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_7131282
_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         'C32 H37 Co N2 O3.187'
_chemical_formula_sum            'C32 H37 Co N2 O3.187'
_chemical_formula_weight         560.619
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-14
_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                79.770(2)
_cell_angle_beta                 73.532(2)
_cell_angle_gamma                71.813(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8330(2)
_cell_length_b                   12.9871(4)
_cell_length_c                   13.3740(4)
_cell_measurement_reflns_used    6930
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.7330
_cell_measurement_theta_min      5.6660
_cell_volume                     1391.06(7)
_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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.9813
_diffrn_measured_fraction_theta_max 0.9362
_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    -47.00 -20.00   0.50    1.00    --    0.00 -70.00  23.00   54
  2  \w    -13.00  27.00   0.50    1.00    --    0.00  70.00 155.00   80
  3  \w     51.00 127.00   0.50    2.50    --  101.30 -70.00  23.00  152
  4  \w     78.00 180.00   0.50    2.50    --  101.30  70.00 155.00  204
  5  \w    -35.00  38.00   0.50    1.00    --    0.00  82.00-150.00  146
  6  \w    -15.00  30.00   0.50    1.00    --    0.00 -70.00  23.00   90
  7  \w    -24.00  83.00   0.50    1.00    --    0.00  38.00  30.00  214
  8  \w     75.00 127.00   0.50    2.50    --  101.30 -38.00-180.00  104
  9  \w     48.00 137.00   0.50    2.50    --  101.30 -82.00 -60.00  178
 10  \w     13.00  87.00   0.50    2.50    --  101.30 -19.00 -60.00  148
 11  \w     15.00  42.00   0.50    2.50    --  101.30 -82.00 -60.00   54
 12  \w     66.00 190.00   0.50    2.50    --  101.30  19.00 -60.00  248
 13  \w     17.00 137.00   0.50    2.50    --  101.30 -82.00  60.00  240
 14  \w    113.00 138.00   0.50    2.50    --  101.30 -19.00 -60.00   50
 15  \w     18.00 129.00   0.50    2.50    --  101.30 -82.00-150.00  222
 16  \w     14.00  71.00   0.50    2.50    --  101.30 -38.00-180.00  114
;
_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      -0.1034066000
_diffrn_orient_matrix_UB_12      0.1199515000
_diffrn_orient_matrix_UB_13      0.0007485000
_diffrn_orient_matrix_UB_21      0.0572306000
_diffrn_orient_matrix_UB_22      0.0108214000
_diffrn_orient_matrix_UB_23      0.0953077000
_diffrn_orient_matrix_UB_31      0.1478699000
_diffrn_orient_matrix_UB_32      0.0351453000
_diffrn_orient_matrix_UB_33      -0.0740516000
_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  0.0329
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.9813
_diffrn_reflns_Laue_measured_fraction_max 0.9362
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11798
_diffrn_reflns_point_group_measured_fraction_full 0.9813
_diffrn_reflns_point_group_measured_fraction_max 0.9362
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         75.72
_diffrn_reflns_theta_min         4.75
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    5.117
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58684
_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            organge
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       block
_exptl_crystal_F_000             589.298
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.4823
_refine_diff_density_min         -0.3851
_refine_diff_density_rms         0.0609
_refine_ls_d_res_high            0.7955
_refine_ls_d_res_low             9.3161
_refine_ls_goodness_of_fit_ref   1.0375
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    62
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0375
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1255
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -10
_reflns_limit_k_max              16
_reflns_limit_k_min              -15
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                5152
_reflns_number_total             5419
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cc00146f3.cif
_cod_data_source_block           exp_2129
_cod_depositor_comments
'Adding full bibliography for 7131278--7131282.cif.'
_cod_database_code               7131282
_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. Others
 Sof(H00c)=Sof(H00d)=1-FVAR(1)
 Sof(O004)=Sof(H01a)=Sof(H01b)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C00L(H00a,H00b), C00M(H00c,H00d), C010(H01a,H01b)
3.b Aromatic/amide H refined with riding coordinates:
 C009(H009), C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H), C00I(H00I),
 C00J(H00J), C00N(H00N), C00O(H00O), C00R(H00R), C00T(H00T), C00V(H00V)
3.c Idealised Me refined as rotating group:
 C00S(H00k,H00l,H00m), C00U(H00p,H00q,H00s), C00W(H00u,H00w,H00x), C00X(H00y,H,
 Ha), C00Z(H00z,Hb,Hc), C011(H01c,H01d,H01e), C012(H01f,H01g,H01h)
;
_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 1.596
_oxdiff_exptl_absorpt_empirical_full_min 0.682