One-pot gram-scale rapid synthesis of MN<sub>4</sub> complexes with 14-membered ring macrocyclic ligand as a precursor for carbon-based ORR and CO<sub>2</sub>RR catalysts.
Ogawa, Mana; Usami, Sayaka; Takahama, Ryo; Iwamoto, Kazuko; Nabeta, Tomomi; Kawashima, Shin; Kojima, Ryoichi; Ohyama, Junya; Hayakawa, Teruaki; Nabae, Yuta; Moriya, Makoto; Dalton transactions (Cambridge, England : 2003) 53 (2024) 4426–4431; doi:10.1039/d3dt04129h

data_7715057
_publ_section_title
;
 One-pot gram-scale rapid synthesis of MN<sub>4</sub> complexes with
 14-membered ring macrocyclic ligand as a precursor for carbon-based ORR
 and CO<sub>2</sub>RR catalysts.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4426
_journal_page_last               4431
_journal_paper_doi               10.1039/d3dt04129h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C24 H14 Co N6, 2(C F3 O3 S)'
_chemical_formula_sum            'C26 H14 Co F6 N6 O6 S2'
_chemical_formula_weight         743.48
_chemical_name_systematic        '[Co(H2HAM)(OTf)2]'
_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             2023-10-06
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-10-12 deposited with the CCDC.	2024-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.596(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5555(3)
_cell_length_b                   18.4245(6)
_cell_length_c                   8.8580(3)
_cell_measurement_reflns_used    9804
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.0500
_cell_measurement_theta_min      3.1220
_cell_volume                     1338.13(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.897
_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     27.00  94.00   0.50    7.91    --    5.00  45.00 120.00  134
  2  \w    -75.00 -44.00   0.50    7.91    --    5.00  45.00 120.00   62
  3  \w     -1.00  25.00   0.50    7.91    --    5.00  45.00 120.00   52
  4  \w    -28.00  70.00   0.50    7.91    --   -6.90  45.00  90.00  196
  5  \w    -96.00 -50.00   0.50    7.91    --   -6.90  45.00 150.00   92
  6  \w    -95.00 -49.00   0.50    7.91    --   -6.90  45.00   0.00   92
  7  \w     15.00  59.00   0.50    7.91    --   -6.90  45.00   0.00   88
  8  \w    -43.00 -13.00   0.50    7.91    --   -6.90  45.00   0.00   60
  9  \w    -95.00 -45.00   0.50    7.91    --   -6.90  45.00  90.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0407955000
_diffrn_orient_matrix_UB_12      0.0267299000
_diffrn_orient_matrix_UB_13      -0.0322750000
_diffrn_orient_matrix_UB_21      0.0543801000
_diffrn_orient_matrix_UB_22      -0.0268244000
_diffrn_orient_matrix_UB_23      -0.0126301000
_diffrn_orient_matrix_UB_31      -0.0534843000
_diffrn_orient_matrix_UB_32      -0.0068751000
_diffrn_orient_matrix_UB_33      -0.0760573000
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            18782
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.085
_diffrn_reflns_theta_min         3.122
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent intense orange'
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_description       block
_exptl_crystal_F_000             746
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethylene glycol'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0477P)^2^+2.4855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1269
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3131
_reflns_number_total             3534
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04129h2.cif
_cod_data_source_block           220208-nbt-15-asahiligand-co(otf)2-eg
_cod_depositor_comments
'Adding full bibliography for 7715057--7715059.cif.'
_cod_database_code               7715057
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C40N10H20CoO6S4F6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N)
;
_shelx_res_checksum              19936
_shelx_hkl_checksum              62622
_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 1.198
_oxdiff_exptl_absorpt_empirical_full_min 0.843