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_7714349
_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         'C11 H20.92 Cl0.413 In N2 Na0.33 O2 S2.92'
_chemical_formula_sum            'C11 H20.92 Cl0.41 In N2 Na0.33 O2 S2.92'
_chemical_formula_weight         443.86
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-28
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.06.10 svn.r3fa896fb for OlexSys, GUI svn.r6535)
;
_audit_update_record
;
2022-11-07 deposited with the CCDC.	2023-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.516(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3992(4)
_cell_length_b                   7.6635(2)
_cell_length_c                   16.9248(5)
_cell_measurement_reflns_used    16490
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.4740
_cell_measurement_theta_min      2.4570
_cell_volume                     1696.62(9)
_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_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33981
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         2.465
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.826
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_description       blockshape
_exptl_crystal_F_000             893
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.933
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3453
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.640
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0913P)^2^+1.1167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1482
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2807
_reflns_number_total             3453
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02681g2.cif
_cod_data_source_block           sb_inl1
_cod_database_code               7714349
_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
 At 1.5 times of:
  All C(H,H,H) groups, All S(H) groups
2. Shared sites
{C1C, C1O}
{O2C, O2O}
3. Restrained distances
 S2-H2 = S3-H3 = S1-H1
 1.96 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Cl2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C1C) = Uanis(C1O)
Uanis(O2C) = Uanis(O2O)
5. Rigid body (RIGU) restrains
 S1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 Na3
 with sigma for 1-2 distances of 0.0004 and sigma for 1-3 distances of 0.0004
6. Others
 Fixed Sof: S2(0.6) H2(0.6) S1(0.92) H1(0.92) Cl1(0.33333) O2O(0.5) O2C(0.5)
 H(0.5) C1C(0.5) H1C(0.5) C1O(0.5) H10(0.5) H10A(0.5) H3A(0.5) H3B(0.5)
 Na1(0.18) Cl2(0.08) S3(0.4) H3(0.4) Na4(0.06) Na2(0.04) Na3(0.05)
7.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C2(H2A,H2B)
7.b Aromatic/amide H refined with riding coordinates:
 O2C(H), C1C(H1C), C10(H10), C10(H10A), C3(H3A), C3(H3B)
7.c Tetrahedral OH refined with riding coordinates:
 S2(H2), S1(H1), S3(H3)
7.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              60133
_olex2_submission_special_instructions 'No special instructions were received'