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#$Date: 2025-08-21 00:40:30 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301839 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/37/4333764.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4333764
loop_
_publ_author_name
'Chih-Chin Tsou'
'Fu-Te Tsai'
'Huang-Yeh Chen'
'I-Jui Hsu'
'Wen-Feng Liaw'
_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         'C24 H40 Fe N4 O2 Si2'
_chemical_formula_sum            'C24 H40 Fe N4 O2 Si2'
_chemical_formula_weight         528.63
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n 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            4
_cell_length_a                   13.1256(10)
_cell_length_b                   11.3614(9)
_cell_length_c                   19.5259(14)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2911.8(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14571
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6829
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue(dark)
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0586P)²+4.0190P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                2017
_reflns_number_total             2570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302537d_si_001_4.cif
_cod_data_source_block           a12109
_cod_database_code               4333764
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.5225(2) 0.2305(2) 0.11415(15) 0.0312(7) Uani 1 1 d .
C2 C 0.4472(2) 0.2367(3) 0.06310(16) 0.0360(7) Uani 1 1 d .
C3 C 0.3448(3) 0.1787(3) 0.07156(17) 0.0461(9) Uani 1 1 d .
H3A H 0.3417 0.1396 0.1162 0.069 Uiso 1 1 calc R
H3B H 0.3350 0.1204 0.0352 0.069 Uiso 1 1 calc R
H3C H 0.2911 0.2384 0.0688 0.069 Uiso 1 1 calc R
C4 C 0.4688(3) 0.2975(3) 0.00290(17) 0.0463(9) Uani 1 1 d .
H4 H 0.4172 0.3029 -0.0311 0.056 Uiso 1 1 calc R
C5 C 0.5620(3) 0.3504(3) -0.00953(18) 0.0492(9) Uani 1 1 d .
C6 C 0.5830(4) 0.4128(4) -0.0762(2) 0.0731(13) Uani 1 1 d .
H6A H 0.5226 0.4083 -0.1056 0.110 Uiso 1 1 calc R
H6B H 0.6408 0.3752 -0.0993 0.110 Uiso 1 1 calc R
H6C H 0.5993 0.4955 -0.0671 0.110 Uiso 1 1 calc R
C7 C 0.6342(3) 0.3442(3) 0.04137(19) 0.0491(9) Uani 1 1 d .
H7 H 0.6982 0.3812 0.0341 0.059 Uiso 1 1 calc R
C8 C 0.6176(2) 0.2861(3) 0.10308(17) 0.0394(8) Uani 1 1 d .
C9 C 0.7009(3) 0.2785(4) 0.15562(19) 0.0533(10) Uani 1 1 d .
H9A H 0.6764 0.2343 0.1955 0.080 Uiso 1 1 calc R
H9B H 0.7206 0.3580 0.1699 0.080 Uiso 1 1 calc R
H9C H 0.7600 0.2382 0.1358 0.080 Uiso 1 1 calc R
C10 C 0.5907(3) -0.0272(3) 0.0982(2) 0.0632(11) Uani 1 1 d .
H10A H 0.6553 0.0160 0.0971 0.095 Uiso 1 1 calc R
H10B H 0.5504 -0.0072 0.0576 0.095 Uiso 1 1 calc R
H10C H 0.6045 -0.1120 0.0985 0.095 Uiso 1 1 calc R
C11 C 0.5905(3) -0.0338(3) 0.25346(19) 0.0586(10) Uani 1 1 d .
H11A H 0.5526 -0.0113 0.2947 0.088 Uiso 1 1 calc R
H11B H 0.6574 0.0044 0.2539 0.088 Uiso 1 1 calc R
H11C H 0.5993 -0.1194 0.2526 0.088 Uiso 1 1 calc R
C12 C 0.3960(3) -0.0693(3) 0.1780(2) 0.0669(12) Uani 1 1 d .
H12A H 0.3574 -0.0477 0.2190 0.100 Uiso 1 1 calc R
H12B H 0.4100 -0.1540 0.1786 0.100 Uiso 1 1 calc R
H12C H 0.3561 -0.0497 0.1371 0.100 Uiso 1 1 calc R
N1 N 0.37445(19) 0.1509(2) 0.29073(13) 0.0346(6) Uani 1 1 d .
N2 N 0.50736(17) 0.1678(2) 0.17675(12) 0.0290(6) Uani 1 1 d .
O1 O 0.3051(2) 0.1029(2) 0.31510(13) 0.0611(8) Uani 1 1 d .
Si1 Si 0.51879(7) 0.01353(8) 0.17640(5) 0.0363(3) Uani 1 1 d .
Fe1 Fe 0.44519(4) 0.2500 0.2500 0.0247(2) Uani 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C2 C1 C8 119.3(3) . .
C2 C1 N2 122.3(3) . .
C8 C1 N2 118.4(3) . .
C4 C2 C1 118.8(3) . .
C4 C2 C3 119.4(3) . .
C1 C2 C3 121.8(3) . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C5 C4 C2 122.9(3) . .
C5 C4 H4 118.6 . .
C2 C4 H4 118.6 . .
C7 C5 C4 117.4(3) . .
C7 C5 C6 121.5(4) . .
C4 C5 C6 121.1(4) . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C5 C7 C8 122.9(3) . .
C5 C7 H7 118.6 . .
C8 C7 H7 118.6 . .
C7 C8 C1 118.8(3) . .
C7 C8 C9 120.4(3) . .
C1 C8 C9 120.8(3) . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
Si1 C10 H10A 109.5 . .
Si1 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
Si1 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
Si1 C11 H11A 109.5 . .
Si1 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
Si1 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
Si1 C12 H12A 109.5 . .
Si1 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
Si1 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
O1 N1 Fe1 161.9(3) . .
C1 N2 Si1 118.78(18) . .
C1 N2 Fe1 117.43(18) . .
Si1 N2 Fe1 122.08(14) . .
N2 Si1 C11 109.20(15) . .
N2 Si1 C10 107.18(16) . .
C11 Si1 C10 109.73(19) . .
N2 Si1 C12 115.38(15) . .
C11 Si1 C12 106.2(2) . .
C10 Si1 C12 109.1(2) . .
N1 Fe1 N1 112.07(18) . 4
N1 Fe1 N2 102.32(11) . 4
N1 Fe1 N2 105.56(11) 4 4
N1 Fe1 N2 105.56(11) . .
N1 Fe1 N2 102.32(11) 4 .
N2 Fe1 N2 128.93(14) 4 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.405(4) .
C1 C8 1.415(4) .
C1 N2 1.429(4) .
C2 C4 1.392(5) .
C2 C3 1.506(4) .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 C5 1.385(5) .
C4 H4 0.9500 .
C5 C7 1.375(5) .
C5 C6 1.508(5) .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 C8 1.391(5) .
C7 H7 0.9500 .
C8 C9 1.501(5) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 Si1 1.855(4) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 Si1 1.854(4) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 Si1 1.867(4) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
N1 O1 1.163(3) .
N1 Fe1 1.662(3) .
N2 Si1 1.759(3) .
N2 Fe1 1.893(2) .
Fe1 N1 1.662(3) 4
Fe1 N2 1.893(2) 4
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139139069
