“On-water” synthesis of thioxoimidazolidinone-isatin/ninhydrin conjugates, followed by temperature-induced dehydration by a ZnMnO3@Ni(OH)2 nano-catalyst
Rana, Soumitra; Basu, Soumyadip; Bera, Aswini; Saha, Pinaki; Ghosh, Prasanta; Khatua, Bhanu Bhusan; Mukhopadhyay, Chhanda; Green Chemistry 26 (2024) 2750–2762; doi:10.1039/D3GC03730D

data_7248012
_publ_section_title
;
 &#x201C;On-water&#x201D; synthesis of
 thioxoimidazolidinone-isatin/ninhydrin conjugates, followed by
 temperature-induced dehydration by a ZnMnO3@Ni(OH)2 nano-catalyst
;
_journal_issue                   5
_journal_name_full               'Green Chemistry'
_journal_page_first              2750
_journal_page_last               2762
_journal_paper_doi               10.1039/D3GC03730D
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C19 H13 Cl N2 O4 S, C2 H3 O S'
_chemical_formula_sum            'C21 H18 Cl N2 O5 S2'
_chemical_formula_weight         477.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2023-08-21 deposited with the CCDC.	2024-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.810(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7787(6)
_cell_length_b                   10.3552(6)
_cell_length_c                   11.3624(7)
_cell_measurement_reflns_used    5930
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.81
_cell_volume                     1131.90(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0326
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13187
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.117
_diffrn_source                   Mo
_exptl_absorpt_coefficient_mu    0.388
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       prism
_exptl_crystal_F_000             494
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 1343 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.43(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.804
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         3995
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.804
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0863P)^2^+0.5758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1160
_reflns_Friedel_coverage         0.884
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                3339
_reflns_number_total             3995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3gc03730d2.cif
_cod_data_source_block           MP_a
_cod_depositor_comments
'Adding full bibliography for 7248010--7248012.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7248012
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              45348
_shelx_hkl_checksum              78829