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_7719345
_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         'C32 H30 Co N2 O6, C6 H16 N, 2(H2 O)'
_chemical_formula_sum            'C38 H50 Co N3 O8'
_chemical_formula_weight         735.74
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2025-03-10
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2585(8)
_cell_length_b                   20.1967(12)
_cell_length_c                   11.8280(5)
_cell_measurement_reflns_used    5480
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.8060
_cell_measurement_theta_min      3.7310
_cell_volume                     3645.1(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)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.880
_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    -73.00  38.00   1.00   32.47    --  -10.76   0.00  60.00  111
  2  \w    -82.00 -56.00   1.00   32.47    --  -10.76 -38.00   0.00   26
  3  \w      6.00  39.00   1.00   32.47    --   10.92  77.00-150.00   33
  4  \w     21.00  47.00   1.00   32.47    --   10.92 -99.00 -90.00   26
;
_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      -0.0440465000
_diffrn_orient_matrix_UB_12      -0.0101021000
_diffrn_orient_matrix_UB_13      -0.0084596000
_diffrn_orient_matrix_UB_21      -0.0143165000
_diffrn_orient_matrix_UB_22      0.0247887000
_diffrn_orient_matrix_UB_23      0.0382427000
_diffrn_orient_matrix_UB_31      -0.0038921000
_diffrn_orient_matrix_UB_32      0.0227272000
_diffrn_orient_matrix_UB_33      -0.0454327000
_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  0.0397
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15184
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.779
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.500
_diffrn_reflns_theta_min         3.445
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74643
_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_density_diffrn    1.341
_exptl_crystal_description       plate
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 'Flack (1983), 5640 Friedel pairs'
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         7909
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0652P)^2^+0.9691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1474
_reflns_Friedel_coverage         0.692
_reflns_Friedel_fraction_full    0.880
_reflns_Friedel_fraction_max     0.668
_reflns_number_gt                5640
_reflns_number_total             7909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01680k2.cif
_cod_data_source_block           ajpoetco
_cod_depositor_comments
'Adding full bibliography for 7719344--7719347.cif.'
_cod_database_code               7719345
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C32 H30 N2 O6 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.a Free rotating group:
 O7(H7A,H7B), O8(H8A,H8B)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C31(H31A,H31B), C33(H33A,H33B), C35(H35A,H35B), C37(H37A,H37B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C19(H19),
 C20(H20), C22(H22), C23(H23), C27(H27), C28(H28), C29(H29)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C30(H30A,H30B,H30C), C32(H32A,H32B,
 H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              86470
_shelx_hkl_checksum              5749
_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 1.400
_oxdiff_exptl_absorpt_empirical_full_min 0.780