#------------------------------------------------------------------------------
#$Date: 2016-03-22 10:27:54 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178871 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/00/4110051.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_4110051
loop_
_publ_author_name
'Chih-Chin Tsou'
'Tsai-Te Lu'
'Wen-Feng Liaw'
_publ_section_title
;
 EPR, UV-Vis, IR, and X-ray Demonstration of the Anionic Dimeric
 Dinitrosyl Iron Complex [(NO)2Fe(μ-StBu)2Fe(NO)2]-: Relevance to the
 Products of Nitrosylation of Cytosolic and Mitochondrial Aconitases, and
 High-Potential Iron Proteins
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12626
_journal_page_last               12627
_journal_paper_doi               10.1021/ja0751375
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C28 H58 Fe2 K N4 O12 S2'
_chemical_formula_sum            'C28 H58 Fe2 K N4 O12 S2'
_chemical_formula_weight         857.70
_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                93.4280(10)
_cell_angle_beta                 97.5560(10)
_cell_angle_gamma                101.8990(10)
_cell_formula_units_Z            1
_cell_length_a                   9.3586(2)
_cell_length_b                   9.8599(2)
_cell_length_c                   11.6271(3)
_cell_measurement_reflns_used    10189
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.037
_cell_volume                     1036.53(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_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_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0740
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15115
_diffrn_reflns_theta_full        25.29
_diffrn_reflns_theta_max         25.29
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.957
_exptl_absorpt_correction_T_max  0.9116
_exptl_absorpt_correction_T_min  0.6435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            'green (dark)'
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       prism
_exptl_crystal_F_000             453
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0414
_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)+(0.0645P)²+0.6184P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1221
_reflns_number_gt                3112
_reflns_number_total             3738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0751375si20070710_103127.cif
_cod_data_source_block           6920
_cod_database_code               4110051
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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 0.7260(3) 0.3156(3) 0.4426(3) 0.0353(7) Uani 1 1 d .
C2 C 0.8400(4) 0.3777(4) 0.3676(3) 0.0481(8) Uani 1 1 d .
H2A H 0.7958 0.4286 0.3102 0.072 Uiso 1 1 calc R
H2B H 0.8746 0.3043 0.3294 0.072 Uiso 1 1 calc R
H2C H 0.9215 0.4393 0.4158 0.072 Uiso 1 1 calc R
C3 C 0.7917(5) 0.2337(4) 0.5350(3) 0.0588(10) Uani 1 1 d .
H3A H 0.8750 0.2936 0.5827 0.088 Uiso 1 1 calc R
H3B H 0.8229 0.1575 0.4979 0.088 Uiso 1 1 calc R
H3C H 0.7185 0.1984 0.5827 0.088 Uiso 1 1 calc R
C4 C 0.5936(4) 0.2217(3) 0.3666(3) 0.0414(7) Uani 1 1 d .
H4A H 0.5524 0.2741 0.3089 0.062 Uiso 1 1 calc R
H4B H 0.5205 0.1860 0.4141 0.062 Uiso 1 1 calc R
H4C H 0.6245 0.1457 0.3287 0.062 Uiso 1 1 calc R
C5 C 0.1190(4) 0.3260(4) -0.1217(3) 0.0523(9) Uani 1 1 d .
H5A H 0.1871 0.4142 -0.1241 0.063 Uiso 1 1 calc R
H5B H 0.0194 0.3420 -0.1312 0.063 Uiso 1 1 calc R
C6 C 0.1476(4) 0.3654(4) 0.0842(3) 0.0575(10) Uani 1 1 d .
H6A H 0.0501 0.3856 0.0811 0.069 Uiso 1 1 calc R
H6B H 0.2182 0.4521 0.0820 0.069 Uiso 1 1 calc R
C7 C 0.1855(4) 0.3008(4) 0.1936(3) 0.0583(10) Uani 1 1 d .
H7A H 0.2787 0.2723 0.1931 0.070 Uiso 1 1 calc R
H7B H 0.1958 0.3678 0.2604 0.070 Uiso 1 1 calc R
C8 C 0.0945(4) 0.1219(4) 0.3086(3) 0.0483(9) Uani 1 1 d .
H8A H 0.0977 0.1893 0.3737 0.058 Uiso 1 1 calc R
H8B H 0.1879 0.0927 0.3160 0.058 Uiso 1 1 calc R
C9 C -0.0277(4) 0.0005(4) 0.3097(3) 0.0483(9) Uani 1 1 d .
H9A H -0.0191 -0.0367 0.3851 0.058 Uiso 1 1 calc R
H9B H -0.1215 0.0285 0.2962 0.058 Uiso 1 1 calc R
C10 C -0.1341(4) -0.2248(4) 0.2171(3) 0.0497(9) Uani 1 1 d .
H10A H -0.2302 -0.2014 0.2032 0.060 Uiso 1 1 calc R
H10B H -0.1252 -0.2654 0.2910 0.060 Uiso 1 1 calc R
C11 C 0.3274(5) -0.0882(7) 0.1435(4) 0.0870(16) Uani 1 1 d .
H11A H 0.2618 -0.1206 0.1988 0.104 Uiso 1 1 calc R
H11B H 0.3715 0.0095 0.1650 0.104 Uiso 1 1 calc R
C12 C 0.4401(6) -0.1671(6) 0.1442(4) 0.0925(12) Uani 1 1 d .
H12A H 0.4208 -0.2430 0.1933 0.111 Uiso 1 1 calc R
H12B H 0.5357 -0.1082 0.1745 0.111 Uiso 1 1 calc R
C13 C 0.4390(6) -0.2219(6) 0.0241(4) 0.0925(12) Uani 1 1 d .
H13A H 0.4393 -0.3204 0.0201 0.111 Uiso 1 1 calc R
H13B H 0.5242 -0.1729 -0.0073 0.111 Uiso 1 1 calc R
C14 C 0.3017(5) -0.1977(6) -0.0397(4) 0.0793(14) Uani 1 1 d .
H14A H 0.3206 -0.1585 -0.1121 0.095 Uiso 1 1 calc R
H14B H 0.2296 -0.2849 -0.0578 0.095 Uiso 1 1 calc R
Fe1 Fe 0.54480(4) 0.58831(4) 0.40692(3) 0.03074(16) Uani 1 1 d .
S1 S 0.67871(8) 0.46534(7) 0.52458(6) 0.03101(19) Uani 1 1 d .
N1 N 0.6239(3) 0.7557(3) 0.4345(2) 0.0368(6) Uani 1 1 d .
N2 N 0.5235(3) 0.5238(3) 0.2686(2) 0.0364(6) Uani 1 1 d .
O1 O 0.6789(3) 0.8759(2) 0.4362(2) 0.0577(7) Uani 1 1 d .
O2 O 0.5257(3) 0.4967(3) 0.1684(2) 0.0564(7) Uani 1 1 d .
O3 O 0.1507(2) 0.2711(2) -0.0126(2) 0.0461(6) Uani 1 1 d .
O4 O 0.0713(2) 0.1830(2) 0.20185(18) 0.0441(5) Uani 1 1 d .
O5 O -0.0218(2) -0.1038(2) 0.22064(18) 0.0421(5) Uani 1 1 d .
O6 O 0.2483(3) -0.1063(4) 0.0298(3) 0.0942(12) Uani 1 1 d .
K1 K 0.0000 0.0000 0.0000 0.0337(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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
K K 0.2009 0.2494 '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 C4 110.0(3) . .
C2 C1 C3 111.2(3) . .
C4 C1 C3 109.9(3) . .
C2 C1 S1 106.6(2) . .
C4 C1 S1 113.5(2) . .
C3 C1 S1 105.6(2) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C1 C3 H3A 109.5 . .
C1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C1 C4 H4A 109.5 . .
C1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
O3 C5 C10 108.9(3) . 2
O3 C5 H5A 109.9 . .
C10 C5 H5A 109.9 2 .
O3 C5 H5B 109.9 . .
C10 C5 H5B 109.9 2 .
H5A C5 H5B 108.3 . .
O3 C6 C7 108.7(3) . .
O3 C6 H6A 109.9 . .
C7 C6 H6A 109.9 . .
O3 C6 H6B 109.9 . .
C7 C6 H6B 109.9 . .
H6A C6 H6B 108.3 . .
O4 C7 C6 109.0(3) . .
O4 C7 H7A 109.9 . .
C6 C7 H7A 109.9 . .
O4 C7 H7B 109.9 . .
C6 C7 H7B 109.9 . .
H7A C7 H7B 108.3 . .
O4 C8 C9 108.8(3) . .
O4 C8 H8A 109.9 . .
C9 C8 H8A 109.9 . .
O4 C8 H8B 109.9 . .
C9 C8 H8B 109.9 . .
H8A C8 H8B 108.3 . .
O5 C9 C8 109.3(3) . .
O5 C9 H9A 109.8 . .
C8 C9 H9A 109.8 . .
O5 C9 H9B 109.8 . .
C8 C9 H9B 109.8 . .
H9A C9 H9B 108.3 . .
O5 C10 C5 108.7(3) . 2
O5 C10 H10A 110.0 . .
C5 C10 H10A 110.0 2 .
O5 C10 H10B 110.0 . .
C5 C10 H10B 110.0 2 .
H10A C10 H10B 108.3 . .
O6 C11 C12 107.6(4) . .
O6 C11 H11A 110.2 . .
C12 C11 H11A 110.2 . .
O6 C11 H11B 110.2 . .
C12 C11 H11B 110.2 . .
H11A C11 H11B 108.5 . .
C11 C12 C13 107.8(4) . .
C11 C12 H12A 110.1 . .
C13 C12 H12A 110.1 . .
C11 C12 H12B 110.1 . .
C13 C12 H12B 110.1 . .
H12A C12 H12B 108.5 . .
C12 C13 C14 104.4(4) . .
C12 C13 H13A 110.9 . .
C14 C13 H13A 110.9 . .
C12 C13 H13B 110.9 . .
C14 C13 H13B 110.9 . .
H13A C13 H13B 108.9 . .
O6 C14 C13 108.3(3) . .
O6 C14 H14A 110.0 . .
C13 C14 H14A 110.0 . .
O6 C14 H14B 110.0 . .
C13 C14 H14B 110.0 . .
H14A C14 H14B 108.4 . .
N1 Fe1 N2 116.08(12) . .
N1 Fe1 S1 107.95(9) . .
N2 Fe1 S1 110.29(9) . .
N1 Fe1 S1 111.98(9) . 2_666
N2 Fe1 S1 109.24(9) . 2_666
S1 Fe1 S1 100.11(3) . 2_666
N1 Fe1 Fe1 122.11(9) . 2_666
N2 Fe1 Fe1 121.78(9) . 2_666
S1 Fe1 Fe1 50.17(2) . 2_666
S1 Fe1 Fe1 49.94(2) 2_666 2_666
C1 S1 Fe1 112.75(9) . .
C1 S1 Fe1 114.09(10) . 2_666
Fe1 S1 Fe1 79.89(3) . 2_666
O1 N1 Fe1 169.9(2) . .
O2 N2 Fe1 169.1(2) . .
C6 O3 C5 112.6(3) . .
C6 O3 K1 114.6(2) . .
C5 O3 K1 114.74(18) . .
C8 O4 C7 112.2(2) . .
C8 O4 K1 116.11(18) . .
C7 O4 K1 112.99(19) . .
C10 O5 C9 112.8(2) . .
C10 O5 K1 113.42(18) . .
C9 O5 K1 113.24(18) . .
C14 O6 C11 110.0(3) . .
C14 O6 K1 132.6(2) . .
C11 O6 K1 116.4(2) . .
O6 K1 O6 180.00(13) 2 .
O6 K1 O3 85.20(10) 2 .
O6 K1 O3 94.80(10) . .
O6 K1 O3 94.80(10) 2 2
O6 K1 O3 85.20(10) . 2
O3 K1 O3 180.00(10) . 2
O6 K1 O4 83.34(8) 2 .
O6 K1 O4 96.66(8) . .
O3 K1 O4 61.09(7) . .
O3 K1 O4 118.91(7) 2 .
O6 K1 O4 96.66(8) 2 2
O6 K1 O4 83.34(8) . 2
O3 K1 O4 118.91(7) . 2
O3 K1 O4 61.09(7) 2 2
O4 K1 O4 180.00(5) . 2
O6 K1 O5 99.99(8) 2 .
O6 K1 O5 80.01(8) . .
O3 K1 O5 119.63(6) . .
O3 K1 O5 60.37(6) 2 .
O4 K1 O5 59.99(7) . .
O4 K1 O5 120.01(7) 2 .
O6 K1 O5 80.01(8) 2 2
O6 K1 O5 99.99(8) . 2
O3 K1 O5 60.37(6) . 2
O3 K1 O5 119.63(6) 2 2
O4 K1 O5 120.01(7) . 2
O4 K1 O5 59.99(7) 2 2
O5 K1 O5 180.00(13) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.521(5) .
C1 C4 1.521(4) .
C1 C3 1.523(5) .
C1 S1 1.870(3) .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C5 O3 1.428(4) .
C5 C10 1.487(5) 2
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 O3 1.424(4) .
C6 C7 1.491(6) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 O4 1.424(4) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 O4 1.423(4) .
C8 C9 1.477(5) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 O5 1.430(4) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 O5 1.413(4) .
C10 C5 1.487(5) 2
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 O6 1.409(5) .
C11 C12 1.433(6) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 C13 1.464(6) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 C14 1.468(6) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C14 O6 1.386(5) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
Fe1 N1 1.657(2) .
Fe1 N2 1.666(2) .
Fe1 S1 2.2991(8) .
Fe1 S1 2.3070(8) 2_666
Fe1 Fe1 2.9575(8) 2_666
S1 Fe1 2.3070(8) 2_666
N1 O1 1.189(3) .
N2 O2 1.183(3) .
O3 K1 2.775(2) .
O4 K1 2.792(2) .
O5 K1 2.835(2) .
O6 K1 2.730(3) .
K1 O6 2.730(3) 2
K1 O3 2.775(2) 2
K1 O4 2.792(2) 2
K1 O5 2.835(2) 2
