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_7060413
_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 F9.59 N7 O, 0.41(F)'
_chemical_formula_sum            'C44 H21 F10 N7 O'
_chemical_formula_weight         853.68
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-03 deposited with the CCDC.	2021-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.953(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.535(2)
_cell_length_b                   26.456(2)
_cell_length_c                   9.6766(10)
_cell_measurement_reflns_used    1307
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      53.3610
_cell_measurement_theta_min      3.0770
_cell_volume                     4356.6(8)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(13)
_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 0.967
_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     34.00  81.00   1.00    2.00    --   40.98 -99.00 -30.00   47
  2  \w     81.00 126.00   1.00    4.00    --  106.95 -61.00   0.00   45
  3  \w     80.00 107.00   1.00    4.00    --  106.95-125.00  30.00   27
  4  \w     39.00 102.00   1.00    4.00    --  106.95 -94.00 150.00   63
  5  \w     37.00  64.00   1.00    4.00    --  106.95-125.00  30.00   27
  6  \w     34.00 121.00   1.00    4.00    --  106.95-125.00  60.00   87
  7  \w     34.00  96.00   1.00    4.00    --  106.95 -45.00 120.00   62
  8  \w     81.00 176.00   1.00    4.00    --  106.95  30.00 150.00   95
  9  \w    102.00 162.00   1.00    4.00    --  106.95  77.00-180.00   60
 10  \w      1.00  57.00   1.00    2.00    --   40.98 -99.00-180.00   56
 11  \w   -112.00   0.00   1.00    2.00    --  -40.98 -19.00 -60.00  112
;
_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      -0.0643081000
_diffrn_orient_matrix_UB_12      -0.0310662000
_diffrn_orient_matrix_UB_13      0.0450395000
_diffrn_orient_matrix_UB_21      -0.0444384000
_diffrn_orient_matrix_UB_22      0.0491357000
_diffrn_orient_matrix_UB_23      0.0157359000
_diffrn_orient_matrix_UB_31      -0.0456306000
_diffrn_orient_matrix_UB_32      -0.0040734000
_diffrn_orient_matrix_UB_33      -0.1568738000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.1069
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17085
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.106
_diffrn_reflns_theta_min         2.596
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.961
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47103
_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    1.302
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         8557
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1632
_refine_ls_R_factor_gt           0.0998
_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^)+(0.1515P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2629
_refine_ls_wR_factor_ref         0.3230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3988
_reflns_number_total             8557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04953k2.cif
_cod_data_source_block           cho
_cod_depositor_comments
'Adding full bibliography for 7060413--7060416.cif.'
_cod_original_cell_volume        4356.7(8)
_cod_database_code               7060413
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.893
_reflns_odcompleteness_completeness 99.94
_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. Restrained distances
 H4-N4
 0.84 with sigma of 0.02
3. Rigid bond restraints
 C36, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C38, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C36 \\sim C37: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C38 \\sim C37: within 2A with sigma of 0.0002 and sigma for terminal atoms of
0.0004
5. Others
 Sof(F4)=1-FVAR(1)
 Sof(F2AA)=FVAR(1)
 Sof(F3)=1-FVAR(2)
 Sof(F16)=FVAR(2)
 Sof(F1AB)=1-FVAR(3)
 Sof(F5)=FVAR(3)
 Sof(F7)=1-FVAR(4)
 Sof(F1AA)=FVAR(4)
 Sof(F6)=1-FVAR(5)
 Sof(F01J)=FVAR(5)
 Sof(F01L)=1-FVAR(6)
 Sof(F10)=FVAR(6)
 Sof(F9)=1-FVAR(7)
 Sof(F3AA)=FVAR(7)
 Sof(C44)=1-FVAR(8)
 Sof(C0AA)=FVAR(8)
 Sof(C43)=1-FVAR(9)
 Sof(C1AA)=FVAR(9)
 Sof(C19A)=1-FVAR(10)
 Sof(C36)=FVAR(10)
 Sof(C44A)=1-FVAR(11)
 Sof(C35)=FVAR(11)
6.a Aromatic/amide H refined with riding coordinates:
 N6(H6), C8(H8), C24(H24), C7(H7), C22(H22), C26(H26), C2(H2A), C11(H11),
 C3(H3), C25(H25), C12(H12), C21(H21), C16(H16), C31(H31), C32(H32), C17(H17),
 C29(H29), C30(H30)
;
_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 1.626
_oxdiff_exptl_absorpt_empirical_full_min 0.556