Insight into One-Electron Oxidation of the {Fe(NO)2}9 Dinitrosyl Iron Complex (DNIC): Aminyl Radical Stabilized by [Fe(NO)2] Motif
Chih-Chin Tsou; Fu-Te Tsai; Huang-Yeh Chen; I-Jui Hsu; Wen-Feng Liaw; Inorganic Chemistry 52 (2013) 1631–1639; doi:10.1021/ic302537d

data_4333763
_publ_section_title
;
 Insight into One-Electron Oxidation of the {Fe(NO)2}9 Dinitrosyl Iron
 Complex (DNIC): Aminyl Radical Stabilized by [Fe(NO)2] Motif
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1631
_journal_page_last               1639
_journal_paper_doi               10.1021/ic302537d
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C44 H80 Fe K N4 O10 Si2'
_chemical_formula_sum            'C44 H80 Fe K N4 O10 Si2'
_chemical_formula_weight         976.25
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   15.8975(9)
_cell_length_b                   22.4576(12)
_cell_length_c                   30.9214(17)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     11039.5(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0656
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            62208
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.9528
_exptl_absorpt_correction_T_min  0.8972
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown(dark)
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       prism
_exptl_crystal_F_000             4200
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         9717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0584P)^2^+8.5360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1386
_reflns_number_gt                6474
_reflns_number_total             9717
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302537d_si_001_3.cif
_cod_data_source_block           a12838
_cod_database_code               4333763