#------------------------------------------------------------------------------
#$Date: 2016-03-25 21:21:48 +0100 (vie 25 de mar de 2016) $
#$Revision: 180009 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/03/7030342.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_7030342
loop_
_publ_author_name
'Yeh, Shih-Wey'
'Tsou, Chih-Chin'
'Liaw, Wen-Feng'
_publ_section_title
;
 The dinitrosyliron complex [Fe4(μ3-S)2(μ2-NO)2(NO)6](2-) containing
 bridging nitroxyls: (15)N (NO) NMR analysis of the bridging and terminal
 NO-coordinate ligands.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9022
_journal_page_last               9025
_journal_paper_doi               10.1039/c4dt00450g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C24 H48 Fe4 K2 N8 O20 S2'
_chemical_formula_sum            'C24 H48 Fe4 K2 N8 O20 S2'
_chemical_formula_weight         1134.42
_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                99.547(4)
_cell_angle_beta                 109.035(3)
_cell_angle_gamma                113.002(3)
_cell_formula_units_Z            1
_cell_length_a                   9.479(2)
_cell_length_b                   11.160(2)
_cell_length_c                   12.966(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1123.7(4)
_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_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9349
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    1.623
_exptl_absorpt_correction_T_max  0.8417
_exptl_absorpt_correction_T_min  0.5558
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown(dark)
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             582
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0408
_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)+(0.0957P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1486
_reflns_number_gt                3194
_reflns_number_total             3956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00450g2.cif
_cod_data_source_block           ch15230
_cod_depositor_comments          'Adding full bibliography for 7030342.cif.'
_cod_database_code               7030342
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 0.9311(5) 1.1954(4) 0.4873(4) 0.0364(11) Uani 1 1 d .
H1A H 1.0537 1.2273 0.5319 0.044 Uiso 1 1 calc R
H1B H 0.9022 1.2621 0.5237 0.044 Uiso 1 1 calc R
C2 C 0.8939(5) 1.1884(5) 0.3651(4) 0.0357(11) Uani 1 1 d .
H2A H 0.9656 1.2797 0.3631 0.043 Uiso 1 1 calc R
H2B H 0.9203 1.1200 0.3282 0.043 Uiso 1 1 calc R
C3 C 0.6753(6) 1.1444(4) 0.1860(4) 0.0349(11) Uani 1 1 d .
H3A H 0.7004 1.0777 0.1452 0.042 Uiso 1 1 calc R
H3B H 0.7427 1.2366 0.1834 0.042 Uiso 1 1 calc R
C4 C 0.4913(6) 1.1013(4) 0.1283(4) 0.0366(11) Uani 1 1 d .
H4A H 0.4636 1.1611 0.1745 0.044 Uiso 1 1 calc R
H4B H 0.4619 1.1108 0.0505 0.044 Uiso 1 1 calc R
C5 C 0.2182(5) 0.9144(5) 0.0720(4) 0.0348(11) Uani 1 1 d .
H5A H 0.1784 0.9271 -0.0041 0.042 Uiso 1 1 calc R
H5B H 0.1930 0.9686 0.1251 0.042 Uiso 1 1 calc R
C6 C 0.1296(5) 0.7645(4) 0.0583(4) 0.0351(11) Uani 1 1 d .
H6A H 0.0051 0.7276 0.0197 0.042 Uiso 1 1 calc R
H6B H 0.1617 0.7114 0.0099 0.042 Uiso 1 1 calc R
C7 C 0.0954(8) 0.6187(6) 0.1730(6) 0.078(2) Uani 1 1 d .
H7A H -0.0091 0.6072 0.1810 0.094 Uiso 1 1 calc R
H7B H 0.0596 0.5518 0.0972 0.094 Uiso 1 1 calc R
C8 C 0.1836(9) 0.5835(5) 0.2577(5) 0.076(2) Uani 1 1 d .
H8A H 0.0996 0.5090 0.2715 0.091 Uiso 1 1 calc R
H8B H 0.2437 0.5431 0.2266 0.091 Uiso 1 1 calc R
C9 C 0.4017(7) 0.6448(5) 0.4420(4) 0.0480(14) Uani 1 1 d .
H9A H 0.4867 0.6370 0.4168 0.058 Uiso 1 1 calc R
H9B H 0.3307 0.5539 0.4449 0.058 Uiso 1 1 calc R
C10 C 0.4887(6) 0.7497(5) 0.5575(4) 0.0438(12) Uani 1 1 d .
H10A H 0.4024 0.7557 0.5821 0.053 Uiso 1 1 calc R
H10B H 0.5556 0.7198 0.6131 0.053 Uiso 1 1 calc R
C11 C 0.7713(5) 0.9124(5) 0.5965(4) 0.0337(10) Uani 1 1 d .
H11A H 0.7766 0.8452 0.5396 0.040 Uiso 1 1 calc R
H11B H 0.8151 0.9015 0.6730 0.040 Uiso 1 1 calc R
C12 C 0.8784(5) 1.0545(5) 0.6035(4) 0.0342(10) Uani 1 1 d .
H12A H 0.8606 1.1211 0.6514 0.041 Uiso 1 1 calc R
H12B H 0.9998 1.0787 0.6402 0.041 Uiso 1 1 calc R
N1 N 0.7704(4) 0.7717(3) 0.0915(3) 0.0283(8) Uani 1 1 d .
N2 N 0.6039(4) 0.6575(3) 0.2165(3) 0.0259(8) Uani 1 1 d .
N3 N 0.3779(5) 0.3730(4) 0.1904(3) 0.0328(9) Uani 1 1 d .
N4 N 0.7335(5) 0.4854(3) 0.3267(3) 0.0334(9) Uani 1 1 d .
O1 O 0.8725(4) 0.8855(3) 0.1088(3) 0.0486(9) Uani 1 1 d .
O2 O 0.6410(4) 0.7562(3) 0.2966(3) 0.0382(8) Uani 1 1 d .
O3 O 0.2526(4) 0.2955(4) 0.1933(3) 0.0551(10) Uani 1 1 d .
O4 O 0.8296(4) 0.4782(3) 0.4075(3) 0.0549(10) Uani 1 1 d .
O5 O 0.8337(4) 1.0618(3) 0.4892(2) 0.0316(7) Uani 1 1 d .
O6 O 0.7202(3) 1.1494(3) 0.3038(3) 0.0297(7) Uani 1 1 d .
O7 O 0.3960(3) 0.9605(3) 0.1178(3) 0.0320(7) Uani 1 1 d .
O8 O 0.1779(4) 0.7510(3) 0.1699(3) 0.0389(8) Uani 1 1 d .
O9 O 0.2985(4) 0.6815(3) 0.3617(3) 0.0503(9) Uani 1 1 d .
O10 O 0.6000(4) 0.8847(3) 0.5627(3) 0.0348(7) Uani 1 1 d .
S1 S 0.63493(13) 0.42962(10) 0.05531(9) 0.0256(3) Uani 1 1 d .
Fe1 Fe 0.61957(7) 0.62523(5) 0.08406(5) 0.0222(2) Uani 1 1 d .
Fe2 Fe 0.57747(7) 0.47242(6) 0.21133(5) 0.0258(2) Uani 1 1 d .
K1 K 0.49907(11) 0.92468(8) 0.33592(8) 0.0286(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'
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'
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
O5 C1 C2 109.2(3) . .
O5 C1 H1A 109.8 . .
C2 C1 H1A 109.8 . .
O5 C1 H1B 109.8 . .
C2 C1 H1B 109.8 . .
H1A C1 H1B 108.3 . .
O6 C2 C1 109.3(4) . .
O6 C2 H2A 109.8 . .
C1 C2 H2A 109.8 . .
O6 C2 H2B 109.8 . .
C1 C2 H2B 109.8 . .
H2A C2 H2B 108.3 . .
O6 C3 C4 109.1(4) . .
O6 C3 H3A 109.9 . .
C4 C3 H3A 109.9 . .
O6 C3 H3B 109.9 . .
C4 C3 H3B 109.9 . .
H3A C3 H3B 108.3 . .
O7 C4 C3 108.9(3) . .
O7 C4 H4A 109.9 . .
C3 C4 H4A 109.9 . .
O7 C4 H4B 109.9 . .
C3 C4 H4B 109.9 . .
H4A C4 H4B 108.3 . .
O7 C5 C6 108.4(3) . .
O7 C5 K1 49.49(19) . .
C6 C5 K1 81.4(2) . .
O7 C5 H5A 110.0 . .
C6 C5 H5A 110.0 . .
K1 C5 H5A 159.5 . .
O7 C5 H5B 110.0 . .
C6 C5 H5B 110.0 . .
K1 C5 H5B 82.0 . .
H5A C5 H5B 108.4 . .
O8 C6 C5 108.6(3) . .
O8 C6 H6A 110.0 . .
C5 C6 H6A 110.0 . .
O8 C6 H6B 110.0 . .
C5 C6 H6B 110.0 . .
H6A C6 H6B 108.3 . .
C8 C7 O8 117.4(5) . .
C8 C7 H7A 107.9 . .
O8 C7 H7A 107.9 . .
C8 C7 H7B 107.9 . .
O8 C7 H7B 107.9 . .
H7A C7 H7B 107.2 . .
O9 C8 C7 119.4(5) . .
O9 C8 K1 47.9(2) . .
C7 C8 K1 82.3(3) . .
O9 C8 H8A 107.5 . .
C7 C8 H8A 107.5 . .
K1 C8 H8A 152.9 . .
O9 C8 H8B 107.5 . .
C7 C8 H8B 107.5 . .
K1 C8 H8B 93.4 . .
H8A C8 H8B 107.0 . .
O9 C9 C10 110.1(4) . .
O9 C9 K1 47.8(2) . .
C10 C9 K1 86.3(3) . .
O9 C9 H9A 109.6 . .
C10 C9 H9A 109.6 . .
K1 C9 H9A 80.5 . .
O9 C9 H9B 109.6 . .
C10 C9 H9B 109.6 . .
K1 C9 H9B 156.9 . .
H9A C9 H9B 108.2 . .
O10 C10 C9 113.6(4) . .
O10 C10 H10A 108.8 . .
C9 C10 H10A 108.8 . .
O10 C10 H10B 108.8 . .
C9 C10 H10B 108.8 . .
H10A C10 H10B 107.7 . .
O10 C11 C12 110.4(3) . .
O10 C11 H11A 109.6 . .
C12 C11 H11A 109.6 . .
O10 C11 H11B 109.6 . .
C12 C11 H11B 109.6 . .
H11A C11 H11B 108.1 . .
O5 C12 C11 109.0(3) . .
O5 C12 H12A 109.9 . .
C11 C12 H12A 109.9 . .
O5 C12 H12B 109.9 . .
C11 C12 H12B 109.9 . .
H12A C12 H12B 108.3 . .
O1 N1 Fe1 170.2(3) . .
O2 N2 Fe1 138.8(3) . .
O2 N2 Fe2 131.0(3) . .
Fe1 N2 Fe2 87.10(14) . .
O3 N3 Fe2 166.7(3) . .
O4 N4 Fe2 171.5(3) . .
N2 O2 K1 135.6(3) . .
C1 O5 C12 113.0(3) . .
C1 O5 K1 116.0(2) . .
C12 O5 K1 118.5(2) . .
C2 O6 C3 112.7(3) . .
C2 O6 K1 114.4(2) . .
C3 O6 K1 115.2(2) . .
C5 O7 C4 112.5(3) . .
C5 O7 K1 108.0(2) . .
C4 O7 K1 110.7(2) . .
C7 O8 C6 115.7(4) . .
C7 O8 K1 118.2(3) . .
C6 O8 K1 119.1(2) . .
C8 O9 C9 117.5(4) . .
C8 O9 K1 111.1(3) . .
C9 O9 K1 110.2(3) . .
C11 O10 C10 113.8(3) . .
C11 O10 K1 123.7(2) . 2_676
C10 O10 K1 106.5(3) . 2_676
C11 O10 K1 104.6(2) . .
C10 O10 K1 112.3(2) . .
K1 O10 K1 94.05(8) 2_676 .
Fe1 S1 Fe1 75.41(4) . 2_665
Fe1 S1 Fe2 69.62(3) . .
Fe1 S1 Fe2 97.75(5) 2_665 .
N1 Fe1 N2 106.51(16) . .
N1 Fe1 S1 122.19(12) . .
N2 Fe1 S1 105.56(11) . .
N1 Fe1 S1 110.66(12) . 2_665
N2 Fe1 S1 106.29(11) . 2_665
S1 Fe1 S1 104.59(4) . 2_665
N1 Fe1 Fe2 137.86(12) . .
N2 Fe1 Fe2 49.78(10) . .
S1 Fe1 Fe2 56.33(3) . .
S1 Fe1 Fe2 109.71(4) 2_665 .
N1 Fe1 Fe1 136.29(13) . 2_665
N2 Fe1 Fe1 116.66(11) . 2_665
S1 Fe1 Fe1 52.87(3) . 2_665
S1 Fe1 Fe1 51.72(3) 2_665 2_665
Fe2 Fe1 Fe1 80.10(3) . 2_665
N4 Fe2 N3 117.35(18) . .
N4 Fe2 N2 109.79(15) . .
N3 Fe2 N2 107.29(16) . .
N4 Fe2 S1 107.93(14) . .
N3 Fe2 S1 115.71(13) . .
N2 Fe2 S1 96.71(10) . .
N4 Fe2 Fe1 124.51(12) . .
N3 Fe2 Fe1 117.25(13) . .
N2 Fe2 Fe1 43.12(10) . .
S1 Fe2 Fe1 54.06(3) . .
O8 K1 O5 169.65(10) . .
O8 K1 O6 121.70(9) . .
O5 K1 O6 61.12(9) . .
O8 K1 O2 97.39(10) . .
O5 K1 O2 72.27(9) . .
O6 K1 O2 96.34(9) . .
O8 K1 O9 59.95(9) . .
O5 K1 O9 115.90(10) . .
O6 K1 O9 172.77(10) . .
O2 K1 O9 76.43(11) . .
O8 K1 O7 60.68(9) . .
O5 K1 O7 120.17(9) . .
O6 K1 O7 61.22(8) . .
O2 K1 O7 99.72(9) . .
O9 K1 O7 119.28(9) . .
O8 K1 O10 93.21(9) . 2_676
O5 K1 O10 96.99(9) . 2_676
O6 K1 O10 85.96(8) . 2_676
O2 K1 O10 165.85(9) . 2_676
O9 K1 O10 101.11(10) . 2_676
O7 K1 O10 93.64(9) . 2_676
O8 K1 O10 118.35(9) . .
O5 K1 O10 60.86(9) . .
O6 K1 O10 119.70(9) . .
O2 K1 O10 80.77(9) . .
O9 K1 O10 59.88(9) . .
O7 K1 O10 178.94(9) . .
O10 K1 O10 85.95(8) 2_676 .
O8 K1 C8 42.07(12) . .
O5 K1 C8 131.33(12) . .
O6 K1 C8 156.38(14) . .
O2 K1 C8 73.50(15) . .
O9 K1 C8 21.03(13) . .
O7 K1 C8 98.82(12) . .
O10 K1 C8 109.19(15) 2_676 .
O10 K1 C8 80.40(12) . .
O8 K1 C9 80.82(11) . .
O5 K1 C9 94.13(11) . .
O6 K1 C9 153.14(11) . .
O2 K1 C9 64.00(11) . .
O9 K1 C9 22.04(11) . .
O7 K1 C9 136.55(10) . .
O10 K1 C9 108.80(11) 2_676 .
O10 K1 C9 42.86(10) . .
C8 K1 C9 39.18(13) . .
O8 K1 C5 42.08(9) . .
O5 K1 C5 141.20(10) . .
O6 K1 C5 80.27(10) . .
O2 K1 C5 111.10(10) . .
O9 K1 C5 101.98(10) . .
O7 K1 C5 22.50(9) . .
O10 K1 C5 83.05(10) 2_676 .
O10 K1 C5 156.44(10) . .
C8 K1 C5 83.64(13) . .
C9 K1 C5 122.76(11) . .
O8 K1 K1 111.33(8) . 2_676
O5 K1 K1 75.46(7) . 2_676
O6 K1 K1 106.97(7) . 2_676
O2 K1 K1 123.39(7) . 2_676
O9 K1 K1 77.70(8) . 2_676
O7 K1 K1 136.80(7) . 2_676
O10 K1 K1 43.17(6) 2_676 2_676
O10 K1 K1 42.78(6) . 2_676
C8 K1 K1 96.28(13) . 2_676
C9 K1 K1 73.54(9) . 2_676
C5 K1 K1 123.11(8) . 2_676
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O5 1.424(5) .
C1 C2 1.489(6) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 O6 1.416(5) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 O6 1.430(5) .
C3 C4 1.486(6) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 O7 1.429(5) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 O7 1.423(5) .
C5 C6 1.497(6) .
C5 K1 3.536(5) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 O8 1.421(5) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.365(8) .
C7 O8 1.389(5) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 O9 1.350(6) .
C8 K1 3.509(5) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 O9 1.413(6) .
C9 C10 1.468(7) .
C9 K1 3.535(5) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 O10 1.437(5) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 O10 1.423(5) .
C11 C12 1.479(6) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 O5 1.428(5) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
N1 O1 1.184(4) .
N1 Fe1 1.660(3) .
N2 O2 1.224(4) .
N2 Fe1 1.761(3) .
N2 Fe2 1.967(3) .
N3 O3 1.182(5) .
N3 Fe2 1.676(4) .
N4 O4 1.181(4) .
N4 Fe2 1.663(4) .
O2 K1 2.777(3) .
O5 K1 2.727(3) .
O6 K1 2.769(3) .
O7 K1 2.827(3) .
O8 K1 2.718(3) .
O9 K1 2.789(3) .
O10 K1 2.928(3) 2_676
O10 K1 2.949(3) .
S1 Fe1 2.2225(12) .
S1 Fe1 2.2573(12) 2_665
S1 Fe2 2.2845(13) .
Fe1 S1 2.2573(12) 2_665
Fe1 Fe2 2.5733(9) .
Fe1 Fe1 2.7398(11) 2_665
K1 O10 2.928(3) 2_676
K1 K1 4.300(2) 2_676
