Co(iii) corroles with pendant amidophenol and amidopyridine as proton-relay arms to facilitate the electrocatalytic hydrogen evolution reaction
Cao, Xu-You; Xu, Shi-Yin; Wu, Ling-Wei; Qiu, Yi-Feng; Zhang, Hao; Si, Li-Ping; Wang, Li-Ming; Liu, Hai-Yang; Catalysis Science & Technology 14 (2024) 5608–5615; doi:10.1039/D4CY00677A

data_1572237
_publ_section_title
;
 Co(iii) corroles with pendant amidophenol and amidopyridine as
 proton-relay arms to facilitate the electrocatalytic hydrogen evolution
 reaction
;
_journal_issue                   19
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              5608
_journal_page_last               5615
_journal_paper_doi               10.1039/D4CY00677A
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C65 H36 Co F10 N4 O2 P'
_chemical_formula_sum            'C65 H36 Co F10 N4 O2 P'
_chemical_formula_weight         1184.88
_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     dual
_audit_creation_date             2023-09-28
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-03-06 deposited with the CCDC.	2024-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.3670(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8638(3)
_cell_length_b                   27.6166(10)
_cell_length_c                   22.2046(8)
_cell_measurement_reflns_used    7947
_cell_measurement_temperature    170
_cell_measurement_theta_max      26.310
_cell_measurement_theta_min      2.396
_cell_volume                     5426.0(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32745
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.398
_diffrn_reflns_theta_min         2.356
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  0.0151
_exptl_absorpt_correction_T_min  0.0033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1323 before and 0.0637 after correction.
The Ratio of minimum to maximum transmission is 0.2185.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
TITL 928co_0m_a.res in P2(1)/c
CELL    8.8638   27.6166   22.2046     90.00     93.37     90.00
SPGR P21/c
C101 0.990 0.556 0.210 !       6.80 eA-3
C102 0.170 0.024 0.400 !       6.15 eA-3
C103 0.717 0.588 0.193 !       2.15 eA-3
C104 0.816 0.944 0.672 !       2.08 eA-3
Q105 0.428 0.187 0.805 !       0.73 eA-3
Q106 0.451 0.755 0.365 !       0.70 eA-3
Q107 0.575 0.756 0.460 !       0.70 eA-3
Q108 0.275 0.305 0.360 !       0.68 eA-3
Q109 0.236 0.289 0.337 !       0.64 eA-3
Q110 0.838 0.968 0.117 !       0.62 eA-3
Q111 0.951 0.104 0.945 !       0.62 eA-3
Q112 0.586 0.835 0.392 !       0.62 eA-3
Q113 0.294 0.331 0.546 !       0.56 eA-3
Q114 0.161 0.601 0.771 !       0.56 eA-3
Q115 0.218 0.461 0.698 !       0.55 eA-3
Q116 0.538 0.471 0.708 !       0.54 eA-3
Q117 0.819 0.975 0.231 !       0.54 eA-3
Q118 0.280 0.179 0.274 !       0.53 eA-3
Q119 0.608 0.357 0.493 !       0.53 eA-3
Q120 0.615 0.109 0.797 !       0.53 eA-3
Q121 0.051 0.345 0.235 !       0.53 eA-3
Q122 0.899 0.773 0.059 !       0.52 eA-3
Q123 0.320 0.852 0.640 !       0.52 eA-3
Q124 0.581 0.727 0.658 !       0.50 eA-3
;
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         10843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0671
_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^)+(0.0821P)^2^+4.8762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1928
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7811
_reflns_number_total             10843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cy00677a2.cif
_cod_data_source_block           928co_0m_sq
_cod_depositor_comments
'Adding full bibliography for 1572236--1572237.cif.'
_cod_database_code               1572237
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.938
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C33(H33), C29(H29), C63(H63), C48(H48), C50(H50), C27(H27), C64(H64),
 C59(H59), C34(H34), C60(H60), C35(H35), C18(H18), C44(H44), C11(H11), C47(H47),
  C42(H42), C8(H8), C2(H2), C16(H16), C14(H14), C43(H43), C15(H15), C17(H17),
 C6(H6), C12(H12), C9(H9), C10(H10), C5(H5), C3(H3), C4(H4)
2.b Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C39(H39A,H39B,H39C)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'