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_7063281
_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_absolute_configuration unk
_chemical_formula_moiety         'C51 H39 Ag Cd O6 P2 S3'
_chemical_formula_sum            'C51 H39 Ag Cd O6 P2 S3'
_chemical_formula_weight         1126.300
_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'
_symmetry_Int_Tables_number      4
_audit_creation_date             2024-01-25
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2024.01.11 svn.r2f8d729c for OlexSys, GUI svn.r6697)
;
_audit_update_record
;
2024-06-06 deposited with the CCDC.	2024-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.136(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6917(3)
_cell_length_b                   14.3238(2)
_cell_length_c                   14.3792(3)
_cell_measurement_reflns_used    12360
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.0280
_cell_measurement_theta_min      3.1980
_cell_volume                     2484.18(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9965
_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    -69.00 118.20   0.30   20.00    --   29.89  54.00-180.00  624
  2  \w    -69.00 118.20   0.30   20.00    --   29.89  54.00  30.00  624
  3  \w    -69.00 -43.80   0.30   20.00    --   29.89  54.00  90.00   84
  4  \w    -69.00 118.20   0.30   20.00    --   29.89  54.00 -90.00  624
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.9985
_diffrn_reflns_Laue_measured_fraction_max 0.9965
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37267
_diffrn_reflns_point_group_measured_fraction_full 0.9987
_diffrn_reflns_point_group_measured_fraction_max 0.9937
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    1.060
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       block
_exptl_crystal_F_000             1130.272
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.4190
_refine_diff_density_min         -0.3753
_refine_diff_density_rms         0.0436
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -0.039(7)
_refine_ls_d_res_high            0.7448
_refine_ls_d_res_low             7.1619
_refine_ls_goodness_of_fit_ref   1.0524
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    99
_refine_ls_number_parameters     706
_refine_ls_number_reflns         12497
_refine_ls_number_restraints     470
_refine_ls_restrained_S_all      1.0321
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+0.4016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.991
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              19
_reflns_limit_l_min              -19
_reflns_number_gt                11299
_reflns_number_total             12497
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3nj04083f3.cif
_cod_data_source_block           cd-ag-rt
_cod_depositor_comments
'Adding full bibliography for 7063277--7063281.cif.'
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               7063281
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O2-C2 = C2-C3 = C3-C4 = C4-C5 = C5-O2
 1.39 with sigma of 0.01
 O4-C10 = C10-C9 = C9-C8 = C8-C7 = C7-O4
 1.39 with sigma of 0.01
 O6-C12 = C12-C13 = C13-C14 = C14-C15 = C15-O6
 1.39 with sigma of 0.01
 O2A-C5A = C5A-C4A = C4A-C3A = C3A-C2A = C2A-O2A
 1.39 with sigma of 0.01
 O4a-C10a = C10a-C9a = C9a-C8a = C8a-C7a = C7a-O4a
 1.39 with sigma of 0.01
 O2A-C2A = C2A-C3A = C3A-C4A = C4A-C5A = C5A-O2A
 1.39 with sigma of 0.01
 C1-C2 \\sim C1-C2A
 with sigma of 0.02
 C8-C7 \\sim C8a-C7a
 with sigma of 0.02
 C2-C3 \\sim C2A-C3A
 with sigma of 0.02
 C8-C9 \\sim C8a-C9a
 with sigma of 0.02
 C2-O2 \\sim C2A-O2A
 with sigma of 0.02
 C8-O4 \\sim C8a-O4a
 with sigma of 0.04
 C4-C3 \\sim C4A-C3A
 with sigma of 0.02
 C8-C6 \\sim C8a-C6
 with sigma of 0.04
 C4-C5 \\sim C4A-C5A
 with sigma of 0.02
 C8-C10 \\sim C8a-C10a
 with sigma of 0.04
 O2-C5 \\sim O2A-C5A
 with sigma of 0.02
 C1-C3 \\sim C1-C3A
 with sigma of 0.04
 C1-O2 \\sim C1-O2A
 with sigma of 0.04
 C2-C4 \\sim C2A-C4A
 with sigma of 0.04
 C2-C5 \\sim C2A-C5A
 with sigma of 0.04
 C4-O2 \\sim C4A-O2A
 with sigma of 0.04
 C3-O2 \\sim C3A-O2A
 with sigma of 0.04
 C3-C5 \\sim C3A-C5A
 with sigma of 0.04
 O2-C3 \\sim C2-C4 \\sim C3-C5 \\sim C4-O2 \\sim C5-C2
 with sigma of 0.02
 O4-C9 \\sim C10-C8 \\sim C9-C7 \\sim C8-O4 \\sim C7-C10
 with sigma of 0.02
 O6-C13 \\sim C12-C14 \\sim C13-C15 \\sim C14-O6 \\sim C15-C12
 with sigma of 0.02
 O2A-C4A \\sim C5A-C3A \\sim C4A-C2A \\sim C3A-O2A \\sim C2A-C5A
 with sigma of 0.02
 O4-C7 \\sim O4a-C7a
 with sigma of 0.02
 O4-C10 \\sim O4a-C10a
 with sigma of 0.02
 C7-C6 \\sim C7a-C6
 with sigma of 0.02
 C10-C9 \\sim C10a-C9a
 with sigma of 0.02
 O4-C6 \\sim O4a-C6
 with sigma of 0.04
 O4-C9 \\sim O4a-C9a
 with sigma of 0.04
 C7-C10 \\sim C7a-C10a
 with sigma of 0.04
 C7-C9 \\sim C7a-C9a
 with sigma of 0.04
 O4a-C9a \\sim C10a-C8a \\sim C9a-C7a \\sim C8a-O4a \\sim C7a-C10a
 with sigma of 0.02
 O2A-C3A \\sim C2A-C4A \\sim C3A-C5A \\sim C4A-O2A \\sim C5A-C2A
 with sigma of 0.02
 O5-C11 \\sim O3-C6 \\sim O1-C1
 with sigma of 0.001
 C12-C13 \\sim C12-C13a
 with sigma of 0.02
 C12-O6 \\sim C12-O6a
 with sigma of 0.02
 C13-C14 \\sim C13a-C14a
 with sigma of 0.02
 C14-C15 \\sim C14a-C15a
 with sigma of 0.02
 C15-O6 \\sim C15a-O6a
 with sigma of 0.02
 C12-C14 \\sim C12-C14a
 with sigma of 0.04
 C12-C15 \\sim C12-C15a
 with sigma of 0.04
 C13-C15 \\sim C13a-C15a
 with sigma of 0.04
 C14-O6 \\sim C14a-O6a
 with sigma of 0.04
3. Restrained planarity
 O2, C2, C3, C4, C5
 with sigma of 0.1
 O4, C10, C9, C8, C7
 with sigma of 0.1
 O6, C12, C13, C14, C15
 with sigma of 0.1
 O2A, C5A, C4A, C3A, C2A
 with sigma of 0.1
 O4a, C10a, C9a, C8a, C7a
 with sigma of 0.1
 O2A, C2A, C3A, C4A, C5A
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 C9a, S2, C6, C7a, O3, C8a, O4a, C10a
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3A, S1, C1, O1, C2A, O2A, C4A, C5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, S1, C1, O1, C2, O2, C4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, S3, C11, O5, C13, O6, C14, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, S2, C6, C7, O3, C8, O4, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, O5, S3, C12, O6a, C15a, C14a, C13a
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C2A)=Sof(C4A)=Sof(H4A)=Sof(C3A)=Sof(H3A)=Sof(O2A)=Sof(C5A)=Sof(H5A)=1-
 FVAR(1)
 Sof(C2)=Sof(C4)=Sof(H4)=Sof(C3)=Sof(H3)=Sof(O2)=Sof(C5)=Sof(H5)=FVAR(1)
 Sof(C8a)=Sof(H8a)=Sof(O4a)=Sof(C7a)=Sof(C10a)=Sof(H10a)=Sof(C9a)=Sof(H9a)=1-
 FVAR(2)
 Sof(C8)=Sof(H8)=Sof(O4)=Sof(C7)=Sof(C10)=Sof(H10)=Sof(C9)=Sof(H9)=FVAR(2)
 Sof(C13a)=Sof(H13a)=Sof(C14a)=Sof(H14a)=Sof(C15a)=Sof(H15a)=Sof(O6a)=1-FVAR(3)
 Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(O6)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C17(H17), C16(H16), C46(H46), C49(H49), C50(H50), C36(H36), C34(H34),
 C43(H43), C40(H40), C48(H48), C47(H47), C44(H44), C20(H20), C22(H22), C18(H18),
  C42(H42), C4(H4), C41(H41), C10(H10), C32(H32), C35(H35), C29(H29), C3(H3),
 C30(H30), C19(H19), C38(H38), C28(H28), C13(H13), C26(H26), C9(H9), C37(H37),
 C25(H25), C31(H31), C14(H14), C23(H23), C24(H24), C15(H15), C5(H5), C4A(H4A),
 C3A(H3A), C5A(H5A), C8a(H8a), C10a(H10a), C9a(H9a), C13a(H13a), C14a(H14a),
 C15a(H15a)
;
_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
;