Synthesis of cobalt A2B triaryl corroles bearing aldehyde and amide pyridyl groups and their performance in electrocatalytic hydrogen evolution
Fang, Jun-Jia; Lan, Jian; Yang, Gang; Yuan, Gao-Qing; Liu, Hai-Yang; Si, Li-Ping; New Journal of Chemistry 45 (2021) 5127–5136; doi:10.1039/D0NJ04953K

data_7060416
_publ_section_title
;
 Synthesis of cobalt A2B triaryl corroles bearing aldehyde and amide
 pyridyl groups and their performance in electrocatalytic hydrogen
 evolution
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5127
_journal_page_last               5136
_journal_paper_doi               10.1039/D0NJ04953K
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C56 H28 Co F10 N4 O P'
_chemical_formula_sum            'C56 H28 Co F10 N4 O P'
_chemical_formula_weight         1052.72
_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             2020-01-07
_audit_creation_method
;
Olex2 1.3-alpha
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-01-07 deposited with the CCDC.	2021-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.160(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6531(6)
_cell_length_b                   32.9883(15)
_cell_length_c                   10.9968(4)
_cell_measurement_reflns_used    3549
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.4270
_cell_measurement_theta_min      3.3760
_cell_volume                     5176.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.972
_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     13.00 105.00   1.00    1.50    --   41.23  57.00  90.00   92
  2  \w     86.00 178.00   1.00    2.00    --  106.95  45.00 120.00   92
  3  \w    126.00 152.00   1.00    2.00    --  106.95  61.00   0.00   26
  4  \w     76.00 170.00   1.00    2.00    --  106.95  77.00 150.00   94
  5  \w     29.00  62.00   1.00    2.00    --  106.95 -95.00-150.00   33
  6  \w     44.00  76.00   1.00    1.50    --   41.23 -99.00-180.00   32
  7  \w     50.00 119.00   1.00    2.00    --  106.95-125.00  90.00   69
  8  \w     26.00 109.00   1.00    2.00    --  106.95 -95.00 150.00   83
  9  \w    107.00 178.00   1.00    2.00    --  106.95 125.00-150.00   71
 10  \w    -65.00  31.00   1.00    1.50    --  -41.23  38.00-150.00   96
 11  \w    -66.00 -33.00   1.00    1.50    --  -41.23  38.00 120.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0969030000
_diffrn_orient_matrix_UB_12      0.0158524000
_diffrn_orient_matrix_UB_13      0.0102847000
_diffrn_orient_matrix_UB_21      -0.0356611000
_diffrn_orient_matrix_UB_22      -0.0439199000
_diffrn_orient_matrix_UB_23      0.0008766000
_diffrn_orient_matrix_UB_31      0.0318355000
_diffrn_orient_matrix_UB_32      -0.0009057000
_diffrn_orient_matrix_UB_33      0.1433840000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_unetI/netI     0.1155
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            21787
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.656
_diffrn_reflns_theta_min         2.679
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.579
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
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    1.351
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         10148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1385
_refine_ls_R_factor_gt           0.0768
_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^)+(0.0568P)^2^+2.7121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1692
_refine_ls_wR_factor_ref         0.1942
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5289
_reflns_number_total             10148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04953k2.cif
_cod_data_source_block           chd-co-2
_cod_depositor_comments
'Adding full bibliography for 7060413--7060416.cif.'
_cod_database_code               7060416
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.739
_shelx_estimated_absorpt_t_min   0.634
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C9(H9), C13(H13), C23(H23), C52(H52), C10(H10), C56(H56), C3(H3),
 C50(H50), C5(H5), C2(H2), C6(H6), C44(H44), C22(H22), C19(H19), C40(H40),
 C18(H18), C43(H43), C42(H42), C53(H53), C46(H46), C41(H41), C55(H55), C54(H54),
  C38(H38), C49(H49), C48(H48), C47(H47)
;
_shelx_res_checksum              60034
_shelx_fab_checksum              21780
_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 1.906
_oxdiff_exptl_absorpt_empirical_full_min 0.439