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_7714350
_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         'C27 H17 In N2 O6 S3, H2 O'
_chemical_formula_sum            'C27 H19 In N2 O7 S3'
_chemical_formula_weight         694.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-24
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-04 deposited with the CCDC.	2023-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                112.718(8)
_cell_angle_beta                 105.609(7)
_cell_angle_gamma                94.128(7)
_cell_formula_units_Z            2
_cell_length_a                   10.406(3)
_cell_length_b                   10.762(3)
_cell_length_c                   13.307(4)
_cell_measurement_reflns_used    9197
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.354
_cell_measurement_theta_min      2.639
_cell_volume                     1297.7(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20104
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.383
_diffrn_reflns_theta_min         3.238
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_T_max  0.4920
_exptl_absorpt_correction_T_min  0.4351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1905 before and 0.0634 after correction.
The Ratio of minimum to maximum transmission is 0.8843.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_description       block-shape
_exptl_crystal_F_000             696
_refine_diff_density_max         2.032
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       0.0031(9)
_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   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         6450
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+4.5672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1346
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5532
_reflns_number_total             6450
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02681g2.cif
_cod_data_source_block           sad_CCDC1
_cod_original_cell_volume        1297.7(6)
_cod_database_code               7714350
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6, C11, C12, C10, C9, C8, C7, N2, N1
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.001
 C18, C13, O2, O1, C19, C14, C15, C16, C21, O3, C20, O4, C22, C17
 with sigma for 1-2 distances of 0.0004 and sigma for 1-3 distances of 0.0004
4. Others
 Fixed Sof: O1(0.7) C18(0.3) C13(0.7) C19(0.3) O4(0.3) C22(0.3) H22(0.3)
 C21(0.3) H21(0.3) C20(0.3) H20(0.3) O3(0.7) C17(0.7) H17(0.7) C16(0.7)
 H16(0.7) C15(0.7) H15(0.7) C14(0.7) O2(0.3) O10(0.5) H10A(0.5) H10B(0.5)
 O9(0.5) H9A(0.5) H9B(0.5)
5.a Riding coordinates:
 O10(H10A,H10B)
5.b Free rotating group:
 O9(H9A,H9B)
5.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C30(H30), C32(H32), C31(H31), C27(H27), C1(H1), C2(H2),
 C11(H11), C3(H3), C7(H7), C8(H8), C9(H9), C12(H12), C22(H22), C21(H21),
 C20(H20), C17(H17), C16(H16), C15(H15)
5.d Fitted pentagon refined as free rotating group:
 C19(O4,C22,C21,C20), O3(C17,C16,C15,C14)
;
_olex2_submission_special_instructions 'No special instructions were received'