Comprehensive enhancement in electrocatalytic oxygen evolution performance of nickel and cobalt complexes derived from π-conjugated N-heterocyclic carbene ligands through carbon composite strategy
Vijayakumar, Monica; Yhobu, Zhoveta; Małecki, Jan Grzegorz; Nagaraju, Dodahhali H.; Keri, Rangappa S.; Budagumpi, Srinivasa; Catalysis Science & Technology 14 (2024) 2489–2502; doi:10.1039/D3CY01732J

data_1571255
_publ_section_title
;
 Comprehensive enhancement in electrocatalytic oxygen evolution
 performance of nickel and cobalt complexes derived from \p-conjugated
 N-heterocyclic carbene ligands through carbon composite strategy
;
_journal_issue                   9
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              2489
_journal_page_last               2502
_journal_paper_doi               10.1039/D3CY01732J
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C20 H18 N3 O2, Br'
_chemical_formula_sum            'C20 H18 Br N3 O2'
_chemical_formula_weight         412.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-02-26
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2023-08-21 deposited with the CCDC.	2024-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.883(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4985(8)
_cell_length_b                   16.3402(11)
_cell_length_c                   8.5914(4)
_cell_measurement_reflns_used    2692
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.7450
_cell_measurement_theta_min      3.7730
_cell_volume                     1866.87(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (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 0.861
_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     15.00  45.00   1.00   20.47    --    9.90 -99.00  60.00   30
  2  \w     18.00  45.00   1.00   20.47    --    9.90 -99.00  90.00   27
  3  \w    -88.00  42.00   1.00   20.47    --  -11.62   0.00 -90.00  130
;
_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      -0.0366160000
_diffrn_orient_matrix_UB_12      0.0305985000
_diffrn_orient_matrix_UB_13      0.0050274000
_diffrn_orient_matrix_UB_21      0.0251116000
_diffrn_orient_matrix_UB_22      0.0269185000
_diffrn_orient_matrix_UB_23      -0.0450286000
_diffrn_orient_matrix_UB_31      -0.0295460000
_diffrn_orient_matrix_UB_32      -0.0150116000
_diffrn_orient_matrix_UB_33      -0.0704605000
_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  0.0287
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9246
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.358
_diffrn_reflns_theta_min         3.308
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.221
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       plate
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0412P)^2^+0.9845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2682
_reflns_number_total             4428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cy01732j2.cif
_cod_data_source_block           s3br2
_cod_depositor_comments
'Adding full bibliography for 1571255--1571256.cif.'
_cod_original_cell_volume        1866.86(19)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1571255
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H18 Br1 N3 O2'
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13), C14(H14)
2.c X=CH2 refined with riding coordinates:
 C19(H19A,H19B)
2.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_shelx_res_checksum              65030
_shelx_hkl_checksum              2941
_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 1.292
_oxdiff_exptl_absorpt_empirical_full_min 0.789