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_7714341
_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         'C20 H12 In O8 S4, C6 H16 N'
_chemical_formula_sum            'C26 H28 In N O8 S4'
_chemical_formula_weight         725.55
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1455(14)
_cell_length_b                   10.9826(8)
_cell_length_c                   16.0897(11)
_cell_measurement_reflns_used    4252
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.101
_cell_measurement_theta_min      2.402
_cell_volume                     3206.4(4)
_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    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7614
_diffrn_reflns_point_group_measured_fraction_full 0.754
_diffrn_reflns_point_group_measured_fraction_max 0.754
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.846
_exptl_absorpt_coefficient_mu    1.042
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       block-shape
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 962 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         4252
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0611P)^2^+5.8126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1318
_reflns_Friedel_coverage         0.457
_reflns_Friedel_fraction_full    0.492
_reflns_Friedel_fraction_max     0.492
_reflns_number_gt                3378
_reflns_number_total             4252
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02681g2.cif
_cod_data_source_block           exp_7218
_cod_database_code               7714341
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-C10 \\sim C10-C9 \\sim C8-C9 \\sim C8-C7 \\sim O4-C7
 with sigma of 0.02
 O2-C2 \\sim C2-C3 \\sim C3-C4 \\sim C5-C4 \\sim O2-C5
 with sigma of 0.02
 C18-C17 \\sim O8-C17 \\sim O8-C20 \\sim C20-C19 \\sim C19-C18
 with sigma of 0.02
 C2-C1 \\sim C6-C7 \\sim C16-C17 \\sim C12-C11
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 N1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C25(H25A,H25B), C23(H23A,H23B)
4.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C19(H19), C18(H18), C15(H15), C14(H14), C13(H13), C3(H3), C4(H4),
 C5(H5), C10(H10), C9(H9), C8(H8)
4.d Fitted pentagon refined as free rotating group:
 C17(O8,C20,C19,C18), C12(O6,C15,C14,C13), C3(C4,C5,O2,C2), C10(C9,C8,C7,O4)
4.e Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              72975
_olex2_submission_special_instructions 'No special instructions were received'