Synthesis of a series of Cd(ii) furan-2-thiocarobxylates: unprecedented coordination geometry of a Cd(ii) complex exhibiting catalytic efficiency for the synthesis of 3,4-dihydropyrimidine-2(1H)-one derivatives
Kumar, Krishna; Shrivastav, Akash; Sakshi,; Choudhury, Angshuman Roy; Bhattacharya, Subrato; New Journal of Chemistry 48 (2024) 12654–12663; doi:10.1039/D3NJ04083F

data_7063280
_publ_section_title
;
 Synthesis of a series of Cd(ii) furan-2-thiocarobxylates: unprecedented
 coordination geometry of a Cd(ii) complex exhibiting catalytic efficiency
 for the synthesis of 3,4-dihydropyrimidine-2(1H)-one derivatives
;
_journal_issue                   28
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12654
_journal_page_last               12663
_journal_paper_doi               10.1039/D3NJ04083F
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C20 H12 Br1.74 Cd2 Cl0.25 O8 S4, 2(C24 H20 P)'
_chemical_formula_sum            'C68 H52 Br1.74 Cd2 Cl0.25 O8 P2 S4'
_chemical_formula_weight         1559.98
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-31
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-06 deposited with the CCDC.	2024-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                84.312(2)
_cell_angle_beta                 76.622(2)
_cell_angle_gamma                81.227(2)
_cell_formula_units_Z            1
_cell_length_a                   9.5004(2)
_cell_length_b                   12.9536(3)
_cell_length_c                   13.7167(3)
_cell_measurement_reflns_used    31624
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.6380
_cell_measurement_theta_min      2.4010
_cell_volume                     1619.44(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_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_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.964
_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     31.00  58.00   0.50    0.68    --  -11.14  77.00  30.00   54
  2  \w     16.00  53.00   0.50    0.68    --  -11.14  60.00  74.00   74
  3  \w    -31.00  12.00   0.50    0.68    --  -11.14  60.00  74.00   86
  4  \w    -34.00  12.00   0.50    0.68    --  -11.14  77.00  30.00   92
  5  \w    -30.00  -5.00   0.50    0.68    --  -11.14  57.00 -60.00   50
  6  \w    -18.00  18.00   0.50    0.68    --  -11.14  38.00 -30.00   72
  7  \w     19.00  57.00   0.50    0.68    --  -11.14  57.00 -60.00   76
  8  \w    -19.00  55.00   0.50    0.68    --  -11.14  38.00-180.00  148
  9  \w    -32.00  61.00   0.50    0.68    --  -11.14  19.00 -90.00  186
 10  \w     24.00  53.00   0.50    0.68    --  -11.14  38.00 -30.00   58
 11  \w    -32.00  61.00   0.50    0.68    --  -11.14  19.00  60.00  186
 12  \w    -69.00 -44.00   0.50    0.68    --  -11.14 136.00  47.70   50
 13  \w    -80.00 -46.00   0.50    0.68    --  -11.14 153.00 130.95   68
 14  \w    -73.00 -41.00   0.50    0.68    --  -11.14 143.00  85.47   64
 15  \w    -71.00 -41.00   0.50    0.68    --  -11.14 140.00   4.95   60
 16  \w    -71.00 -43.00   0.50    0.68    --  -11.14 140.00 -61.37   56
 17  \w    -70.00 -39.00   0.50    0.68    --  -11.14 138.00-101.61   62
 18  \w    -72.00 -44.00   0.50    0.68    --  -11.14 141.00-158.52   56
 19  \w     16.00  65.00   0.50    0.68    --   11.77  77.00 -60.00   98
 20  \w     -4.00  41.00   0.50    0.68    --   11.77  38.00 -90.00   90
 21  \w    -11.00  15.00   0.50    0.68    --   11.77  77.00 -60.00   52
 22  \w     -4.00  72.00   0.50    0.68    --   11.77  38.00 -30.00  152
 23  \w     49.00  75.00   0.50    0.68    --   11.77  38.00 -90.00   52
 24  \w     49.00  76.00   0.50    0.68    --   11.77  19.00 -90.00   54
 25  \w     45.00  79.00   0.50    0.68    --   11.77  19.00-180.00   68
 26  \w      0.00  33.00   0.50    0.68    --   11.77  19.00-180.00   66
 27  \w     11.00  36.00   0.50    0.68    --   11.77  19.00 -90.00   50
 28  \w     17.00  42.00   0.50    0.68    --   11.77  60.00  74.00   50
 29  \w     49.00  75.00   0.50    0.68    --   11.77  60.00  74.00   52
 30  \w    -13.00  70.00   0.50    0.68    --   11.77  77.00 150.00  166
 31  \w    -22.00  16.00   0.50    0.68    --   11.77 -60.00 -65.00   76
 32  \w    -52.00   4.00   0.50    0.68    --   11.77 -57.00-150.00  112
 33  \w    -55.00 -29.00   0.50    0.68    --   11.77 -57.00  30.00   52
 34  \w    -47.00   2.00   0.50    0.68    --   11.77 -19.00 120.00   98
 35  \w    -13.00  12.00   0.50    0.68    --   11.77 -38.00  90.00   50
 36  \w      6.00  31.00   0.50    0.68    --   11.77 -57.00  30.00   50
 37  \w    -50.00  -8.00   0.50    0.68    --   11.77 -19.00-150.00   84
 38  \w    -36.00   5.00   0.50    0.68    --  -11.14 -19.00-120.00   82
 39  \w    -16.00  10.00   0.50    0.68    --  -11.14 -60.00 -65.00   52
 40  \w    -63.00 -23.00   0.50    0.68    --  -11.14 -60.00 -65.00   80
 41  \w    -80.00 -41.00   0.50    0.68    --  -11.14 -77.00   0.00   78
 42  \w    -29.00  15.00   0.50    0.68    --  -11.14 -77.00   0.00   88
 43  \w    -83.00 -42.00   0.50    0.68    --  -11.14 -19.00-120.00   82
 44  \w    -69.00   4.00   0.50    0.68    --  -11.14 -38.00 -30.00  146
 45  \w    -76.00 -10.00   0.50    0.68    --  -11.14 -38.00  60.00  132
 46  \w    -75.00   7.00   0.50    0.68    --  -11.14 -57.00 150.00  164
 47  \w    -24.00  23.00   0.50    0.68    --  -11.14 -99.00 120.00   94
 48  \w    -23.00  14.00   0.50    0.68    --  -11.14 -99.00  90.00   74
 49  \w    -21.00  21.00   0.50    0.68    --  -11.14 -99.00 -90.00   84
 50  \w    -25.00  17.00   0.50    0.68    --  -11.14 -99.00-150.00   84
 51  \w    -25.00  16.00   0.50    0.68    --  -11.14 -99.00 -30.00   82
 52  \w     24.00  70.00   0.50    0.68    --   11.77-136.00  45.83   92
 53  \w     16.00  41.00   0.50    0.68    --   11.77-125.00 150.00   50
 54  \w    -22.00  37.00   0.50    0.68    --   11.77 -99.00 150.00  118
 55  \w     18.00  48.00   0.50    0.68    --   11.77-125.00 -60.00   60
 56  \w     17.00  43.00   0.50    0.68    --   11.77-125.00-120.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0563221000
_diffrn_orient_matrix_UB_12      -0.0189251000
_diffrn_orient_matrix_UB_13      0.0379398000
_diffrn_orient_matrix_UB_21      -0.0380480000
_diffrn_orient_matrix_UB_22      0.0514962000
_diffrn_orient_matrix_UB_23      0.0039472000
_diffrn_orient_matrix_UB_31      -0.0371082000
_diffrn_orient_matrix_UB_32      -0.0085634000
_diffrn_orient_matrix_UB_33      -0.0371852000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            60075
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.122
_diffrn_reflns_theta_min         2.406
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.973
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       block
_exptl_crystal_F_000             779
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6901
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0505P)^2^+0.9411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5107
_reflns_number_total             6901
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04083f3.cif
_cod_data_source_block           fk86kksbsirlab_auto
_cod_depositor_comments
'Adding full bibliography for 7063277--7063281.cif.'
_cod_database_code               7063280
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.671
_shelx_estimated_absorpt_t_min   0.589
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of
0.003 and sigma for terminal atoms of 0.02
Uanis(Br2) = Uanis(Cl2)
3.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C34(H34), C18(H18), C24(H24), C16(H16), C28(H28), C22(H22),
 C30(H30), C33(H33), C32(H32), C19(H19), C26(H26), C25(H25), C20(H20), C27(H27),
  C3(H3), C21(H21), C11(H11), C12(H12), C31(H31), C13(H13), C4(H4), C5(H5),
 C9(H9), C8(H8), C10(H10)
;
_shelx_res_checksum              72211
_shelx_hkl_checksum              2394
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.411
_oxdiff_exptl_absorpt_empirical_full_min 0.761