A Comparison of Structure-Activity Relationships between Bis(imino)Pyridine Pincers of Nickel and Cobalt for Electrochemical Reduction of CO2
Das, Anjan; Mukhopadhyay, Titas Kumar; Maitra, Biswajit; Pal, Dibyendu; Mondal, Moumita; New Journal of Chemistry  (2026) –; doi:10.1039/D5NJ02563J

data_7064201
_publ_section_title
;
 A Comparison of Structure-Activity Relationships between
 Bis(imino)Pyridine Pincers of Nickel and Cobalt for Electrochemical
 Reduction of CO2
;
_journal_name_full               'New Journal of Chemistry'
_journal_paper_doi               10.1039/D5NJ02563J
_journal_year                    2026
_chemical_formula_moiety         'C21 H31 Br2 N3 Ni'
_chemical_formula_sum            'C21 H31 Br2 N3 Ni'
_chemical_formula_weight         544.02
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-03-01
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-24 deposited with the CCDC.	2025-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.7374(6)
_cell_length_b                   17.0804(9)
_cell_length_c                   24.3869(13)
_cell_measurement_reflns_used    2768
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.0460
_cell_measurement_theta_min      2.3810
_cell_volume                     4472.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0303
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.773
_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      5.00  57.00   1.00  175.00    --   13.76  57.00 150.00   52
  2  \w    -43.00   7.00   1.00  175.00    --   13.76 -57.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0584735000
_diffrn_orient_matrix_UB_12      -0.0190498000
_diffrn_orient_matrix_UB_13      -0.0023636000
_diffrn_orient_matrix_UB_21      -0.0306548000
_diffrn_orient_matrix_UB_22      0.0365800000
_diffrn_orient_matrix_UB_23      0.0026521000
_diffrn_orient_matrix_UB_31      0.0019767000
_diffrn_orient_matrix_UB_32      0.0049024000
_diffrn_orient_matrix_UB_33      -0.0288665000
_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  0.0317
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.773
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            10136
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.773
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.202
_diffrn_reflns_theta_min         2.385
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.452
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       needle
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.275
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0428P)^2^+6.3202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1166
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3369
_reflns_number_total             4696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj02563j2.cif
_cod_data_source_block           s1
_cod_database_code               7064201
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C168 H248 Br24 N24 '
_shelx_estimated_absorpt_t_max   0.485
_shelx_estimated_absorpt_t_min   0.455
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C18(H18A,H18B), C20(H20A,H20B), C17(H17A,H17B), C19(H19A,
 H19B), C13(H13A,H13B), C11(H11A,H11B), C10(H10A,H10B), C9(H9A,H9B), C12(H12A,
 H12B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C2(H2), C3(H3)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              438
_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 1.504
_oxdiff_exptl_absorpt_empirical_full_min 0.736