#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:39:36 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179758 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/54/7005473.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_7005473
loop_
_publ_author_name
'Dillinger, Sandra A. T.'
'Schmalle, Helmut W.'
'Fox, Thomas'
'Berke, Heinz'
_publ_section_title
;
 Developing iron nitrosyl complexes as NO donor prodrugs.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3562
_journal_page_last               3571
_journal_paper_doi               10.1039/b702461d
_journal_year                    2007
_chemical_formula_moiety         'C4 H16 Fe2 N6 O4 S2, H2 O, 2(I)'
_chemical_formula_sum            'C4 H18 Fe2 I2 N6 O5 S2'
_chemical_formula_weight         659.88
_chemical_name_systematic
;
Bis-[dinitrosyl-cysteamine-iron(II)] iodide water
;
_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                90.403(8)
_cell_angle_beta                 93.515(8)
_cell_angle_gamma                116.319(8)
_cell_formula_units_Z            2
_cell_length_a                   6.3097(5)
_cell_length_b                   6.8752(5)
_cell_length_c                   24.5366(17)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.50
_cell_volume                     951.58(14)
_computing_cell_refinement       'Stoe IPDS software'
_computing_data_collection       'Stoe IPDS software'
_computing_data_reduction        'XRED (Stoe & Cie, 1999)'
_computing_molecular_graphics    'PLATON, PLUTON (Spek, 1990, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Stoe IPDS diffractometer'
_diffrn_measurement_method       'φ rotation scan'
_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  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0153
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            10041
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count ' image'
_diffrn_standards_interval_time  3.50
_diffrn_standards_number         '50 to 200'
_exptl_absorpt_coefficient_mu    5.011
_exptl_absorpt_correction_T_max  0.6612
_exptl_absorpt_correction_T_min  0.2970
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Coppens et al. 1965'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.500
_refine_diff_density_min         -1.582
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         4195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0600P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                3491
_reflns_number_total             4195
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b702461d.txt
_cod_data_source_block           7
_cod_database_code               7005473
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe -0.32750(8) 1.15415(8) 0.033333(18) 0.01325(11) Uani 1 d . . .
I1 I 0.05737(4) 1.17775(4) 0.182667(8) 0.02047(8) Uani 1 d . . .
S1 S -0.52575(14) 0.79746(14) 0.04908(3) 0.01551(16) Uani 1 d . . .
H1 H -0.4216 0.6878 0.0523 0.019 Uiso 1 calc R . .
N1 N -0.0459(5) 1.2041(5) 0.02644(11) 0.0177(6) Uani 1 d . . .
O1 O 0.1570(4) 1.2579(5) 0.02703(13) 0.0331(7) Uani 1 d . . .
N2 N -0.3737(5) 1.3025(5) 0.08146(11) 0.0179(6) Uani 1 d . . .
O2 O -0.3582(5) 1.4224(5) 0.11712(11) 0.0309(6) Uani 1 d . . .
C1 C -0.7538(6) 0.7590(6) 0.09593(13) 0.0185(7) Uani 1 d . . .
H1A H -0.8151 0.8673 0.0893 0.022 Uiso 1 calc R . .
H1B H -0.8874 0.6124 0.0895 0.022 Uiso 1 calc R . .
C2 C -0.6504(6) 0.7847(6) 0.15467(13) 0.0187(7) Uani 1 d . . .
H2A H -0.5686 0.6915 0.1599 0.022 Uiso 1 calc R . .
H2B H -0.5328 0.9374 0.1627 0.022 Uiso 1 calc R . .
N3 N -0.8436(5) 0.7221(5) 0.19245(11) 0.0194(6) Uani 1 d . . .
H3A H -0.9152 0.8110 0.1883 0.029 Uiso 1 calc R . .
H3B H -0.7819 0.7347 0.2275 0.029 Uiso 1 calc R . .
H3C H -0.9521 0.5822 0.1846 0.029 Uiso 1 calc R . .
Fe2 Fe 0.82367(8) 0.83373(8) 0.470231(17) 0.01197(11) Uani 1 d . . .
I2 I 0.44653(4) 0.79306(4) 0.322853(9) 0.01939(8) Uani 1 d . . .
S2 S 0.98916(13) 0.81707(14) 0.55334(3) 0.01387(16) Uani 1 d . . .
H2 H 1.0983 0.7122 0.5583 0.017 Uiso 1 calc R . .
N4 N 0.5428(5) 0.7834(5) 0.47810(11) 0.0166(6) Uani 1 d . . .
O3 O 0.3394(4) 0.7274(5) 0.47781(13) 0.0329(7) Uani 1 d . . .
N5 N 0.8656(5) 0.6752(5) 0.42415(11) 0.0167(6) Uani 1 d . . .
O4 O 0.8507(5) 0.5525(5) 0.38961(11) 0.0287(6) Uani 1 d . . .
C3 C 0.7702(6) 0.7889(6) 0.60211(13) 0.0197(7) Uani 1 d . . .
H3D H 0.6891 0.8780 0.5905 0.024 Uiso 1 calc R . .
H3E H 0.6493 0.6355 0.6013 0.024 Uiso 1 calc R . .
C4 C 0.8772(6) 0.8576(6) 0.66014(13) 0.0176(7) Uani 1 d . . .
H4A H 0.9833 1.0155 0.6620 0.021 Uiso 1 calc R . .
H4B H 0.7487 0.8302 0.6846 0.021 Uiso 1 calc R . .
N6 N 1.0149(5) 0.7385(5) 0.67976(11) 0.0162(5) Uani 1 d . . .
H6A H 0.9292 0.5943 0.6711 0.024 Uiso 1 calc R . .
H6B H 1.0447 0.7584 0.7167 0.024 Uiso 1 calc R . .
H6C H 1.1544 0.7905 0.6635 0.024 Uiso 1 calc R . .
O5 O -0.2895(5) 0.4690(5) 0.25330(13) 0.0392(8) Uani 1 d . . .
H51 H -0.4318 0.3833 0.2310 0.08(2) Uiso 1 d . . .
H52 H -0.2726 0.5812 0.2775 0.07(2) Uiso 1 d . . .
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'
I I -0.4742 1.8119 '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'
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
_geom_angle_publ_flag
N1 Fe1 N2 116.70(14) . . ?
N1 Fe1 S1 106.42(11) . . ?
N2 Fe1 S1 110.40(11) . . ?
N1 Fe1 S1 106.82(10) . 2_475 ?
N2 Fe1 S1 109.65(10) . 2_475 ?
S1 Fe1 S1 106.30(3) . 2_475 ?
N1 Fe1 Fe1 118.48(10) . 2_475 ?
N2 Fe1 Fe1 124.82(10) . 2_475 ?
S1 Fe1 Fe1 53.27(3) . 2_475 ?
S1 Fe1 Fe1 53.04(3) 2_475 2_475 ?
C1 S1 Fe1 108.77(13) . . ?
C1 S1 Fe1 105.40(11) . 2_475 ?
Fe1 S1 Fe1 73.70(3) . 2_475 ?
C1 S1 H1 119.9 . . ?
Fe1 S1 H1 119.9 . . ?
Fe1 S1 H1 119.9 2_475 . ?
O1 N1 Fe1 171.4(3) . . ?
O2 N2 Fe1 166.6(3) . . ?
C2 C1 S1 109.9(2) . . ?
C2 C1 H1A 109.7 . . ?
S1 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
S1 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 109.6(3) . . ?
N3 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
N3 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
C2 N3 H3A 109.5 . . ?
C2 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
C2 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
N4 Fe2 N5 116.53(14) . . ?
N4 Fe2 S2 106.16(11) . 2_776 ?
N5 Fe2 S2 109.40(11) . 2_776 ?
N4 Fe2 S2 107.44(10) . . ?
N5 Fe2 S2 110.59(10) . . ?
S2 Fe2 S2 106.16(3) 2_776 . ?
N4 Fe2 Fe2 118.75(10) . 2_776 ?
N5 Fe2 Fe2 124.69(10) . 2_776 ?
S2 Fe2 Fe2 53.18(3) 2_776 2_776 ?
S2 Fe2 Fe2 52.98(3) . 2_776 ?
C3 S2 Fe2 109.44(13) . 2_776 ?
C3 S2 Fe2 105.99(11) . . ?
Fe2 S2 Fe2 73.84(3) 2_776 . ?
C3 S2 H2 119.5 . . ?
Fe2 S2 H2 119.5 2_776 . ?
Fe2 S2 H2 119.5 . . ?
O3 N4 Fe2 170.7(3) . . ?
O4 N5 Fe2 167.4(3) . . ?
C4 C3 S2 113.3(2) . . ?
C4 C3 H3D 108.9 . . ?
S2 C3 H3D 108.9 . . ?
C4 C3 H3E 108.9 . . ?
S2 C3 H3E 108.9 . . ?
H3D C3 H3E 107.7 . . ?
N6 C4 C3 112.2(3) . . ?
N6 C4 H4A 109.2 . . ?
C3 C4 H4A 109.2 . . ?
N6 C4 H4B 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C4 N6 H6A 109.5 . . ?
C4 N6 H6B 109.5 . . ?
H6A N6 H6B 109.5 . . ?
C4 N6 H6C 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
H51 O5 H52 123.9 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 1.673(3) . ?
Fe1 N2 1.676(3) . ?
Fe1 S1 2.2540(10) . ?
Fe1 S1 2.2606(9) 2_475 ?
Fe1 Fe1 2.7075(10) 2_475 ?
S1 C1 1.825(3) . ?
S1 Fe1 2.2607(9) 2_475 ?
S1 H1 1.2000 . ?
N1 O1 1.163(4) . ?
N2 O2 1.167(4) . ?
C1 C2 1.521(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.487(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
Fe2 N4 1.673(3) . ?
Fe2 N5 1.677(3) . ?
Fe2 S2 2.2544(10) 2_776 ?
Fe2 S2 2.2606(8) . ?
Fe2 Fe2 2.7122(10) 2_776 ?
S2 C3 1.829(3) . ?
S2 Fe2 2.2544(10) 2_776 ?
S2 H2 1.2000 . ?
N4 O3 1.165(4) . ?
N5 O4 1.161(4) . ?
C3 C4 1.515(4) . ?
C3 H3D 0.9900 . ?
C3 H3E 0.9900 . ?
C4 N6 1.498(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
N6 H6A 0.9100 . ?
N6 H6B 0.9100 . ?
N6 H6C 0.9100 . ?
O5 H51 0.958 . ?
O5 H52 0.934 . ?
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
_geom_torsion_publ_flag
N1 Fe1 S1 C1 145.28(15) . . . . ?
N2 Fe1 S1 C1 17.73(15) . . . . ?
S1 Fe1 S1 C1 -101.12(11) 2_475 . . . ?
Fe1 Fe1 S1 C1 -101.12(11) 2_475 . . . ?
N1 Fe1 S1 Fe1 -113.60(10) . . . 2_475 ?
N2 Fe1 S1 Fe1 118.85(10) . . . 2_475 ?
S1 Fe1 S1 Fe1 0.0 2_475 . . 2_475 ?
N1 Fe1 N2 O2 -3.2(13) . . . . ?
S1 Fe1 N2 O2 118.5(13) . . . . ?
S1 Fe1 N2 O2 -124.8(13) 2_475 . . . ?
Fe1 Fe1 N2 O2 177.2(12) 2_475 . . . ?
Fe1 S1 C1 C2 -87.4(2) . . . . ?
Fe1 S1 C1 C2 -165.0(2) 2_475 . . . ?
S1 C1 C2 N3 -171.8(2) . . . . ?
N4 Fe2 S2 C3 -7.14(18) . . . . ?
N5 Fe2 S2 C3 -135.33(18) . . . . ?
S2 Fe2 S2 C3 106.11(14) 2_776 . . . ?
Fe2 Fe2 S2 C3 106.11(14) 2_776 . . . ?
N4 Fe2 S2 Fe2 -113.24(11) . . . 2_776 ?
N5 Fe2 S2 Fe2 118.57(12) . . . 2_776 ?
S2 Fe2 S2 Fe2 0.0 2_776 . . 2_776 ?
N4 Fe2 N5 O4 10.0(14) . . . . ?
S2 Fe2 N5 O4 -110.4(13) 2_776 . . . ?
S2 Fe2 N5 O4 133.1(13) . . . . ?
Fe2 Fe2 N5 O4 -168.4(13) 2_776 . . . ?
Fe2 S2 C3 C4 -80.5(3) 2_776 . . . ?
Fe2 S2 C3 C4 -158.6(2) . . . . ?
S2 C3 C4 N6 -55.5(4) . . . . ?
