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_7714344
_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 H29.8 In N O8 S4'
_chemical_formula_weight         727.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_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                 98.209(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.341(3)
_cell_length_b                   18.830(6)
_cell_length_c                   14.472(4)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.40
_cell_volume                     3058.8(15)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36004
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.824
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1099 before and 0.0700 after correction.
The Ratio of minimum to maximum transmission is 0.6249.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            lightbrown
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       block-shape
_exptl_crystal_F_000             1479
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.00193(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5378
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0361
_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^)+6.4071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0670
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4941
_reflns_number_total             5378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02681g2.cif
_cod_data_source_block           1febe_0m_a
_cod_original_cell_volume        3058.8(16)
_cod_original_formula_sum        'C26 H29.80 In N O8 S4'
_cod_database_code               7714344
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 O4, C7, C10, C9, C8, C11, O5, C13, C12
 with sigma for 1-2 distances of 0.0004 and sigma for 1-3 distances of 0.0004
4. Others
 Fixed Sof: O4(0.6) C10(0.6) H10(0.6) C9(0.6) H9(0.6) C8(0.6) H8(0.6) C11(0.4)
 H11(0.4) O5(0.4) C13(0.4) H13(0.4) C12(0.4) H12(0.4)
5.a Ternary CH refined with riding coordinates:
 C27(H27), C24(H24)
5.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
5.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C8(H8), C21(H21), C23(H23), C5(H5), C16(H16), C22(H22),
 C4(H4), C3(H3), C17(H17), C18(H18), C11(H11), C13(H13), C12(H12)
5.d Fitted pentagon refined as free rotating group:
 O4(C7,C10,C9,C8)
5.e Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C25(H25A,H25B,H25C), C29(H29A,H29B,
 H29C)
;
_shelx_res_checksum              81082
_olex2_submission_special_instructions 'No special instructions were received'