.5) C2(0.5) C17(0.5) H17(0.5) C9(0.5)
 H9(0.5) C19(0.5) H19(0.5) C5(0.5) H5(0.5) C21(0.5) H21(0.5) C11(0.5) C23(0.5)
 H23(0.5) C3(0.5) H3(0.5) C25(0.5) H25(0.5) C13(0.5) H13(0.5) C27(0.5) H27(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C14(H14), C16(H16), C18(H18), C24(H24), C26(H26), C28(H28), C7(H7),
 C15(H15), C17(H17), C9(H9), C19(H19), C5(H5), C21(H21), C23(H23), C3(H3),
 C25(H25), C13(H13), C27(H27)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              13042
_shelx_fab_checksum              95650
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.315
_oxdiff_exptl_absorpt_empirical_full_min 0.760