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_4132986
_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 Co N9'
_chemical_formula_sum            'C31 H29 B2 Co N9'
_chemical_formula_weight         608.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1792(11)
_cell_length_b                   19.504(3)
_cell_length_c                   18.065(3)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    174(2)
_cell_measurement_theta_max      72.12
_cell_measurement_theta_min      2.45
_cell_volume                     2881.9(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.  5.3.0'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      174(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0415
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33855
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         67.487
_diffrn_reflns_theta_min         3.335
_exptl_absorpt_coefficient_mu    4.975
_exptl_absorpt_correction_T_max  0.8644
_exptl_absorpt_correction_T_min  0.7487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         2684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0640P)^2^+0.3962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2453
_reflns_number_total             2684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07726_si_003.cif
_cod_data_source_block           ds123
_cod_original_cell_volume        2881.8(7)
_cod_database_code               4132986
_shelxl_version_number           2013-4
_shelx_res_checksum              86534
_shelx_hkl_checksum              4331