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_7063278
_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         'C68 H54.30 Cd2 Na2 O14 P2 S6, 0.3(C H4 O)'
_chemical_formula_sum            'C68.3 H55.5 Cd2 Na2 O14.3 P2 S6'
_chemical_formula_weight         1630.13
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-06
_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                86.810(16)
_cell_angle_beta                 81.612(17)
_cell_angle_gamma                64.754(15)
_cell_formula_units_Z            1
_cell_length_a                   10.359(3)
_cell_length_b                   10.818(4)
_cell_length_c                   18.626(6)
_cell_measurement_reflns_used    9777
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.450
_cell_measurement_theta_min      2.319
_cell_volume                     1867.7(11)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25875
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.105
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0616 before and 0.0428 after correction.
The Ratio of minimum to maximum transmission is 0.8794.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       rod-shape
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.698
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         7612
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0418P)^2^+1.2552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6169
_reflns_number_total             7612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04083f3.cif
_cod_data_source_block           ups3754_bhu_fk52_0m
_cod_depositor_comments
'Adding full bibliography for 7063277--7063281.cif.'
_cod_original_cell_volume        1867.6(11)
_cod_original_formula_sum        'C68.30 H55.50 Cd2 Na2 O14.30 P2 S6'
_cod_database_code               7063278
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.784
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C34-O7
 1.8 with sigma of 0.02
 O7-H7
 0.85 with sigma of 0.01
 O3-C12
 1.5 with sigma of 0.02
 C34-Na1
 4.5 with sigma of 0.04
 C34-H7
 1.903571 with sigma of 0.02
 Na1-H7
 2.83835 with sigma of 0.02
 C3-C35 \\sim C3A-C35
 with sigma of 0.02
 C3-C4 \\sim C3A-C4A
 with sigma of 0.02
 C35-O2 \\sim C35-O2A
 with sigma of 0.02
 O2-C5 \\sim O2A-C5A
 with sigma of 0.02
 C4-C5 \\sim C4A-C5A
 with sigma of 0.02
 C3-C5 \\sim C3A-C5A
 with sigma of 0.04
 C35-C4 \\sim C35-C4A
 with sigma of 0.04
 C35-C5 \\sim C35-C5A
 with sigma of 0.04
 O2-C4 \\sim O2A-C4A
 with sigma of 0.04
 C2-C13B \\sim C14B-C36B
 with sigma of 0.02
 C2-O13A \\sim C14A-C36A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(P1) = Uanis(Cd1)
4. Rigid body (RIGU) restrains
 C3, O2, C4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3A, O2A, C4A, C5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C3A)=Sof(H3A)=Sof(C5A)=Sof(H5A)=Sof(C4A)=Sof(H4A)=Sof(O2A)=Sof(O15B)=
 Sof(C13B)=Sof(H13B)=1-FVAR(1)
 Sof(C3)=Sof(H3)=Sof(O2)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C15A)=Sof(H15A)=
 Sof(O13A)=FVAR(1)
 Fixed Sof: H34A(0.15) C14B(0.5) H14B(0.5) C36B(0.5) H36B(0.5) C36A(0.5)
 H36A(0.5) C14A(0.5) H14A(0.5) O3(0.15) H3B(0.15) C12(0.15) H12A(0.15)
 H12B(0.15) H12C(0.15)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C28(H28), C23(H23), C29(H29), C21(H21), C33(H33), C24(H24), C25(H25),
 C26(H26), C30(H30), C32(H32), C17(H17), C20(H20), C31(H31), C18(H18), C19(H19),
  C8(H8), C10(H10), C9(H9), C4(H4), C5(H5), C3A(H3A), C5A(H5A), C4A(H4A),
 C14B(H14B), C36B(H36B), C13B(H13B), C15A(H15A), C36A(H36A), C14A(H14A)
6.b Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C12(H12A,H12B,H12C)
6.c Idealised tetrahedral OH refined as rotating group:
 O3(H3B)
;
_shelx_res_checksum              52595
_shelx_hkl_checksum              83782
_olex2_submission_special_instructions 'No special instructions were received'