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_4117822
_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            'C51 H62 B Fe N7 O'
_chemical_formula_weight         855.73
_chemical_name_systematic
;
 (Phenyltris(3-mesitylimidazol-2-ylidine)borato)
(2,2',6,6'-tetramethylpipyridylnitroxido)iron(II)
;
_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                88.234(2)
_cell_angle_beta                 73.097(2)
_cell_angle_gamma                86.124(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7577(4)
_cell_length_b                   14.9817(5)
_cell_length_c                   16.9882(5)
_cell_measurement_reflns_used    7891
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.0
_cell_measurement_theta_min      2.2
_cell_volume                     2856.45(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  diffractometer
_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  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0138
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48283
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.995
_exptl_crystal_description       prism
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.32
_platon_squeeze_details
;
;
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.0035(7)
_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   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         7940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0813P)^2^+1.1583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1283
_reflns_number_gt                7178
_reflns_number_total             7940
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja211882e_si_001_1.cif
_cod_data_source_block           js092
_cod_database_code               4117822