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_7060415
_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      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                94.017(4)
_cell_angle_beta                 93.627(5)
_cell_angle_gamma                93.244(5)
_cell_formula_units_Z            2
_cell_length_a                   8.5533(5)
_cell_length_b                   12.3838(7)
_cell_length_c                   23.3415(12)
_cell_measurement_reflns_used    5186
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.5820
_cell_measurement_theta_min      2.6410
_cell_volume                     2456.7(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -12.00  79.00   1.00    6.50    --   11.74  57.00  60.00   91
  2  \w     40.00  66.00   1.00    6.50    --   11.74 178.00-120.00   26
  3  \w    -15.00  80.00   1.00    6.50    --   11.74  77.00-180.00   95
  4  \w    -59.00  38.00   1.00    6.50    --   11.74 -57.00 -90.00   97
;
_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      -0.0109068000
_diffrn_orient_matrix_UB_12      0.0120057000
_diffrn_orient_matrix_UB_13      -0.0292012000
_diffrn_orient_matrix_UB_21      -0.0026811000
_diffrn_orient_matrix_UB_22      -0.0561609000
_diffrn_orient_matrix_UB_23      -0.0086755000
_diffrn_orient_matrix_UB_31      -0.0824894000
_diffrn_orient_matrix_UB_32      -0.0033202000
_diffrn_orient_matrix_UB_33      0.0020628000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17642
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.318
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65970
_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    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.054
_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     658
_refine_ls_number_reflns         8657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0492P)^2^+0.7122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1221
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6533
_reflns_number_total             8657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04953k2.cif
_cod_data_source_block           copph3
_cod_depositor_comments
'Adding full bibliography for 7060413--7060416.cif.'
_cod_database_code               7060415
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C49(H49), C19(H19), C23(H23), C10(H10), C18(H18), C14(H14), C43(H43), C9(H9),
 C15(H15), C24(H24), C6(H6), C2(H2), C48(H48), C55(H55), C45(H45), C51(H51),
 C39(H39), C5(H5), C42(H42), C4(H4), C53(H53), C41(H41), C54(H54), C46(H46),
 C47(H47), C52(H52), C40(H40), C56(H56)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              20499
_shelx_fab_checksum              54378
_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 1.569
_oxdiff_exptl_absorpt_empirical_full_min 0.583