Influence of structural diversity in Co(ii)–oxamide complexes towards single molecule magnets and electrochemical oxygen evolution reaction
Nag, Swati; Kumar, Raman; Singh, Manjeet; Panda, Atanu; Patra, Ranjan; Sahu, Pradip Kumar; Goswami, Soumyabrata; Sahoo, Subash C.; Nanda, Prasant K.; New Journal of Chemistry 49 (2025) 15236–15251; doi:10.1039/D5NJ01208B

data_7063918
_publ_section_title
;
 Influence of structural diversity in Co(ii)--oxamide complexes towards
 single molecule magnets and electrochemical oxygen evolution reaction
;
_journal_issue                   35
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15236
_journal_page_last               15251
_journal_paper_doi               10.1039/D5NJ01208B
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C36 H32 Co2 N14 O4 S2'
_chemical_formula_sum            'C36 H32 Co2 N14 O4 S2'
_chemical_formula_weight         906.74
_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
_audit_creation_date             2025-07-17
_audit_creation_method
;
Olex2 1.5-ac6-016
(compiled 2024.01.13 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6897)
;
_audit_update_record
;
2025-07-17 deposited with the CCDC.	2025-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                113.382(8)
_cell_angle_beta                 101.243(6)
_cell_angle_gamma                109.981(8)
_cell_formula_units_Z            1
_cell_length_a                   10.1438(8)
_cell_length_b                   10.8180(10)
_cell_length_c                   11.0892(7)
_cell_measurement_reflns_used    8093
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.2570
_cell_measurement_theta_min      3.3880
_cell_volume                     969.58(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5-ac6-016 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-016 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.934
_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    -60.00 -35.00   0.50   25.00    --   -9.91 -40.00  47.00   50
  2  \w    -10.00  53.00   0.50   25.00    --   -9.91  40.00-159.00  126
  3  \w     29.00  55.00   0.50   25.00    --   10.22  40.00-159.00   52
  4  \w    -52.00  21.00   0.50   25.00    --   10.22 -40.00  47.00  146
  5  \w    -33.00  -7.00   0.50   25.00    --   -9.91  77.00 -60.00   52
  6  \w    -74.00 -34.00   0.50   25.00    --   -9.91 -77.00   0.00   80
  7  \w    -56.00 -21.00   0.50   25.00    --   -9.91 125.00  90.00   70
  8  \w     23.00  55.00   0.50   25.00    --   -9.91  77.00 -60.00   64
  9  \w     -3.00  24.00   0.50   25.00    --   10.22  38.00 120.00   54
 10  \w    -13.00  18.00   0.50   25.00    --   10.22  77.00-120.00   62
 11  \w     21.00  54.00   0.50   25.00    --   10.22-125.00 -90.00   66
 12  \w     -2.00  67.00   0.50   25.00    --   10.22  19.00   0.00  138
 13  \w     36.00  74.00   0.50   25.00    --   10.22  77.00-120.00   76
 14  \w     49.00  74.00   0.50   25.00    --   10.22  38.00-120.00   50
 15  \w      3.00  59.00   0.50   25.00    --   10.22-125.00  60.00  112
 16  \w     11.00  39.00   0.50   25.00    --   10.22 -99.00 -30.00   56
 17  \w     -5.00  74.00   0.50   25.00    --   10.22  77.00 120.00  158
 18  \w    -35.00   1.00   0.50   25.00    --   10.22 120.00 -76.53   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1571
_diffrn_reflns_av_unetI/netI     0.0907
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12691
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.441
_diffrn_reflns_theta_min         3.394
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.31d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.012
_exptl_crystal_size_min          0.006
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4140
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0851
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1674P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2326
_refine_ls_wR_factor_ref         0.2634
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2847
_reflns_number_total             4140
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01208b2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7063918--7063919.cif.'
_cod_original_cell_volume        969.58(15)
_cod_database_code               7063918
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Co1-H2A \\sim Co1-H2B
 with sigma of 0.02
 N6-C9 \\sim N6-C9A
 with sigma of 0.02
 N6-C13 \\sim N6-C13A
 with sigma of 0.02
 C9-C10 \\sim C9A-C10A
 with sigma of 0.02
 C10-C11 \\sim C10A-C11A
 with sigma of 0.02
 C11-C12 \\sim C11A-C12A
 with sigma of 0.02
 C12-C13 \\sim C12A-C13A
 with sigma of 0.02
 N6-C10 \\sim N6-C10A
 with sigma of 0.04
 N6-C12 \\sim N6-C12A
 with sigma of 0.04
 C9-C11 \\sim C9A-C11A
 with sigma of 0.04
 C10-C12 \\sim C10A-C12A
 with sigma of 0.04
 C11-C13 \\sim C11A-C13A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C13A) = Uanis(C12A) = Uanis(C11A) = Uanis(C10A) = Uanis(C9A)
4. Rigid body (RIGU) restrains
 C9, C12, C10, C13, C11, N6
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C13A, C11A, C9A, C12A, C10A
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
5. Others
 Sof(C13A)=Sof(H13A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=
 Sof(C12A)=Sof(H12A)=1-FVAR(1)
 Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=
 Sof(C13)=Sof(H13)=FVAR(1)
6.a Free rotating group:
 O2(H2A,H2B)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C14(H14), C18(H18), C9(H9), C15(H15), C3(H3), C16(H16), C10(H10),
 C11(H11), C17(H17), C5(H5), C4(H4), C12(H12), C13(H13), C13A(H13A), C9A(H9A),
 C10A(H10A), C11A(H11A), C12A(H12A)
;
_shelx_res_checksum              54631
_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
;