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_4132989
_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
'2(C31 H31 B2 Co N9 O), 2(C2 F6 N O4 S2), 4(C18 H15 O P), C6 H6'
_chemical_formula_sum            'C144 H128 B4 Co2 F12 N20 O14 P4 S4'
_chemical_formula_weight         3003.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/5
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.5774(17)
_cell_length_b                   14.5959(8)
_cell_length_c                   41.157(3)
_cell_measurement_reflns_used    3292
_cell_measurement_temperature    173
_cell_measurement_theta_max      71.35
_cell_measurement_theta_min      12.27
_cell_volume                     14163.5(16)
_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. 5.9.6 (Spasyuk, 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1236
_diffrn_reflns_av_unetI/netI     0.2584
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            69444
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        64.495
_diffrn_reflns_theta_max         64.495
_diffrn_reflns_theta_min         2.147
_exptl_absorpt_coefficient_mu    3.533
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_correction_T_min  0.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6200
_exptl_crystal_size_max          0.391
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.016(9)
_refine_ls_extinction_coef       0.00045(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/5 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1957
_refine_ls_number_reflns         22148
_refine_ls_number_restraints     2405
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_gt           0.0872
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2276
_refine_ls_wR_factor_ref         0.2676
_reflns_Friedel_coverage         0.969
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                14650
_reflns_number_total             22148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07726_si_008.cif
_cod_data_source_block           co1
_cod_database_code               4132989
_shelx_shelxl_version_number     2016/5
_shelx_res_checksum              92329
_shelx_hkl_checksum              55854