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_7063919
_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
'C64 H34 Co4 N16 O11 S8, 2(C6 H16 N), 1[C3H7NO], 2[H2O]'
_chemical_formula_sum            'C79 H77 Co4 N19 O14 S8'
_chemical_formula_weight         2008.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 110.240(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4593(6)
_cell_length_b                   25.0962(7)
_cell_length_c                   21.9318(6)
_cell_measurement_reflns_used    28941
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4320
_cell_measurement_theta_min      2.4840
_cell_volume                     9016.3(5)
_computing_cell_refinement       'CrysAlisPro 1.171.44.111a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 39.46 (release 15-03-2018))'
_computing_data_reduction        'CrysAlisPro 1.171.44.111a (Rigaku OD, 2025)'
_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-ac6-016 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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    -45.00  16.00   0.50   20.00    --   -9.95 102.00  70.00  122
  2  \w      6.00  45.00   0.50   20.00    --   10.22-102.00 -32.00   78
  3  \w    -56.00  -4.00   0.50   20.00    --   -9.95 125.00 120.00  104
  4  \w    -55.00 -25.00   0.50   20.00    --   -9.95 125.00-180.00   60
  5  \w    -56.00  -7.00   0.50   20.00    --   -9.95 125.00 -30.00   98
  6  \w    -23.00  36.00   0.50   20.00    --   -9.95  38.00 -90.00  118
  7  \w    -72.00 -44.00   0.50   20.00    --   -9.95 -57.00 -30.00   56
  8  \w    -33.00   4.00   0.50   20.00    --   10.22 117.00-157.40   74
  9  \w      4.00  35.00   0.50   20.00    --   10.22-125.00-180.00   62
 10  \w    -60.00 -13.00   0.50   20.00    --   10.22 -19.00 -90.00   94
 11  \w    -35.00  -9.00   0.50   20.00    --   10.22 121.00 -23.18   52
 12  \w      3.00  28.00   0.50   20.00    --   10.22 -57.00-120.00   50
 13  \w      6.00  32.00   0.50   20.00    --   10.22  38.00 -30.00   52
 14  \w    -54.00   6.00   0.50   20.00    --   10.22 -19.00 -60.00  120
 15  \w    -54.00 -27.00   0.50   20.00    --   10.22 -38.00-180.00   54
;
_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  0.0625
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45759
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.120
_diffrn_reflns_theta_max         25.120
_diffrn_reflns_theta_min         2.102
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51136
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.111a (Rigaku Oxford Diffraction, 2025)
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    1.480
_exptl_crystal_description       block
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.030
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         7994
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0503
_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^)+(0.1001P)^2^+3.0400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1593
_refine_ls_wR_factor_ref         0.1672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6260
_reflns_number_total             7994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01208b2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7063918--7063919.cif.'
_cod_database_code               7063919
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{N9, N9A}
3. Restrained distances
 N9-C37
 1.5 with sigma of 0.01
 C38-C37
 1.5 with sigma of 0.01
 N9-C38
 2.5 with sigma of 0.01
 N9A-N9 = N9-O2
 2.9 with sigma of 0.02
 C33A-N9A
 1.4 with sigma of 0.01
 N9-C33 \\sim N9-C37 \\sim N9-C35
 with sigma of 0.01
 N9-C38 \\sim N9A-C38A
 with sigma of 0.04
 N9-C35 \\sim N9A-C35A
 with sigma of 0.02
 C37-C38 \\sim C37A-C38A
 with sigma of 0.02
 N9-C33 \\sim N9A-C33A
 with sigma of 0.02
 C38-C37 \\sim C34-C33 \\sim C36-C35
 with sigma of 0.01
 N9-C37 \\sim N9A-C37A
 with sigma of 0.02
 C33-C35 \\sim C35-C37 \\sim C37-C33
 with sigma of 0.02
 N9-C36 \\sim N9A-C36A
 with sigma of 0.04
 N9-C34 \\sim N9A-C34A
 with sigma of 0.04
 N9-C34 \\sim N9-C36 \\sim N9-C38
 with sigma of 0.02
 C35-C36 \\sim C35A-C36A
 with sigma of 0.02
 C33-C34 \\sim C33A-C34A
 with sigma of 0.02
 C35-C33 \\sim C35A-C33A
 with sigma of 0.04
 C35-C37 \\sim C35A-C37A
 with sigma of 0.04
 C33-C37 \\sim C33A-C37A
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(N9A) = Uanis(C35A) = Uanis(C33A) = Uanis(C37A) = Uanis(C36A) =
Uanis(C34A) = Uanis(C38A) = Uanis(C35) = Uanis(N9) = Uanis(C33) = Uanis(C37) =
Uanis(C36) = Uanis(C34) = Uanis(C38)
5. Others
 Sof(N9A)=Sof(H9A)=Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=
 Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=
 Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C38A)=Sof(H38D)=Sof(H38E)=
 Sof(H38F)=1-FVAR(1)
 Sof(N9)=Sof(H9)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C33)=Sof(H33A)=Sof(H33B)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C36)=
 Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Fixed Sof: H7(0.5) H6(0.5)
6.a Ternary CH refined with riding coordinates:
 N9(H9), N9A(H9A)
6.b Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C33(H33A,H33B), C37(H37A,H37B), C35A(H35C,H35D), C33A(H33C,
 H33D), C37A(H37C,H37D)
6.c Me refined with riding coordinates:
 C38(H38A,H38B,H38C), C36(H36A,H36B,H36C), C34(H34A,H34B,H34C), C36A(H36D,H36E,
 H36F), C34A(H34D,H34E,H34F), C38A(H38D,H38E,H38F)
6.d Aromatic/amide H refined with riding coordinates:
 C12(H12), C28(H28), C15(H15), C31(H31), C29(H29), C30(H30), C14(H14),
 C18(H18), C13(H13), C20(H20), C19(H19), C21(H21), C2(H2), C3(H3), C5(H5),
 C4(H4)
;
_shelx_res_checksum              97876
_shelx_fab_checksum              54454
_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
;