C-H bond activations by the HO˙/(Salophen<sup><i>t</i>-Bu</sup>)Co(II) radical pair generated <i>via</i> homolysis of a terminal Co(III)-OH bond.
Zhang, Jia; Li, Songyi; Fang, Huayi; Chemical communications (Cambridge, England) 59 (2023) 3245–3248; doi:10.1039/d3cc00146f

data_7131281
_publ_section_title
;
 C-H bond activations by the
 HO&#x2d9;/(Salophen<sup><i>t</i>-Bu</sup>)Co(II) radical pair generated
 <i>via</i> homolysis of a terminal Co(III)-OH bond.
;
_journal_issue                   22
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3245
_journal_page_last               3248
_journal_paper_doi               10.1039/d3cc00146f
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         '2(C30 H32 Co N3 O2)'
_chemical_formula_sum            'C60 H64 Co2 N6 O4'
_chemical_formula_weight         1051.03
_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             2022-04-22
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-11-20 deposited with the CCDC.	2023-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.2580(10)
_cell_angle_beta                 95.743(2)
_cell_angle_gamma                94.842(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8058(3)
_cell_length_b                   13.8879(2)
_cell_length_c                   14.8417(2)
_cell_measurement_reflns_used    7711
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.4330
_cell_measurement_theta_min      4.1650
_cell_volume                     2821.02(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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    -38.00  36.00   0.50    5.00    --    0.00 -82.00-150.00  148
  2  \w    -58.00  58.00   0.50    5.00    --    0.00   0.00  60.00  232
  3  \w     25.00  80.00   0.50    9.50    --  101.30 -82.00 120.00  110
  4  \w     25.00 126.00   0.50    9.50    --  101.30 -38.00 -90.00  202
  5  \w     65.00 178.00   0.50    9.50    --  101.30  19.00  60.00  226
  6  \w     48.00 101.00   0.50    9.50    --  101.30 -82.00  60.00  106
  7  \w     15.00 109.00   0.50    9.50    --  101.30 -38.00 120.00  188
  8  \w     17.00 123.00   0.50    9.50    --  101.30 -57.00 -90.00  212
  9  \w     15.00 121.00   0.50    9.50    --  101.30 -57.00 120.00  212
 10  \w     76.00 167.00   0.50    9.50    --  101.30  38.00  90.00  182
 11  \w     92.00 130.00   0.50    9.50    --  101.30 -82.00 120.00   76
 12  \w     19.00 128.00   0.50    9.50    --  101.30 -82.00 -90.00  218
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0780970000
_diffrn_orient_matrix_UB_12      0.0731795000
_diffrn_orient_matrix_UB_13      -0.0029000000
_diffrn_orient_matrix_UB_21      -0.0062825000
_diffrn_orient_matrix_UB_22      -0.0004777000
_diffrn_orient_matrix_UB_23      -0.1042248000
_diffrn_orient_matrix_UB_31      -0.0808168000
_diffrn_orient_matrix_UB_32      -0.0839049000
_diffrn_orient_matrix_UB_33      -0.0037436000
_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  0.0358
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22315
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.000
_diffrn_reflns_theta_min         4.177
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    4.997
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         10121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0549P)^2^+0.5109P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8364
_reflns_number_total             10121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00146f3.cif
_cod_data_source_block           exp_2674
_cod_depositor_comments
'Adding full bibliography for 7131278--7131282.cif.'
_cod_database_code               7131281
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00K(H00C,H00D), C00S(H00A,H00B)
2.b Aromatic/amide H refined with riding coordinates:
 C00L(H00L), C00N(H00N), C00Q(H00Q), C00R(H00R), C00Y(H00Y), C010(H010),
 C011(H011), C012(H012), C015(H015), C017(H017), C019(H019), C01A(H01W),
 C01D(H01D), C01E(H01E), C01F(H01), C01I(H01I), C01K(H01K), C01M(H01M),
 C01N(H01N), C01O(H3), C01Q(H4), C01R(H5), C01V(H01V), C01Y(H7)
2.c Idealised Me refined as rotating group:
 C01B(H01X,H01Y,H), C01C(H01Z,HA,HB), C01H(H1,HC,HD), C01J(H2,HE,HF),
 C01P(H01A,H01B,H01C), C01S(H01F,H01G,H01H), C01T(H6,HG,HH), C01U(H01J,H01L,
 H01O), C01W(H01P,H01Q,H01R), C01X(H01S,H01T,H01U), C01Z(H8,HI,HJ), C020(H02A,
 H02B,H02C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              97492
_shelx_hkl_checksum              49198
_shelx_fab_checksum              9438
_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 1.322
_oxdiff_exptl_absorpt_empirical_full_min 0.748