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_1571256
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-05-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-08-21 deposited with the CCDC.	2024-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.727(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7857(16)
_cell_length_b                   14.519(2)
_cell_length_c                   11.7467(18)
_cell_measurement_reflns_used    1817
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.6420
_cell_measurement_theta_min      3.8620
_cell_volume                     1787.0(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (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 0.998
_diffrn_measured_fraction_theta_max 0.845
_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     -6.00  19.00   1.00   11.26    --   10.68 -77.00-120.00   25
  2  \w    -22.00  47.00   1.00   11.26    --  -10.84  38.00 -60.00   69
  3  \w    -47.00  58.00   1.00   11.26    --  -10.84  19.00  60.00  105
;
_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      -0.0238354000
_diffrn_orient_matrix_UB_12      0.0365069000
_diffrn_orient_matrix_UB_13      0.0291213000
_diffrn_orient_matrix_UB_21      -0.0500031000
_diffrn_orient_matrix_UB_22      0.0073939000
_diffrn_orient_matrix_UB_23      -0.0504624000
_diffrn_orient_matrix_UB_31      -0.0389993000
_diffrn_orient_matrix_UB_32      -0.0316035000
_diffrn_orient_matrix_UB_33      0.0214598000
_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  0.0678
_diffrn_reflns_av_unetI/netI     0.0882
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9181
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.385
_diffrn_reflns_theta_min         3.414
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.320
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       prism
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.0121(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0562P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2403
_reflns_number_total             4160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cy01732j2.cif
_cod_data_source_block           m2szbr
_cod_depositor_comments
'Adding full bibliography for 1571255--1571256.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1571256
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H18 Br1 N3 O2'
_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:
 C3(H3A,H3B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16),
 C20(H20)
2.c X=CH2 refined with riding coordinates:
 C5(H5A,H5B)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_shelx_res_checksum              44895
_shelx_hkl_checksum              55151
_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 2.434
_oxdiff_exptl_absorpt_empirical_full_min 0.542