Oxygen-Oxygen Bond Cleavage and Formation in Co(II)-Mediated Stoichiometric O<sub>2</sub> Reduction via the Potential Intermediacy of a Co(IV) Oxyl Radical.
Nurdin, Lucie; Spasyuk, Denis M.; Fairburn, Laura; Piers, Warren E.; Maron, Laurent; Journal of the American Chemical Society 140 (2018) 16094–16105; doi:10.1021/jacs.8b07726

data_4132984
_publ_section_title
;
 Oxygen-Oxygen Bond Cleavage and Formation in Co(II)-Mediated
 Stoichiometric O<sub>2</sub> Reduction via the Potential Intermediacy of
 a Co(IV) Oxyl Radical.
;
_journal_issue                   47
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16094
_journal_page_last               16105
_journal_paper_doi               10.1021/jacs.8b07726
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C31 H29 B2 Br Co N9 '
_chemical_formula_sum            'C31 H29 B2 Br Co N9'
_chemical_formula_weight         688.09
_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   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 98.0107(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.1544(3)
_cell_length_b                   17.4378(3)
_cell_length_c                   8.42250(10)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.15
_cell_measurement_theta_min      2.21
_cell_volume                     2931.19(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'LinXTL v.  5.5.1'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            22075
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.497
_diffrn_reflns_theta_min         2.214
_exptl_absorpt_coefficient_mu    6.502
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         5110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.002
_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^+1.4507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4550
_reflns_number_total             5110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07726_si_005.cif
_cod_data_source_block           lf1501
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4132984
_shelxl_version_number           2014/6
_shelx_res_checksum              85231
_shelx_hkl_checksum              45467