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_7719346
_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         'C28 H20 Co N4 O10, C6 H16 N, H2 O'
_chemical_formula_sum            'C34 H38 Co N5 O11'
_chemical_formula_weight         751.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2025-03-13
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-05-12 deposited with the CCDC.	2025-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.828(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9680(6)
_cell_length_b                   18.6450(9)
_cell_length_c                   13.7485(6)
_cell_measurement_reflns_used    6041
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.3640
_cell_measurement_theta_min      4.0010
_cell_volume                     3307.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.90 (release 15-09-2023))'
_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      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4015
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.858
_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    -30.00  26.00   1.00   36.03    --  -10.76  77.00 120.00   56
  2  \w     28.00  63.00   1.00   36.03    --  -10.76  38.00 120.00   35
  3  \w    -83.00  10.00   1.00   36.03    --  -10.76 -57.00  30.00   93
  4  \w    -59.00  39.00   1.00   36.03    --   10.76 -57.00 150.00   98
;
_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      0.0503195000
_diffrn_orient_matrix_UB_12      0.0082892000
_diffrn_orient_matrix_UB_13      0.0222758000
_diffrn_orient_matrix_UB_21      0.0170657000
_diffrn_orient_matrix_UB_22      -0.0349211000
_diffrn_orient_matrix_UB_23      -0.0111268000
_diffrn_orient_matrix_UB_31      0.0141027000
_diffrn_orient_matrix_UB_32      0.0126037000
_diffrn_orient_matrix_UB_33      -0.0454998000
_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  0.0394
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19675
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.505
_diffrn_reflns_theta_min         3.407
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       prism
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         7900
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.0704
_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^)+(0.0955P)^2^+3.9177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1787
_refine_ls_wR_factor_ref         0.2151
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4998
_reflns_number_total             7900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01680k2.cif
_cod_data_source_block           anpovco
_cod_depositor_comments
'Adding full bibliography for 7719344--7719347.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7719346
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C29 H21 N4 O10 Co1'
_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, All O(H,H) groups
2. Restrained distances
 H5A-N5
 1 with sigma of 0.02
 C33-C34
 1.4 with sigma of 0.02
3.a Riding coordinates:
 O11(H11A,H11B), C29(H29A,H29B), C30(H30A,H30B,H30C), C31(H31A,H31B), C32(H32A,
 H32B,H32C), C33(H33A,H33B), C34(H34A,H34B,H34C)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C15(H15),
 C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C27(H27)
3.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              74268
_shelx_hkl_checksum              63752
_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 1.187
_oxdiff_exptl_absorpt_empirical_full_min 0.909