#------------------------------------------------------------------------------
#$Date: 2017-03-04 06:24:43 +0200 (Sat, 04 Mar 2017) $
#$Revision: 193027 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/56/4125626.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_4125626
loop_
_publ_author_name
'Ke, Chun-Hung'
'Chen, Chien-Hong'
'Tsai, Ming-Li'
'Wang, Hsuan-Chi'
'Tsai, Fu-Te'
'Chiang, Yun-Wei'
'Shih, Wei-Chih'
'Bohle, D. Scott'
'Liaw, Wen-Feng'
_publ_section_title
;
 {Fe(NO)2}(9) Dinitrosyl Iron Complex Acting as a Vehicle for the NO
 Radical.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              67
_journal_page_last               70
_journal_paper_doi               10.1021/jacs.6b11454
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C28 H40 Fe N4 O2'
_chemical_formula_sum            'C28 H40 Fe N4 O2'
_chemical_formula_weight         520.49
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2n'
_symmetry_space_group_name_H-M   'P n a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   12.478(5)
_cell_length_b                   10.528(5)
_cell_length_c                   21.296(5)
_cell_measurement_reflns_used    6847
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.53
_cell_volume                     2797.6(19)
_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    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15995
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  0.8802
_exptl_absorpt_correction_T_min  0.7337
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.462
_refine_diff_density_rms
'0.161 *********************************************************'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2554
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0371
_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)+(0.0625P)²+1.3692P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1189
_reflns_number_gt                2241
_reflns_number_total             2554
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b11454_si_002.cif
_cod_data_source_block           1-Iso
_cod_database_code               4125626
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x-1/2, -y-1/2, z'
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 0.39311(16) 0.0875(2) 0.62442(10) 0.0214(5) Uani 1 1 d .
C2 C 0.42269(17) 0.1807(2) 0.58094(10) 0.0245(5) Uani 1 1 d .
C3 C 0.48137(19) 0.3006(2) 0.60008(11) 0.0296(5) Uani 1 1 d .
H3 H 0.4942 0.2962 0.6464 0.035 Uiso 1 1 calc R
C4 C 0.4138(2) 0.4182(3) 0.58713(14) 0.0486(7) Uani 1 1 d .
H4A H 0.4533 0.4941 0.6003 0.073 Uiso 1 1 calc R
H4B H 0.3465 0.4126 0.6106 0.073 Uiso 1 1 calc R
H4C H 0.3983 0.4235 0.5421 0.073 Uiso 1 1 calc R
C5 C 0.5903(2) 0.3105(3) 0.56777(15) 0.0502(8) Uani 1 1 d .
H5A H 0.6319 0.2334 0.5761 0.075 Uiso 1 1 calc R
H5B H 0.6290 0.3845 0.5841 0.075 Uiso 1 1 calc R
H5C H 0.5799 0.3200 0.5224 0.075 Uiso 1 1 calc R
C6 C 0.39558(19) 0.1599(3) 0.51817(11) 0.0330(6) Uani 1 1 d .
H6 H 0.4145 0.2216 0.4876 0.040 Uiso 1 1 calc R
C7 C 0.3420(2) 0.0517(3) 0.49973(11) 0.0356(6) Uani 1 1 d .
H7 H 0.3241 0.0395 0.4568 0.043 Uiso 1 1 calc R
C8 C 0.31430(19) -0.0388(2) 0.54352(11) 0.0325(6) Uani 1 1 d .
H8 H 0.2779 -0.1133 0.5302 0.039 Uiso 1 1 calc R
C9 C 0.33841(17) -0.0235(2) 0.60680(10) 0.0260(5) Uani 1 1 d .
C10 C 0.3064(2) -0.1243(2) 0.65420(12) 0.0363(6) Uani 1 1 d .
H10 H 0.3272 -0.0929 0.6968 0.044 Uiso 1 1 calc R
C11 C 0.3659(3) -0.2481(4) 0.64255(19) 0.076 Uani 1 1 d .
H11A H 0.3441 -0.3111 0.6740 0.114 Uiso 1 1 calc R
H11B H 0.4432 -0.2333 0.6457 0.114 Uiso 1 1 calc R
H11C H 0.3486 -0.2797 0.6005 0.114 Uiso 1 1 calc R
C12 C 0.1858(2) -0.1478(4) 0.65455(17) 0.0635(10) Uani 1 1 d .
H12A H 0.1686 -0.2133 0.6856 0.095 Uiso 1 1 calc R
H12B H 0.1629 -0.1762 0.6128 0.095 Uiso 1 1 calc R
H12C H 0.1484 -0.0689 0.6654 0.095 Uiso 1 1 calc R
C13 C 0.50412(16) 0.06998(19) 0.71544(9) 0.0201(5) Uani 1 1 d .
C14 C 0.59951(19) 0.0254(3) 0.67929(11) 0.0350(6) Uani 1 1 d .
H14A H 0.5848 0.0320 0.6342 0.053 Uiso 1 1 calc R
H14B H 0.6147 -0.0633 0.6901 0.053 Uiso 1 1 calc R
H14C H 0.6616 0.0782 0.6899 0.053 Uiso 1 1 calc R
N1 N 0.1910(2) 0.1598(3) 0.7500 0.0259(6) Uani 1 2 d S
N2 N 0.3451(2) 0.3529(3) 0.7500 0.0266(6) Uani 1 2 d S
N3 N 0.41396(13) 0.10497(16) 0.69049(8) 0.0188(4) Uani 1 1 d .
O1 O 0.09521(19) 0.1665(3) 0.7500 0.0466(7) Uani 1 2 d S
O2 O 0.3594(2) 0.4647(2) 0.7500 0.0453(7) Uani 1 2 d S
Fe1 Fe 0.31956(3) 0.19880(4) 0.7500 0.01947(17) 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'
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 C9 122.4(2) . .
C2 C1 N3 120.55(19) . .
C9 C1 N3 117.04(19) . .
C6 C2 C1 117.4(2) . .
C6 C2 C3 120.3(2) . .
C1 C2 C3 122.3(2) . .
C2 C3 C4 111.2(2) . .
C2 C3 C5 111.5(2) . .
C4 C3 C5 110.8(2) . .
C2 C3 H3 107.7 . .
C4 C3 H3 107.7 . .
C5 C3 H3 107.7 . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C3 C5 H5A 109.5 . .
C3 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C3 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C7 C6 C2 121.3(2) . .
C7 C6 H6 119.3 . .
C2 C6 H6 119.3 . .
C8 C7 C6 120.0(2) . .
C8 C7 H7 120.0 . .
C6 C7 H7 120.0 . .
C7 C8 C9 121.5(2) . .
C7 C8 H8 119.3 . .
C9 C8 H8 119.3 . .
C8 C9 C1 117.4(2) . .
C8 C9 C10 120.5(2) . .
C1 C9 C10 122.1(2) . .
C9 C10 C11 111.2(2) . .
C9 C10 C12 112.1(2) . .
C11 C10 C12 110.1(3) . .
C9 C10 H10 107.7 . .
C11 C10 H10 107.7 . .
C12 C10 H10 107.7 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N3 C13 C13 114.17(11) . 6_557
N3 C13 C14 124.70(19) . .
C13 C13 C14 121.03(12) 6_557 .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
O1 N1 Fe1 162.3(3) . .
O2 N2 Fe1 177.5(3) . .
C13 N3 C1 121.29(17) . .
C13 N3 Fe1 113.14(13) . .
C1 N3 Fe1 125.25(13) . .
N2 Fe1 N1 115.45(14) . .
N2 Fe1 N3 111.88(9) . .
N1 Fe1 N3 116.74(9) . .
N2 Fe1 N3 111.88(9) . 6_557
N1 Fe1 N3 116.74(9) . 6_557
N3 Fe1 N3 79.00(10) . 6_557
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.399(3) .
C1 C9 1.404(3) .
C1 N3 1.443(3) .
C2 C6 1.396(3) .
C2 C3 1.515(3) .
C3 C4 1.523(3) .
C3 C5 1.527(4) .
C3 H3 1.0000 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 C7 1.378(4) .
C6 H6 0.9500 .
C7 C8 1.377(4) .
C7 H7 0.9500 .
C8 C9 1.390(3) .
C8 H8 0.9500 .
C9 C10 1.518(3) .
C10 C11 1.520(5) .
C10 C12 1.525(4) .
C10 H10 1.0000 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 N3 1.298(3) .
C13 C13 1.472(4) 6_557
C13 C14 1.493(3) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
N1 O1 1.197(3) .
N1 Fe1 1.656(3) .
N2 O2 1.190(4) .
N2 Fe1 1.654(3) .
N3 Fe1 1.9923(17) .
Fe1 N3 1.9923(17) 6_557
