#------------------------------------------------------------------------------
#$Date: 2024-04-05 02:17:35 +0300 (Fri, 05 Apr 2024) $
#$Revision: 290915 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/50/7715057.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7715057
loop_
_publ_author_name
'Ogawa, Mana'
'Usami, Sayaka'
'Takahama, Ryo'
'Iwamoto, Kazuko'
'Nabeta, Tomomi'
'Kawashima, Shin'
'Kojima, Ryoichi'
'Ohyama, Junya'
'Hayakawa, Teruaki'
'Nabae, Yuta'
'Moriya, Makoto'
_publ_section_title
;
 One-pot gram-scale rapid synthesis of MN₄ complexes with
 14-membered ring macrocyclic ligand as a precursor for carbon-based ORR
 and CO₂RR 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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     27.00  94.00   0.50    7.91    --    5.00  45.00 120.00  134
  2  ω    -75.00 -44.00   0.50    7.91    --    5.00  45.00 120.00   62
  3  ω     -1.00  25.00   0.50    7.91    --    5.00  45.00 120.00   52
  4  ω    -28.00  70.00   0.50    7.91    --   -6.90  45.00  90.00  196
  5  ω    -96.00 -50.00   0.50    7.91    --   -6.90  45.00 150.00   92
  6  ω    -95.00 -49.00   0.50    7.91    --   -6.90  45.00   0.00   92
  7  ω     15.00  59.00   0.50    7.91    --   -6.90  45.00   0.00   88
  8  ω    -43.00 -13.00   0.50    7.91    --   -6.90  45.00   0.00   60
  9  ω    -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       'ω 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/[σ²(Fo²)+(0.0477P)²+2.4855P] where P=(Fo²+2Fc²)/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 > 2σ(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
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co01 Co 0.500000 0.500000 0.500000 0.01743(14) Uani 1 2 d S . P . .
S002 S 0.32916(8) 0.36777(4) 0.20718(8) 0.02185(16) Uani 1 1 d . . . . .
O003 O 0.3354(2) 0.40144(12) 0.3564(2) 0.0269(4) Uani 1 1 d . . . . .
F004 F 0.5867(2) 0.29746(11) 0.3724(3) 0.0483(6) Uani 1 1 d . . . . .
F005 F 0.3673(3) 0.23809(12) 0.3310(3) 0.0581(7) Uani 1 1 d . . . . .
O006 O 0.4231(3) 0.40532(13) 0.1195(3) 0.0358(5) Uani 1 1 d . . . . .
N007 N 0.6654(3) 0.48534(12) 0.4032(3) 0.0178(4) Uani 1 1 d . . . . .
N008 N 0.5620(3) 0.56059(13) 0.1838(3) 0.0205(4) Uani 1 1 d . . . . .
O009 O 0.1712(3) 0.34353(16) 0.1162(3) 0.0460(7) Uani 1 1 d . . . . .
N00A N 0.3851(3) 0.56323(12) 0.3427(2) 0.0185(4) Uani 1 1 d . . . . .
F00B F 0.4722(4) 0.25063(15) 0.1453(3) 0.0785(10) Uani 1 1 d . . . . .
C00C C 0.1381(3) 0.63694(15) 0.2754(3) 0.0233(5) Uani 1 1 d . . . . .
C00D C 0.9131(3) 0.41424(15) 0.4379(3) 0.0236(5) Uani 1 1 d . . . . .
C00E C 0.4210(3) 0.58408(14) 0.2138(3) 0.0188(5) Uani 1 1 d . . . . .
C00F C 0.6779(3) 0.51284(14) 0.2690(3) 0.0196(5) Uani 1 1 d . . . . .
C00G C 0.2463(3) 0.58830(14) 0.3721(3) 0.0189(5) Uani 1 1 d . . . . .
C00H C 0.7802(3) 0.43747(14) 0.4865(3) 0.0193(5) Uani 1 1 d . . . . .
C00I C 0.9242(3) 0.44394(17) 0.2931(4) 0.0280(6) Uani 1 1 d . . . . .
H00I H 1.009624 0.430188 0.253815 0.034 Uiso 1 1 calc R U . . .
C00J C 0.0019(4) 0.66104(17) 0.3262(4) 0.0319(7) Uani 1 1 d . . . . .
H00J H -0.071887 0.693681 0.264021 0.038 Uiso 1 1 calc R U . . .
C00K C 0.8111(3) 0.49226(16) 0.2114(3) 0.0247(6) Uani 1 1 d . . . . .
H00K H 0.820708 0.511906 0.117697 0.030 Uiso 1 1 calc R U . . .
C00L C 0.1764(3) 0.65751(16) 0.1360(3) 0.0265(6) Uani 1 1 d . . . . .
H00L H 0.107572 0.688950 0.065245 0.032 Uiso 1 1 calc R U . . .
C00M C -0.0219(4) 0.63700(18) 0.4643(4) 0.0315(7) Uani 1 1 d . . . . .
H00M H -0.110277 0.654288 0.495034 0.038 Uiso 1 1 calc R U . . .
C00N C 0.3136(3) 0.63163(15) 0.1044(3) 0.0244(6) Uani 1 1 d . . . . .
H00N H 0.336922 0.644940 0.011873 0.029 Uiso 1 1 calc R U . . .
C00O C 0.4454(4) 0.28431(17) 0.2663(4) 0.0305(6) Uani 1 1 d . . . . .
H008 H 0.581(4) 0.5727(18) 0.106(4) 0.017(8) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N007 Co01 N007 180.00(6) . 3_666 ?
N00A Co01 N007 93.10(9) . . ?
N00A Co01 N007 93.10(9) 3_666 3_666 ?
N00A Co01 N007 86.90(9) . 3_666 ?
N00A Co01 N007 86.90(9) 3_666 . ?
N00A Co01 N00A 180.0 3_666 . ?
O003 S002 C00O 102.95(13) . . ?
O006 S002 O003 113.89(13) . . ?
O006 S002 C00O 102.53(15) . . ?
O009 S002 O003 115.48(14) . . ?
O009 S002 O006 115.29(16) . . ?
O009 S002 C00O 104.34(16) . . ?
C00F N007 Co01 128.42(18) . . ?
C00F N007 C00H 120.0(2) . . ?
C00H N007 Co01 111.50(17) . . ?
C00E N008 C00F 128.9(2) . . ?
C00E N00A Co01 128.59(18) . . ?
C00E N00A C00G 119.7(2) . . ?
C00G N00A Co01 111.69(17) . . ?
C00G C00C C00J 117.6(3) . . ?
C00G C00C C00L 115.4(2) . . ?
C00L C00C C00J 127.0(3) . . ?
C00H C00D C00I 115.5(3) . . ?
C00H C00D C00M 117.5(3) . 3_666 ?
C00I C00D C00M 126.9(3) . 3_666 ?
N008 C00E C00N 119.4(2) . . ?
N00A C00E N008 120.5(2) . . ?
N00A C00E C00N 120.1(2) . . ?
N007 C00F N008 120.4(2) . . ?
N007 C00F C00K 119.8(2) . . ?
N008 C00F C00K 119.8(2) . . ?
N00A C00G C00C 124.1(2) . . ?
N00A C00G C00H 115.0(2) . 3_666 ?
C00C C00G C00H 120.8(2) . 3_666 ?
N007 C00H C00D 123.7(2) . . ?
N007 C00H C00G 114.9(2) . 3_666 ?
C00D C00H C00G 121.4(2) . 3_666 ?
C00K C00I C00D 120.7(2) . . ?
C00M C00J C00C 121.4(3) . . ?
C00I C00K C00F 120.2(3) . . ?
C00N C00L C00C 120.7(3) . . ?
C00J C00M C00D 121.2(3) . 3_666 ?
C00L C00N C00E 119.9(3) . . ?
F004 C00O S002 111.2(2) . . ?
F005 C00O S002 111.7(2) . . ?
F005 C00O F004 106.5(3) . . ?
F005 C00O F00B 106.2(3) . . ?
F00B C00O S002 111.8(2) . . ?
F00B C00O F004 109.2(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co01 N007 1.871(2) . ?
Co01 N007 1.871(2) 3_666 ?
Co01 N00A 1.866(2) . ?
Co01 N00A 1.866(2) 3_666 ?
S002 O003 1.447(2) . ?
S002 O006 1.444(2) . ?
S002 O009 1.433(2) . ?
S002 C00O 1.825(3) . ?
F004 C00O 1.325(4) . ?
F005 C00O 1.311(4) . ?
N007 C00F 1.324(3) . ?
N007 C00H 1.369(3) . ?
N008 C00E 1.377(3) . ?
N008 C00F 1.378(4) . ?
N00A C00E 1.321(3) . ?
N00A C00G 1.367(3) . ?
F00B C00O 1.315(4) . ?
C00C C00G 1.393(4) . ?
C00C C00J 1.434(4) . ?
C00C C00L 1.417(4) . ?
C00D C00H 1.393(4) . ?
C00D C00I 1.422(4) . ?
C00D C00M 1.431(4) 3_666 ?
C00E C00N 1.429(4) . ?
C00F C00K 1.427(4) . ?
C00G C00H 1.417(4) 3_666 ?
C00I C00K 1.361(4) . ?
C00J C00M 1.370(5) . ?
C00L C00N 1.368(4) . ?
