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_4132988
_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_sum            'C62 H58 B4 Co2 N18 O2'
_chemical_formula_weight         1248.36
_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
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                89.947(4)
_cell_angle_beta                 77.865(3)
_cell_angle_gamma                86.508(3)
_cell_formula_units_Z            2
_cell_length_a                   13.6686(8)
_cell_length_b                   15.0534(8)
_cell_length_c                   18.3053(10)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      72.00
_cell_measurement_theta_min      2.94
_cell_volume                     3675.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.961
_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  0.1000
_diffrn_reflns_av_unetI/netI     0.0853
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            96352
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.494
_diffrn_reflns_theta_min         3.693
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.934
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.00095(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         12744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0608
_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^)+(0.1074P)^2^+0.0492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9859
_reflns_number_total             12744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07726_si_004.cif
_cod_data_source_block           TEST_a
_cod_database_code               4132988
_shelxl_version_number           2014/6
_shelx_res_checksum              90770
_shelx_hkl_checksum              90187
_shelx_fab_checksum              96748