N-O Bond Homolysis of an Iron(II) TEMPO Complex Yields an Iron(III) Oxo Intermediate
Jeremy M. Smith; Derick E. Mayberry; Charles G. Margarit; Jörg Sutter; Haobin Wang; Karsten Meyer; Ranko P. Bontchev; Journal of the American Chemical Society 134 (2012) 6516–6519; doi:10.1021/ja211882e

data_4117823
_publ_section_title
;
 N-O Bond Homolysis of an Iron(II) TEMPO Complex Yields an Iron(III) Oxo
 Intermediate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6516
_journal_page_last               6519
_journal_paper_doi               10.1021/ja211882e
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C61 H59 B Fe N6 O'
_chemical_formula_weight         958.80
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.278(2)
_cell_angle_beta                 99.104(2)
_cell_angle_gamma                100.639(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1292(4)
_cell_length_b                   12.2360(4)
_cell_length_c                   17.9044(6)
_cell_measurement_temperature    293(2)
_cell_volume                     2537.27(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            81027
_diffrn_reflns_theta_full        33.72
_diffrn_reflns_theta_max         33.72
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.346
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         19874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.056
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0846P)^2^+0.1805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1576
_reflns_number_gt                13698
_reflns_number_total             19874
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja211882e_si_001_2.cif
_cod_data_source_block           js98_0m
_cod_database_code               4117823