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_7714345
_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         'C25 H17 In N2 O6 S3'
_chemical_formula_sum            'C25 H17 In N2 O6 S3'
_chemical_formula_weight         652.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-23
_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                 96.274(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2359(3)
_cell_length_b                   11.5628(5)
_cell_length_c                   24.6971(9)
_cell_measurement_reflns_used    6729
_cell_measurement_temperature    250.00(2)
_cell_measurement_theta_max      27.2650
_cell_measurement_theta_min      2.8460
_cell_volume                     2621.68(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_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_environment      N~2~
_diffrn_ambient_temperature      250.00(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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    -69.00 119.30   0.35    5.00    --   29.89  54.00 120.00  538
  2  \w    -69.00 119.30   0.35    5.00    --   29.89  54.00-180.00  538
  3  \w    -67.00 116.05   0.35    5.00    --   29.89  54.00 -60.00  523
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0018411000
_diffrn_orient_matrix_UB_12      0.0601999000
_diffrn_orient_matrix_UB_13      0.0054042000
_diffrn_orient_matrix_UB_21      0.0636430000
_diffrn_orient_matrix_UB_22      -0.0053916000
_diffrn_orient_matrix_UB_23      0.0186551000
_diffrn_orient_matrix_UB_31      0.0437679000
_diffrn_orient_matrix_UB_32      0.0104177000
_diffrn_orient_matrix_UB_33      -0.0213922000
_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  0.0377
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28201
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.833
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.184
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.441
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5995
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+3.5427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5002
_reflns_number_total             5995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02681g2.cif
_cod_data_source_block           in_22by_rt
_cod_database_code               7714345
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{C23, O7}
{C26, O6}
3. Restrained distances
 C14-C15 \\sim C14-C13 \\sim C13-C12
 with sigma of 0.02
 O2-C15 \\sim O2-C12
 with sigma of 0.02
 O4-C17 \\sim O4-C20
 with sigma of 0.02
 C20-C19 \\sim C19-C18 \\sim C18-C17
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C23) = Uanis(O7)
Uanis(C26) = Uanis(O6)
5. Others
 Sof(H25)=1-FVAR(1)
 Sof(H25A)=FVAR(1)
 Sof(H24)=1-FVAR(2)
 Sof(H24A)=FVAR(2)
 Fixed Sof: C23(0.2) H23(0.2) O7(0.8) C26(0.8) H26(0.8) O6(0.2)
6.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C1(H1), C4(H4), C2(H2), C3(H3), C7(H7), C8(H8), C10(H10), C26(H26),
 C18(H18), C9(H9), C15(H15), C24(H24), C24(H24A), C13(H13), C14(H14), C19(H19),
 C25(H25), C25(H25A), C20(H20)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              50821
_shelx_fab_checksum              82772
_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 1.225
_oxdiff_exptl_absorpt_empirical_full_min 0.892