#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:08:22 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178770 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/24/4102424.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_4102424
loop_
_publ_author_name
'Zachary J. Tonzetich'
'Hongxin Wang'
'Devrani Mitra'
'Christine E. Tinberg'
'Loi H. Do'
'Francis E. Jenney'
'Michael W. W. Adams'
'Stephen P. Cramer'
'Stephen J. Lippard'
_publ_section_title
;
 Identification of Protein-Bound Dinitrosyl Iron Complexes by Nuclear
 Resonance Vibrational Spectroscopy
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6914
_journal_page_last               6916
_journal_paper_doi               10.1021/ja101002f
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C20 H30 Fe2 N5 O4 S2'
_chemical_formula_weight         580.31
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 94.989(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1729(13)
_cell_length_b                   10.0823(17)
_cell_length_c                   15.840(3)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.17
_cell_measurement_theta_min      2.40
_cell_volume                     1300.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27404
_diffrn_reflns_theta_full        30.20
_diffrn_reflns_theta_max         30.20
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    1.311
_exptl_absorpt_correction_T_max  0.8177
_exptl_absorpt_correction_T_min  0.5779
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             602
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3857
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0343
_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/[σ²(Fo²)+(0.0270P)²+0.7913P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                3188
_reflns_number_total             3857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja101002f_si_002_2.cif
_cod_data_source_block           rRRE-Ph
_cod_database_code               4102424
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe -0.55491(3) -0.08441(3) 0.431313(16) 0.02356(8) Uani 1 1 d . . .
S1 S -0.29404(6) -0.00057(5) 0.46456(3) 0.02275(10) Uani 1 1 d . . .
C1 C -0.2620(2) 0.11864(18) 0.38483(11) 0.0217(4) Uani 1 1 d . . .
O1 O -0.5242(2) -0.36441(16) 0.42096(11) 0.0478(5) Uani 1 1 d . . .
C2 C -0.3719(2) 0.22070(19) 0.36212(12) 0.0257(4) Uani 1 1 d . . .
H2 H -0.4696 0.2292 0.3901 0.031 Uiso 1 1 calc R . .
O2 O -0.6891(2) 0.0222(2) 0.27371(10) 0.0549(5) Uani 1 1 d . . .
N2 N -0.6350(2) -0.01462(19) 0.34156(11) 0.0330(4) Uani 1 1 d . . .
C6 C -0.1197(3) 0.1064(2) 0.34294(13) 0.0321(5) Uani 1 1 d . . .
H6 H -0.0434 0.0376 0.3582 0.039 Uiso 1 1 calc R . .
N1 N -0.5334(2) -0.24910(17) 0.43357(11) 0.0316(4) Uani 1 1 d . . .
C3 C -0.3399(3) 0.3098(2) 0.29911(14) 0.0352(5) Uani 1 1 d . . .
H3 H -0.4145 0.3801 0.2847 0.042 Uiso 1 1 calc R . .
C5 C -0.0895(3) 0.1949(3) 0.27887(17) 0.0509(7) Uani 1 1 d . . .
H5 H 0.0069 0.1856 0.2499 0.061 Uiso 1 1 calc R . .
C4 C -0.1988(3) 0.2967(3) 0.25695(17) 0.0504(7) Uani 1 1 d . . .
H4 H -0.1774 0.3572 0.2133 0.060 Uiso 1 1 calc R . .
N3 N -1.0000 0.5000 0.5000 0.0262(5) Uani 1 2 d SD . .
C14 C -0.8130(4) 0.4809(4) 0.5066(2) 0.0247(8) Uani 0.50 1 d PD A -1
H14A H -0.7585 0.5681 0.5028 0.030 Uiso 0.50 1 calc PR A -1
H14B H -0.7762 0.4412 0.5622 0.030 Uiso 0.50 1 calc PR A -1
C10 C -1.0184(4) 0.5905(4) 0.5802(2) 0.0247(7) Uani 0.50 1 d PD A -1
H10A H -0.9841 0.5384 0.6317 0.030 Uiso 0.50 1 calc PR A -1
H10B H -0.9419 0.6663 0.5783 0.030 Uiso 0.50 1 calc PR A -1
C12 C -1.0927(5) 0.3759(3) 0.5081(3) 0.0263(8) Uani 0.50 1 d PD A -1
H12A H -1.2092 0.3993 0.5126 0.032 Uiso 0.50 1 calc PR A -1
H12B H -1.0875 0.3246 0.4551 0.032 Uiso 0.50 1 calc PR A -1
C8 C -1.0588(5) 0.5803(4) 0.4232(2) 0.0273(8) Uani 0.50 1 d PD A -1
H8A H -1.0517 0.5230 0.3729 0.033 Uiso 0.50 1 calc PR A -1
H8B H -1.1766 0.5998 0.4272 0.033 Uiso 0.50 1 calc PR A -1
C7 C -0.976(2) 0.7085(19) 0.4060(13) 0.036(3) Uani 0.50 1 d P A -1
H7A H -1.0275 0.7478 0.3538 0.054 Uiso 0.50 1 calc PR A -1
H7B H -0.8592 0.6922 0.3997 0.054 Uiso 0.50 1 calc PR A -1
H7C H -0.9861 0.7696 0.4534 0.054 Uiso 0.50 1 calc PR A -1
C9 C -1.1919(6) 0.6450(5) 0.5885(4) 0.0295(11) Uani 0.50 1 d P A -1
H9A H -1.1914 0.6990 0.6400 0.044 Uiso 0.50 1 calc PR A -1
H9B H -1.2688 0.5710 0.5919 0.044 Uiso 0.50 1 calc PR A -1
H9C H -1.2260 0.6998 0.5390 0.044 Uiso 0.50 1 calc PR A -1
C13 C -0.7634(6) 0.3908(5) 0.4357(3) 0.0280(10) Uani 0.50 1 d P A -1
H13A H -0.6438 0.3799 0.4408 0.042 Uiso 0.50 1 calc PR A -1
H13B H -0.7986 0.4308 0.3807 0.042 Uiso 0.50 1 calc PR A -1
H13C H -0.8159 0.3040 0.4401 0.042 Uiso 0.50 1 calc PR A -1
C11 C -1.040(2) 0.288(2) 0.5798(12) 0.031(3) Uani 0.50 1 d P A -1
H11A H -1.1104 0.2094 0.5782 0.046 Uiso 0.50 1 calc PR A -1
H11B H -1.0479 0.3356 0.6332 0.046 Uiso 0.50 1 calc PR A -1
H11C H -0.9256 0.2608 0.5755 0.046 Uiso 0.50 1 calc PR A -1
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'
S S 0.1246 0.1234 '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
N2 Fe1 N1 118.06(9) . .
N2 Fe1 S1 104.93(6) . 3_456
N1 Fe1 S1 114.55(6) . 3_456
N2 Fe1 S1 109.02(6) . .
N1 Fe1 S1 105.39(7) . .
S1 Fe1 S1 103.970(19) 3_456 .
N2 Fe1 Fe1 118.28(7) . 3_456
N1 Fe1 Fe1 123.56(7) . 3_456
S1 Fe1 Fe1 52.016(16) 3_456 3_456
S1 Fe1 Fe1 51.954(14) . 3_456
C1 S1 Fe1 112.16(6) . 3_456
C1 S1 Fe1 105.98(6) . .
Fe1 S1 Fe1 76.030(19) 3_456 .
C2 C1 C6 119.27(17) . .
C2 C1 S1 123.43(13) . .
C6 C1 S1 117.29(15) . .
C3 C2 C1 120.49(18) . .
O2 N2 Fe1 172.88(19) . .
C5 C6 C1 120.0(2) . .
O1 N1 Fe1 169.01(17) . .
C2 C3 C4 120.1(2) . .
C4 C5 C6 120.5(2) . .
C5 C4 C3 119.7(2) . .
C12 N3 C12 180.000(1) 3_366 .
C12 N3 C8 66.6(2) 3_366 .
C12 N3 C8 113.4(2) . .
C12 N3 C8 113.4(2) 3_366 3_366
C12 N3 C8 66.6(2) . 3_366
C8 N3 C8 180.00(16) . 3_366
C12 N3 C14 66.2(2) 3_366 .
C12 N3 C14 113.8(2) . .
C8 N3 C14 111.6(2) . .
C8 N3 C14 68.4(2) 3_366 .
C12 N3 C14 113.8(2) 3_366 3_366
C12 N3 C14 66.2(2) . 3_366
C8 N3 C14 68.4(2) . 3_366
C8 N3 C14 111.6(2) 3_366 3_366
C14 N3 C14 180.000(1) . 3_366
C12 N3 C10 109.5(2) 3_366 3_366
C12 N3 C10 70.5(2) . 3_366
C8 N3 C10 73.0(2) . 3_366
C8 N3 C10 107.0(2) 3_366 3_366
C14 N3 C10 79.53(19) . 3_366
C14 N3 C10 100.47(19) 3_366 3_366
C12 N3 C10 70.5(2) 3_366 .
C12 N3 C10 109.5(2) . .
C8 N3 C10 107.0(2) . .
C8 N3 C10 73.0(2) 3_366 .
C14 N3 C10 100.47(19) . .
C14 N3 C10 79.53(19) 3_366 .
C10 N3 C10 180.00(15) 3_366 .
C13 C14 N3 110.6(3) . .
C9 C10 N3 115.3(3) . .
C11 C12 N3 117.3(8) . .
C7 C8 N3 119.6(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N2 1.6684(19) .
Fe1 N1 1.6698(18) .
Fe1 S1 2.3093(6) 3_456
Fe1 S1 2.3113(6) .
Fe1 Fe1 2.8457(6) 3_456
S1 C1 1.7793(18) .
S1 Fe1 2.3093(6) 3_456
C1 C2 1.393(3) .
C1 C6 1.394(2) .
O1 N1 1.183(2) .
C2 C3 1.385(3) .
O2 N2 1.185(2) .
C6 C5 1.390(3) .
C3 C4 1.388(3) .
C5 C4 1.385(4) .
N3 C12 1.474(3) 3_366
N3 C12 1.474(3) .
N3 C8 1.505(3) .
N3 C8 1.505(3) 3_366
N3 C14 1.535(3) .
N3 C14 1.535(3) 3_366
N3 C10 1.582(3) 3_366
N3 C10 1.582(3) .
C14 C13 1.525(6) .
C10 C9 1.537(6) .
C12 C11 1.47(2) .
C8 C7 1.50(2) .
