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_7060414
_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         'C44 H21 F10 N7 O'
_chemical_formula_sum            'C44 H21 F10 N7 O'
_chemical_formula_weight         853.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   41.430(4)
_cell_length_b                   16.3457(14)
_cell_length_c                   12.9588(16)
_cell_measurement_reflns_used    3141
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      62.4910
_cell_measurement_theta_min      2.8910
_cell_volume                     8775.7(16)
_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  (Sheldrick, 2015)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.958
_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    -81.00  46.00   1.00    4.00    --  -41.23   0.00-180.00  127
  2  \w     43.00  69.00   1.00    4.00    --   41.23-125.00  30.00   26
  3  \w     30.00  58.00   1.00    4.00    --   41.23-125.00 120.00   28
  4  \w     35.00 126.00   1.00    5.00    --  106.95 -45.00  30.00   91
  5  \w    127.00 154.00   1.00    5.00    --  106.95  61.00  60.00   27
  6  \w     78.00 104.00   1.00    5.00    --  106.95  61.00  60.00   26
  7  \w     37.00 130.00   1.00    5.00    --  106.95 -61.00 -90.00   93
  8  \w     43.00  95.00   1.00    5.00    --  106.95 -95.00-150.00   52
  9  \w     83.00 112.00   1.00    8.00    --   41.23  77.00-150.00   29
 10  \w    123.00 164.00   1.00   10.00    --  106.95  77.00  60.00   41
 11  \w     46.00  72.00   1.00   10.00    --  106.95 -95.00 169.00   26
;
_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      0.0225101000
_diffrn_orient_matrix_UB_12      -0.0697414000
_diffrn_orient_matrix_UB_13      0.0341002000
_diffrn_orient_matrix_UB_21      0.0289748000
_diffrn_orient_matrix_UB_22      0.0454585000
_diffrn_orient_matrix_UB_23      -0.0482137000
_diffrn_orient_matrix_UB_31      0.0060259000
_diffrn_orient_matrix_UB_32      0.0441251000
_diffrn_orient_matrix_UB_33      0.1032335000
_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  0.0698
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            27395
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.714
_diffrn_reflns_theta_min         2.133
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.954
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55375
_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    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.00015(4)
_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   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         8624
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1388
_refine_ls_R_factor_gt           0.0851
_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^)+(0.1288P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2324
_refine_ls_wR_factor_ref         0.2883
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4282
_reflns_number_total             8624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04953k2.cif
_cod_data_source_block           jianfree
_cod_depositor_comments
'Adding full bibliography for 7060413--7060416.cif.'
_cod_database_code               7060414
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N2(H2), N6(H6), C4(H4A), C37(H37), C3(H3), C33(H33), C18(H18),
 C17(H17), C34(H34), C35(H35), C38(H38), C42(H42), C41(H41), C14(H14), C44(H44),
  C8(H8), C43(H43), C9(H9), C13(H13)
;
_shelx_res_checksum              74721
_shelx_fab_checksum              80068
_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 2.153
_oxdiff_exptl_absorpt_empirical_full_min 0.697