A Structurally Characterized Nonheme Cobalt-Hydroperoxo Complex Derived from Its Superoxo Intermediate via Hydrogen Atom Abstraction.
Wang, Chun-Chieh; Chang, Hao-Ching; Lai, Yei-Chen; Fang, Huayi; Li, Chieh-Chin; Hsu, Hung-Kai; Li, Zong-Yan; Lin, Tien-Sung; Kuo, Ting-Shen; Neese, Frank; Ye, Shengfa; Chiang, Yun-Wei; Tsai, Ming-Li; Liaw, Wen-Feng; Lee, Way-Zen; Journal of the American Chemical Society 138 (2016) 14186–14189; doi:10.1021/jacs.6b08642

data_4131004
_publ_section_title
;
 A Structurally Characterized Nonheme Cobalt-Hydroperoxo Complex Derived
 from Its Superoxo Intermediate via Hydrogen Atom Abstraction.
;
_journal_issue                   43
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14186
_journal_page_last               14189
_journal_paper_doi               10.1021/jacs.6b08642
_journal_volume                  138
_journal_year                    2016
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C45 H51 B Co F4 N3 O4'
_chemical_formula_sum            'C45 H51 B Co F4 N3 O4'
_chemical_formula_weight         843.63
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6583(12)
_cell_length_b                   13.9494(13)
_cell_length_c                   20.9920(16)
_cell_measurement_reflns_used    6416
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.82
_cell_measurement_theta_min      2.30
_cell_volume                     3999.5(6)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX2'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_sigmaI/netI    0.0593
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26645
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  0.8614
_exptl_absorpt_correction_T_min  0.6982
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.226
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.218
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         7109
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1230P)^2^+0.1568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1855
_reflns_number_gt                6003
_reflns_number_total             7109
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b08642_si_002.cif
_cod_data_source_block           ch15147
_cod_database_code               4131004