Microwave assisted cobalt(III)-catalysed C-H aminocarbonylation reactions with isocyanates for the synthesis of thiophenecarboxamides.
Taboada-Seras, Borja; Santiago, Carlos; Sustatxa, Eider; Carral-Menoyo, Asier; Sotomayor, Nuria; Lete, Esther; Organic & biomolecular chemistry 23 (2025) 7283–7293; doi:10.1039/d5ob00781j

data_7160610
_publ_section_title
;
 Microwave assisted cobalt(III)-catalysed C-H aminocarbonylation reactions
 with isocyanates for the synthesis of thiophenecarboxamides.
;
_journal_issue                   31
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              7283
_journal_page_last               7293
_journal_paper_doi               10.1039/d5ob00781j
_journal_volume                  23
_journal_year                    2025
_chemical_formula_moiety         'C15 H10 I N3 O S'
_chemical_formula_sum            'C15 H10 I N3 O S'
_chemical_formula_weight         407.22
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-12T13:14:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2025-06-12 deposited with the CCDC.	2025-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.0049(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.55121(11)
_cell_length_b                   17.91412(18)
_cell_length_c                   10.37495(13)
_cell_measurement_reflns_used    7756
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      73.009
_cell_measurement_theta_min      5.23
_cell_volume                     1462.92(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.33a 64-bit (release 26-10-2021))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -51.00   0.00   0.50    0.20    --  -37.11 108.00  61.00  102
  2  \w     28.00  90.00   0.50    0.20    --   37.11-108.00 -35.00  124
  3  \w     43.00  68.00   0.50    0.80    --  110.57-108.00 -35.00   50
  4  \w    104.00 174.00   0.50    0.80    --  110.57 108.00  61.00  140
  5  \w   -116.00 -67.00   0.50    0.20    --  -37.11 -77.00 -30.00   98
  6  \w     52.00  78.00   0.50    0.20    --   37.11  57.00-120.00   52
  7  \w     12.00 107.00   0.50    0.20    --   37.11  57.00 -90.00  190
  8  \w      7.00  49.00   0.50    0.20    --   37.11  57.00-120.00   84
  9  \w     66.00 111.00   0.50    0.20    --   37.11-178.00-120.00   90
 10  \w     81.00 113.00   0.50    0.20    --   37.11  57.00 120.00   64
 11  \w      8.00  35.00   0.50    0.20    --   37.11  57.00 120.00   54
 12  \w     64.00  98.00   0.50    0.80    --  110.57-111.00-150.00   68
 13  \w     26.00  57.00   0.50    0.80    --  110.57 -94.00  60.00   62
 14  \w    128.00 163.00   0.50    0.80    --  110.57  45.00 120.00   70
 15  \w     70.00 101.00   0.50    0.80    --  110.57 -94.00   0.00   62
 16  \w    147.00 176.00   0.50    0.80    --  110.57  61.00-150.00   58
 17  \w     61.00  87.00   0.50    0.80    --  110.57 -94.00  60.00   52
 18  \w     59.00 168.00   0.50    0.80    --  110.57  30.00  30.00  218
 19  \w     80.00 113.00   0.50    0.80    --  110.57  45.00 120.00   66
 20  \w     55.00 100.00   0.50    0.80    --  110.57 -94.00 -30.00   90
 21  \w     84.00 124.00   0.50    0.80    --  110.57  61.00-150.00   80
 22  \w     26.00 105.00   0.50    0.80    --  110.57 -94.00 120.00  158
 23  \w     78.00 174.00   0.50    0.80    --  110.57  45.00 150.00  192
 24  \w    -34.00  -8.00   0.50    0.20    --  -37.11  38.00-120.00   52
 25  \w     11.00  42.00   0.50    0.20    --  -37.11  38.00-120.00   62
 26  \w    -63.00 -38.00   0.50    0.20    --  -37.11  57.00  30.00   50
 27  \w    -74.00 -48.00   0.50    0.20    --  -37.11  77.00 120.00   52
 28  \w    -36.00  42.00   0.50    0.20    --  -37.11  77.00 120.00  156
 29  \w    -78.00 -51.00   0.50    0.20    --  -37.11 178.00 -90.00   54
 30  \w    -35.00  19.00   0.50    0.20    --  -37.11  57.00  30.00  108
 31  \w     78.00 119.00   0.50    0.20    --   37.11 178.00  30.00   82
 32  \w     32.00  70.00   0.50    0.80    --  110.57 -77.00-120.00   76
 33  \w    100.00 126.00   0.50    0.80    --  110.57  45.00-150.00   52
 34  \w    106.00 174.00   0.50    0.80    --  110.57  45.00  60.00  136
 35  \w    103.00 160.00   0.50    0.80    --  110.57 111.00 -60.00  114
 36  \w     30.00  79.00   0.50    0.80    --  110.57-111.00  60.00   98
 37  \w     83.00 108.00   0.50    0.80    --  110.57-111.00  60.00   50
 38  \w     96.00 135.00   0.50    0.80    --  110.57 -61.00  90.00   78
 39  \w     60.00  95.00   0.50    0.80    --  110.57 -94.00-120.00   70
 40  \w     42.00  93.00   0.50    0.80    --  110.57 -61.00  90.00  102
 41  \w     66.00  97.00   0.50    0.80    --  110.57 178.00-150.00   62
 42  \w    118.00 149.00   0.50    0.80    --  110.57 -77.00-120.00   62
 43  \w     84.00 115.00   0.50    0.80    --  110.57  30.00 -30.00   62
 44  \w    105.00 131.00   0.50    0.80    --  110.57  45.00  90.00   52
 45  \w     74.00 109.00   0.50    0.80    --  110.57 -77.00-120.00   70
 46  \w    121.00 146.00   0.50    0.80    --  110.57 178.00 -30.00   50
 47  \w    135.00 167.00   0.50    0.80    --  110.57  45.00-150.00   64
 48  \w     74.00 115.00   0.50    0.80    --  110.57 178.00 -30.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0192518
_diffrn_orient_matrix_UB_12      0.0815191
_diffrn_orient_matrix_UB_13      -0.0388247
_diffrn_orient_matrix_UB_21      0.0970726
_diffrn_orient_matrix_UB_22      0.0186919
_diffrn_orient_matrix_UB_23      0.1561328
_diffrn_orient_matrix_UB_31      0.1688274
_diffrn_orient_matrix_UB_32      -0.0200371
_diffrn_orient_matrix_UB_33      -0.0122111
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_unetI/netI     0.097
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12871
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         4.937
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    18.613
_exptl_absorpt_correction_T_max  0.231
_exptl_absorpt_correction_T_min  0.055
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
        Analytical numeric absorption correction using a multifaceted crystal
        model based on expressions derived by R.C. Clark & J.S. Reid.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_description       prism
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.878
_refine_diff_density_min         -1.762
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2614
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1251P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1554
_refine_ls_wR_factor_ref         0.1583
_reflns_Friedel_coverage         0
_reflns_number_gt                2418
_reflns_number_total             2614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ob00781j2.cif
_cod_data_source_block           b20250129_bts076ducu3
_cod_depositor_comments          'Adding full bibliography for 7160610.cif.'
_cod_database_code               7160610