#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:51:26 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180099 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/45/7054550.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_7054550
loop_
_publ_author_name
'Sanina, Nataliya A.'
'Aldoshin, Sergey M.'
'Shmatko, Natal'ya Yu.'
'Korchagin, Denis V.'
'Shilov, Gennadii V.'
'Knyazkina, Ekaterine V.'
'Ovanesyan, Nikolay S.'
'Kulikov, Alexander V.'
_publ_section_title
;
 Nitrosyl iron complexes with enhanced NO donating ability: synthesis,
 structure and properties of a new type of salt with the DNIC cations
 [Fe(SC(NH2)2)2(NO)2]+
;
_journal_issue                   2
_journal_name_full               'New J. Chem.'
_journal_page_first              1022
_journal_paper_doi               10.1039/C4NJ01693A
_journal_volume                  39
_journal_year                    2015
_chemical_formula_sum            'C4 H16 Fe4 N16 O14 S8'
_chemical_formula_weight         992.21
_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                86.462(4)
_cell_angle_beta                 88.363(4)
_cell_angle_gamma                87.613(4)
_cell_formula_units_Z            1
_cell_length_a                   6.2712(3)
_cell_length_b                   10.4132(5)
_cell_length_c                   12.1912(5)
_cell_measurement_reflns_used    4289
_cell_measurement_temperature    99.9(2)
_cell_measurement_theta_max      37.2837
_cell_measurement_theta_min      3.2458
_cell_volume                     793.65(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      99.9(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13522
_diffrn_reflns_theta_full        36.09
_diffrn_reflns_theta_max         36.09
_diffrn_reflns_theta_min         3.25
_exptl_absorpt_coefficient_mu    2.399
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.708
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         7581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0415
_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)+(0.0268P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                5810
_reflns_number_total             7581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4nj01693a2.cif
_cod_data_source_block           CompoundII
_cod_depositor_comments
'Adding full bibliography for 7054549--7054550.cif.'
_cod_database_code               7054550
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
Fe1 Fe 0.09609(4) 0.50420(3) 0.89720(2) 0.01071(6) Uani 1 1 d .
Fe2 Fe 0.23823(4) 0.73944(3) 0.48034(2) 0.01167(6) Uani 1 1 d .
S1 S 0.06361(7) 0.66511(5) 1.01360(4) 0.01112(9) Uani 1 1 d .
S2 S -0.17879(7) 0.79409(5) 0.95120(4) 0.01041(9) Uani 1 1 d .
S3 S 0.21529(7) 0.92555(5) 0.57825(4) 0.01268(9) Uani 1 1 d .
S4 S 0.44013(7) 0.77717(5) 0.32073(4) 0.01381(10) Uani 1 1 d .
N1 N 0.3601(2) 0.47286(17) 0.88461(13) 0.0125(3) Uani 1 1 d .
N2 N -0.0366(2) 0.54960(19) 0.78303(14) 0.0153(3) Uani 1 1 d .
N3 N -0.0104(3) 0.69384(19) 0.45599(14) 0.0167(3) Uani 1 1 d .
N4 N 0.3807(3) 0.63284(18) 0.56191(14) 0.0146(3) Uani 1 1 d .
N5 N 0.6144(2) 0.88509(18) 0.64943(14) 0.0145(3) Uani 1 1 d .
H5A H 0.7083 0.8602 0.6971 0.017 Uiso 1 1 calc R
H5B H 0.6542 0.9145 0.5849 0.017 Uiso 1 1 calc R
N6 N 0.3452(3) 0.8336(2) 0.77314(14) 0.0180(4) Uani 1 1 d .
H6A H 0.4375 0.8084 0.8215 0.022 Uiso 1 1 calc R
H6B H 0.2110 0.8296 0.7889 0.022 Uiso 1 1 calc R
N7 N 0.0660(2) 0.86512(18) 0.23505(14) 0.0150(3) Uani 1 1 d .
H7A H -0.0088 0.9014 0.1829 0.018 Uiso 1 1 calc R
H7B H 0.0047 0.8383 0.2957 0.018 Uiso 1 1 calc R
N8 N 0.3651(3) 0.89289(18) 0.12761(14) 0.0149(3) Uani 1 1 d .
H8A H 0.2872 0.9289 0.0766 0.018 Uiso 1 1 calc R
H8B H 0.5011 0.8844 0.1174 0.018 Uiso 1 1 calc R
O1 O 0.5388(2) 0.45523(17) 0.86156(13) 0.0193(3) Uani 1 1 d .
O2 O -0.0988(3) 0.5844(2) 0.69654(13) 0.0293(4) Uani 1 1 d .
O3 O -0.1655(2) 0.63437(19) 0.45543(14) 0.0275(4) Uani 1 1 d .
O4 O 0.4503(2) 0.55430(17) 0.62438(14) 0.0234(3) Uani 1 1 d .
O5 O -0.0932(2) 0.84403(15) 0.84500(12) 0.0151(3) Uani 1 1 d .
O6 O -0.3750(2) 0.72789(15) 0.94184(12) 0.0152(3) Uani 1 1 d .
O7 O -0.1946(2) 0.89207(15) 1.03271(12) 0.0144(3) Uani 1 1 d .
C1 C 0.4091(3) 0.8781(2) 0.67531(16) 0.0121(3) Uani 1 1 d .
C2 C 0.2756(3) 0.8505(2) 0.22196(16) 0.0123(3) Uani 1 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'
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'
H H 0.0000 0.0000 '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 117.85(8) . .
N2 Fe1 S1 108.53(7) . .
N1 Fe1 S1 104.65(6) . .
N2 Fe1 S1 109.61(6) . 2_567
N1 Fe1 S1 110.08(6) . 2_567
S1 Fe1 S1 105.275(19) . 2_567
N2 Fe1 Fe1 122.58(6) . 2_567
N1 Fe1 Fe1 119.43(6) . 2_567
S1 Fe1 Fe1 52.751(16) . 2_567
S1 Fe1 Fe1 52.523(16) 2_567 2_567
N3 Fe2 N4 114.18(9) . .
N3 Fe2 S4 112.72(6) . .
N4 Fe2 S4 106.97(6) . .
N3 Fe2 S3 109.19(7) . .
N4 Fe2 S3 103.95(6) . .
S4 Fe2 S3 109.42(2) . .
S2 S1 Fe1 106.35(2) . .
S2 S1 Fe1 107.87(2) . 2_567
Fe1 S1 Fe1 74.73(2) . 2_567
O6 S2 O5 112.78(9) . .
O6 S2 O7 113.01(8) . .
O5 S2 O7 112.48(9) . .
O6 S2 S1 110.32(7) . .
O5 S2 S1 104.59(6) . .
O7 S2 S1 102.84(6) . .
C1 S3 Fe2 97.34(7) . .
C2 S4 Fe2 108.27(7) . .
O1 N1 Fe1 171.12(16) . .
O2 N2 Fe1 169.71(15) . .
O3 N3 Fe2 162.53(18) . .
O4 N4 Fe2 170.10(16) . .
N6 C1 N5 120.94(18) . .
N6 C1 S3 118.44(14) . .
N5 C1 S3 120.61(15) . .
N7 C2 N8 118.48(18) . .
N7 C2 S4 123.67(15) . .
N8 C2 S4 117.85(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N2 1.6751(18) .
Fe1 N1 1.6787(16) .
Fe1 S1 2.2608(6) .
Fe1 S1 2.2676(6) 2_567
Fe1 Fe1 2.7482(5) 2_567
Fe2 N3 1.6883(17) .
Fe2 N4 1.6887(18) .
Fe2 S4 2.3130(5) .
Fe2 S3 2.3353(6) .
S1 S2 2.1127(7) .
S1 Fe1 2.2677(6) 2_567
S2 O6 1.4459(14) .
S2 O5 1.4612(14) .
S2 O7 1.4660(16) .
S3 C1 1.755(2) .
S4 C2 1.729(2) .
N1 O1 1.1574(19) .
N2 O2 1.166(2) .
N3 O3 1.175(2) .
N4 O4 1.163(2) .
N5 C1 1.321(2) .
N6 C1 1.311(2) .
N7 C2 1.323(2) .
N8 C2 1.324(2) .
