#------------------------------------------------------------------------------
#$Date: 2017-09-29 15:18:04 +0300 (Fri, 29 Sep 2017) $
#$Revision: 201508 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/74/1547478.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_1547478
loop_
_publ_author_name
'Hsieh, Chung-Hung'
'Ding, Shengda'
'Erdem, Ozlen F.'
'Crouthers, Danielle J.'
'Liu, Tianbiao'
'McCrory, Charles C. L.'
'Lubitz, Wolfgang'
'Popescu, Codrina V.'
'Reibenspies, Joseph H.'
'Hall, Michael B.'
'Darenbourg, Marcetta Y.'
_publ_section_title
;
 Redox active iron nitrosyl units in proton reduction electrocatalysis
;
_journal_name_full               'Nature Communications'
_journal_page_first              3684
_journal_paper_doi               10.1038/ncomms4684
_journal_volume                  5
_journal_year                    2014
_chemical_formula_sum            'C9 H18 Fe2 N5 O3 S2'
_chemical_formula_weight         420.10
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.240(7)
_cell_length_b                   14.263(7)
_cell_length_c                   14.821(7)
_cell_measurement_reflns_used    7783
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      2.44
_cell_volume                     3010(3)
_computing_cell_refinement       'APEXII (Bruker, 2012a)'
_computing_data_collection       'APEXII (Bruker, 2012a)'
_computing_data_reduction        'SAINT (Bruker, 2012b)'
_computing_molecular_graphics    'shelXLe (Hübschle 2011)'
_computing_publication_material  'Ciftab (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS (Sheldrick 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32153
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.444
_exptl_absorpt_coefficient_mu    2.220
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2009/1 (Bruker,2009) was employed for absorption correction.
wR2(int) was   0.1108 before and   0.0733 after correction.
The ratio of minimum to maximum transmission factors was   0.8082.
Additional spherical absorption correction applied with mu*r =  0.2000.
The λ/2 correction factor of 0.0015 was applied.
;
_exptl_crystal_colour            'dark green '
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_description       'plate     '
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3470
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0293P)²+3.0424P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0729
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2853
_reflns_number_total             3470
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ncomms4684-s2.cif
_cod_data_source_block           fefe
_cod_database_code               1547478
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.665
_shelx_estimated_absorpt_t_max   0.808
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.44726(2) 0.52854(2) 0.21793(2) 0.01468(9) Uani 1 1 d . . . . .
Fe2 Fe 0.48677(2) 0.66966(2) 0.36373(2) 0.01933(10) Uani 1 1 d . . . . .
S1 S 0.50055(4) 0.50740(4) 0.35879(4) 0.01878(13) Uani 1 1 d . . . . .
S2 S 0.53059(4) 0.66238(5) 0.21189(4) 0.02154(14) Uani 1 1 d . . . . .
O1 O 0.29768(13) 0.72509(15) 0.39713(14) 0.0361(5) Uani 1 1 d . . . . .
O2 O 0.61313(16) 0.76164(17) 0.48318(14) 0.0466(6) Uani 1 1 d . . . . .
O3 O 0.58465(13) 0.41349(15) 0.14111(14) 0.0389(5) Uani 1 1 d . . . . .
N1 N 0.32748(13) 0.45980(13) 0.25384(13) 0.0167(4) Uani 1 1 d . . . . .
N2 N 0.35350(13) 0.58660(15) 0.13078(13) 0.0191(4) Uani 1 1 d . . . . .
N3 N 0.37600(15) 0.70080(15) 0.37911(14) 0.0233(5) Uani 1 1 d . . . . .
N4 N 0.56855(15) 0.71869(16) 0.42847(14) 0.0258(5) Uani 1 1 d . . . . .
N5 N 0.51461(14) 0.45203(15) 0.15938(14) 0.0204(4) Uani 1 1 d . . . . .
C1 C 0.39208(18) 0.46117(18) 0.40956(16) 0.0239(5) Uani 1 1 d . . . . .
H1A H 0.4078 0.4203 0.4614 0.029 Uiso 1 1 calc R U . . .
H1B H 0.3530 0.5136 0.4319 0.029 Uiso 1 1 calc R U . . .
C2 C 0.33839(17) 0.40603(17) 0.33994(16) 0.0209(5) Uani 1 1 d . . . . .
H2A H 0.3719 0.3466 0.3275 0.025 Uiso 1 1 calc R U . . .
H2B H 0.2755 0.3903 0.3641 0.025 Uiso 1 1 calc R U . . .
C3 C 0.29798(17) 0.39168(18) 0.18228(17) 0.0235(5) Uani 1 1 d . . . . .
H3A H 0.2475 0.3512 0.2066 0.028 Uiso 1 1 calc R U . . .
H3B H 0.3520 0.3510 0.1670 0.028 Uiso 1 1 calc R U . . .
C4 C 0.26294(18) 0.4391(2) 0.09673(18) 0.0270(6) Uani 1 1 d . . . . .
H4A H 0.2560 0.3907 0.0493 0.032 Uiso 1 1 calc R U . . .
H4B H 0.1997 0.4651 0.1088 0.032 Uiso 1 1 calc R U . . .
C5 C 0.32448(18) 0.51714(19) 0.06012(16) 0.0266(6) Uani 1 1 d . . . . .
H5A H 0.3815 0.4892 0.0329 0.032 Uiso 1 1 calc R U . . .
H5B H 0.2900 0.5505 0.0118 0.032 Uiso 1 1 calc R U . . .
C6 C 0.25556(16) 0.53595(17) 0.26218(16) 0.0204(5) Uani 1 1 d . . . . .
H6A H 0.2596 0.5647 0.3229 0.025 Uiso 1 1 calc R U . . .
H6B H 0.1919 0.5090 0.2550 0.025 Uiso 1 1 calc R U . . .
C7 C 0.27197(16) 0.61170(19) 0.18957(17) 0.0231(5) Uani 1 1 d . . . . .
H7A H 0.2148 0.6182 0.1520 0.028 Uiso 1 1 calc R U . . .
H7B H 0.2841 0.6727 0.2192 0.028 Uiso 1 1 calc R U . . .
C8 C 0.39196(19) 0.67136(19) 0.08417(17) 0.0270(6) Uani 1 1 d . . . . .
H8A H 0.3395 0.7075 0.0575 0.032 Uiso 1 1 calc R U . . .
H8B H 0.4336 0.6511 0.0344 0.032 Uiso 1 1 calc R U . . .
C9 C 0.44629(18) 0.7339(2) 0.14738(18) 0.0274(6) Uani 1 1 d . . . . .
H9A H 0.4026 0.7658 0.1892 0.033 Uiso 1 1 calc R U . . .
H9B H 0.4803 0.7824 0.1125 0.033 Uiso 1 1 calc R U . . .
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
N5 Fe1 N2 108.00(10) . .
N5 Fe1 N1 107.33(10) . .
N2 Fe1 N1 79.18(8) . .
N5 Fe1 S1 101.47(8) . .
N2 Fe1 S1 150.28(6) . .
N1 Fe1 S1 88.59(6) . .
N5 Fe1 S2 103.17(8) . .
N2 Fe1 S2 88.59(7) . .
N1 Fe1 S2 149.33(6) . .
S1 Fe1 S2 88.43(3) . .
N3 Fe2 N4 118.37(11) . .
N3 Fe2 S1 110.63(8) . .
N4 Fe2 S1 112.20(8) . .
N3 Fe2 S2 113.52(7) . .
N4 Fe2 S2 112.78(8) . .
S1 Fe2 S2 84.43(2) . .
C1 S1 Fe1 98.33(8) . .
C1 S1 Fe2 105.85(9) . .
Fe1 S1 Fe2 82.35(2) . .
C9 S2 Fe1 98.43(9) . .
C9 S2 Fe2 107.52(10) . .
Fe1 S2 Fe2 81.87(2) . .
C6 N1 C2 111.84(18) . .
C6 N1 C3 109.69(18) . .
C2 N1 C3 107.48(19) . .
C6 N1 Fe1 104.18(14) . .
C2 N1 Fe1 112.47(14) . .
C3 N1 Fe1 111.21(14) . .
C8 N2 C7 111.1(2) . .
C8 N2 C5 108.19(19) . .
C7 N2 C5 110.57(19) . .
C8 N2 Fe1 112.45(15) . .
C7 N2 Fe1 103.72(14) . .
C5 N2 Fe1 110.82(15) . .
O1 N3 Fe2 174.8(2) . .
O2 N4 Fe2 167.5(2) . .
O3 N5 Fe1 154.74(19) . .
C2 C1 S1 109.46(17) . .
C2 C1 H1A 109.8 . .
S1 C1 H1A 109.8 . .
C2 C1 H1B 109.8 . .
S1 C1 H1B 109.8 . .
H1A C1 H1B 108.2 . .
N1 C2 C1 111.67(19) . .
N1 C2 H2A 109.3 . .
C1 C2 H2A 109.3 . .
N1 C2 H2B 109.3 . .
C1 C2 H2B 109.3 . .
H2A C2 H2B 107.9 . .
N1 C3 C4 113.2(2) . .
N1 C3 H3A 108.9 . .
C4 C3 H3A 108.9 . .
N1 C3 H3B 108.9 . .
C4 C3 H3B 108.9 . .
H3A C3 H3B 107.8 . .
C5 C4 C3 115.8(2) . .
C5 C4 H4A 108.3 . .
C3 C4 H4A 108.3 . .
C5 C4 H4B 108.3 . .
C3 C4 H4B 108.3 . .
H4A C4 H4B 107.4 . .
N2 C5 C4 113.2(2) . .
N2 C5 H5A 108.9 . .
C4 C5 H5A 108.9 . .
N2 C5 H5B 108.9 . .
C4 C5 H5B 108.9 . .
H5A C5 H5B 107.8 . .
N1 C6 C7 110.29(19) . .
N1 C6 H6A 109.6 . .
C7 C6 H6A 109.6 . .
N1 C6 H6B 109.6 . .
C7 C6 H6B 109.6 . .
H6A C6 H6B 108.1 . .
N2 C7 C6 110.88(19) . .
N2 C7 H7A 109.5 . .
C6 C7 H7A 109.5 . .
N2 C7 H7B 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 108.1 . .
N2 C8 C9 112.3(2) . .
N2 C8 H8A 109.2 . .
C9 C8 H8A 109.2 . .
N2 C8 H8B 109.1 . .
C9 C8 H8B 109.2 . .
H8A C8 H8B 107.9 . .
C8 C9 S2 109.24(19) . .
C8 C9 H9A 109.8 . .
S2 C9 H9A 109.8 . .
C8 C9 H9B 109.8 . .
S2 C9 H9B 109.8 . .
H9A C9 H9B 108.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N5 1.692(2) .
Fe1 N2 2.034(2) .
Fe1 N1 2.038(2) .
Fe1 S1 2.2416(11) .
Fe1 S2 2.2495(11) .
Fe2 N3 1.654(2) .
Fe2 N4 1.663(2) .
Fe2 S1 2.3238(13) .
Fe2 S2 2.3377(12) .
S1 C1 1.840(3) .
S2 C9 1.843(3) .
O1 N3 1.198(3) .
O2 N4 1.198(3) .
O3 N5 1.171(3) .
N1 C6 1.498(3) .
N1 C2 1.497(3) .
N1 C3 1.498(3) .
N2 C8 1.496(3) .
N2 C7 1.495(3) .
N2 C5 1.500(3) .
C1 C2 1.506(3) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.521(4) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C5 1.517(4) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 C7 1.543(3) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C9 1.507(4) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
N3 Fe2 N4 O2 5.0(10) . . . .
S1 Fe2 N4 O2 -125.7(10) . . . .
S2 Fe2 N4 O2 141.0(9) . . . .
N2 Fe1 N5 O3 143.0(5) . . . .
N1 Fe1 N5 O3 -133.1(5) . . . .
S1 Fe1 N5 O3 -40.9(5) . . . .
S2 Fe1 N5 O3 50.1(5) . . . .
Fe1 S1 C1 C2 32.36(18) . . . .
Fe2 S1 C1 C2 116.72(16) . . . .
C6 N1 C2 C1 -74.9(2) . . . .
C3 N1 C2 C1 164.7(2) . . . .
Fe1 N1 C2 C1 42.0(2) . . . .
S1 C1 C2 N1 -49.6(2) . . . .
C6 N1 C3 C4 45.1(3) . . . .
C2 N1 C3 C4 166.9(2) . . . .
Fe1 N1 C3 C4 -69.5(2) . . . .
N1 C3 C4 C5 47.8(3) . . . .
C8 N2 C5 C4 -165.8(2) . . . .
C7 N2 C5 C4 -43.9(3) . . . .
Fe1 N2 C5 C4 70.5(2) . . . .
C3 C4 C5 N2 -48.3(3) . . . .
C2 N1 C6 C7 158.3(2) . . . .
C3 N1 C6 C7 -82.6(2) . . . .
Fe1 N1 C6 C7 36.5(2) . . . .
C8 N2 C7 C6 -159.2(2) . . . .
C5 N2 C7 C6 80.6(2) . . . .
Fe1 N2 C7 C6 -38.2(2) . . . .
N1 C6 C7 N2 1.1(3) . . . .
C7 N2 C8 C9 73.7(3) . . . .
C5 N2 C8 C9 -164.7(2) . . . .
Fe1 N2 C8 C9 -42.0(3) . . . .
N2 C8 C9 S2 49.0(3) . . . .
Fe1 S2 C9 C8 -31.49(19) . . . .
Fe2 S2 C9 C8 -115.56(17) . . . .
