Tuning the ligand periphery in homoleptic Co(III) complexes: a versatile strategy to modulate electrocatalytic oxygen evolution reaction efficiency.
Aiswarya, Janardhanan; Madhu, Ragunath; Anitha, Ottoor; Malecki, Jan Grzegorz; Kundu, Subrata; Murugesapandian, Balasubramanian; Dalton transactions (Cambridge, England : 2003) 54 (2025) 14740–14752; doi:10.1039/d5dt01680k

data_7719344
_publ_section_title
;
 Tuning the ligand periphery in homoleptic Co(III) complexes: a versatile
 strategy to modulate electrocatalytic oxygen evolution reaction
 efficiency.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14740
_journal_page_last               14752
_journal_paper_doi               10.1039/d5dt01680k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C30 H26 Co N2 O6, C6 H16 N, 2(H2 O)'
_chemical_formula_sum            'C36 H46 Co N3 O8'
_chemical_formula_weight         707.69
_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     direct
_audit_creation_date             2024-08-03
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-05-12 deposited with the CCDC.	2025-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                96.621(4)
_cell_angle_beta                 109.747(5)
_cell_angle_gamma                106.675(5)
_cell_formula_units_Z            2
_cell_length_a                   11.3535(6)
_cell_length_b                   12.4969(7)
_cell_length_c                   13.5917(6)
_cell_measurement_reflns_used    95
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.2530
_cell_measurement_theta_min      5.3140
_cell_volume                     1689.84(18)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4015
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.815
_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    -77.00  11.00   1.00   44.47    --  -10.84 -57.00 120.00   88
  2  \w    -38.00  62.00   1.00   44.47    --  -10.84  57.00 -90.00  100
  3  \w    -17.00  38.00   1.00   44.47    --   10.84 -77.00   0.00   55
  4  \w    -19.00  21.00   1.00   44.47    --   10.84  77.00 120.00   40
  5  \w     37.00  68.00   1.00   44.47    --   10.84  38.00-150.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0369794000
_diffrn_orient_matrix_UB_12      0.0502912000
_diffrn_orient_matrix_UB_13      0.0213184000
_diffrn_orient_matrix_UB_21      -0.0845815000
_diffrn_orient_matrix_UB_22      -0.0189771000
_diffrn_orient_matrix_UB_23      0.0064339000
_diffrn_orient_matrix_UB_31      0.0053095000
_diffrn_orient_matrix_UB_32      -0.0486969000
_diffrn_orient_matrix_UB_33      0.0674387000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.815
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16370
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.815
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.465
_diffrn_reflns_theta_min         3.502
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       plate
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0868P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1660
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5354
_reflns_number_total             7660
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01680k2.cif
_cod_data_source_block           ajovco
_cod_depositor_comments
'Adding full bibliography for 7719344--7719347.cif.'
_cod_original_cell_volume        1689.82(16)
_cod_database_code               7719344
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C30 H26 N2 O6 Co1'
_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, All O(H,H) groups
2.a Free rotating group:
 O8(H8A,H8B), O7(H7A,H7B)
2.b Ternary CH refined with riding coordinates:
 N3(H3)
2.c Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C33(H33A,H33B), C35(H35A,H35B)
2.d Aromatic/amide H refined with riding coordinates:
 C19(H19), C1(H1), C11(H11), C20(H20), C21(H21), C7(H7), C24(H24), C15(H15),
 C10(H10), C6(H6), C13(H13), C27(H27), C5(H5), C25(H25)
2.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C28(H28A,H28B,
 H28C), C36(H36A,H36B,H36C), C34(H34A,H34B,H34C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              84581
_shelx_hkl_checksum              11651
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.474
_oxdiff_exptl_absorpt_empirical_full_min 0.406