Isonicotinate-Zn(ii)/Cd(ii) bridged dicobaloximes: synthesis, characterization and electrocatalytic proton reduction studies
Yadav, Jitendra Kumar; Mishra, Anjali; Mishra, Gaurav Kumar; Pal, Sarvesh Kumar; Narvekar, Kedar Umakant; Rahaman, Ahibur; Singh, Nanhai; Lama, Prem; Kumar, Kamlesh; New Journal of Chemistry 47 (2023) 20583–20593; doi:10.1039/D3NJ04014C

data_7062901
_publ_section_title
;
 Isonicotinate-Zn(ii)/Cd(ii) bridged dicobaloximes: synthesis,
 characterization and electrocatalytic proton reduction studies
;
_journal_issue                   44
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20583
_journal_page_last               20593
_journal_paper_doi               10.1039/D3NJ04014C
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety
'C31 H49 Cd Cl2 Co2 N11 O16, C3 H7 N O, 4(H2 O)'
_chemical_formula_sum            'C34 H64 Cd Cl2 Co2 N12 O21'
_chemical_formula_weight         1278.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-10-13 deposited with the CCDC.	2023-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.191(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7747(5)
_cell_length_b                   22.7674(12)
_cell_length_c                   23.7065(12)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.74
_cell_volume                     5245.0(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-III photon detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            59463
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.569
_exptl_absorpt_coefficient_mu    1.213
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       plate
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.052
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.6870
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         9236
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+9.8754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7481
_reflns_number_total             9236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04014c2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7062901
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.861
_shelx_estimated_absorpt_t_max   0.940
_shelx_res_checksum              316