#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:05:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179230 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/50/4315075.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_4315075
loop_
_publ_author_name
'Chien-Hong Chen'
'Show-Jen Chiou'
'Hsuan-Yin Chen'
_publ_section_title
;
 Dinuclear [{Fe(NO)2}10-{Fe(NO)2}10] Dinitrosyl Iron Complex with
 Thiolate-CO-Bridged Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2023
_journal_page_last               2025
_journal_paper_doi               10.1021/ic902324d
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C33 H30 Fe2 N5 O5 P S'
_chemical_formula_weight         751.35
_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                97.546(1)
_cell_angle_beta                 107.892(1)
_cell_angle_gamma                103.524(1)
_cell_formula_units_Z            2
_cell_length_a                   10.7977(6)
_cell_length_b                   11.7717(7)
_cell_length_c                   14.8627(9)
_cell_measurement_reflns_used    6157
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.33
_cell_volume                     1705.28(17)
_computing_cell_refinement       'Bruker SAINT'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'BRUKER SMART APEXCCD area detector'
_diffrn_measurement_method       '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  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22120
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  0.7870
_exptl_absorpt_correction_T_min  0.6890
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            deep-blue
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.097
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         7793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0599P)²+1.2875P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1181
_reflns_number_gt                6741
_reflns_number_total             7793
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902324d_si_003_3.cif
_cod_data_source_block           ic13598
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4315075
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.42399(4) 0.02926(3) 0.20825(3) 0.02831(10) Uani 1 1 d . . .
Fe2 Fe 0.45904(4) 0.24250(3) 0.30244(3) 0.02894(10) Uani 1 1 d . . .
S1 S 0.63010(6) 0.16805(6) 0.28840(4) 0.02908(14) Uani 1 1 d . . .
N1 N 0.3819(2) 0.02405(19) 0.08996(16) 0.0310(5) Uani 1 1 d . . .
N2 N 0.3976(2) -0.0956(2) 0.24889(17) 0.0361(5) Uani 1 1 d . . .
N3 N 0.4569(2) 0.2799(2) 0.41297(16) 0.0390(5) Uani 1 1 d . . .
N4 N 0.4431(2) 0.3335(2) 0.22602(17) 0.0341(5) Uani 1 1 d . . .
N5 N 0.9304(2) 0.2287(2) 0.3787(2) 0.0453(6) Uani 1 1 d . . .
C1 C 0.2953(3) 0.1029(2) 0.24327(18) 0.0314(5) Uani 1 1 d . . .
C2 C 0.7175(2) 0.1307(2) 0.39801(18) 0.0276(5) Uani 1 1 d . . .
C3 C 0.6498(3) 0.0695(2) 0.4506(2) 0.0341(6) Uani 1 1 d . . .
H3 H 0.5534 0.0495 0.4296 0.041 Uiso 1 1 calc R . .
C4 C 0.7201(3) 0.0369(3) 0.5335(2) 0.0375(6) Uani 1 1 d . . .
H4 H 0.6724 -0.0041 0.5693 0.045 Uiso 1 1 calc R . .
C5 C 0.8595(3) 0.0645(2) 0.5631(2) 0.0362(6) Uani 1 1 d . . .
H5 H 0.9082 0.0410 0.6190 0.043 Uiso 1 1 calc R . .
C6 C 0.9286(3) 0.1259(2) 0.5123(2) 0.0359(6) Uani 1 1 d . . .
H6 H 1.0249 0.1445 0.5336 0.043 Uiso 1 1 calc R . .
C7 C 0.8600(3) 0.1614(2) 0.4299(2) 0.0318(5) Uani 1 1 d . . .
C8 C 0.9349(6) 0.3594(4) 0.4041(4) 0.0577(13) Uani 0.67 1 d P . .
H8A H 0.8441 0.3644 0.4001 0.086 Uiso 0.67 1 calc PR . .
H8B H 0.9642 0.4020 0.3583 0.086 Uiso 0.67 1 calc PR . .
H8C H 0.9992 0.3960 0.4700 0.086 Uiso 0.67 1 calc PR . .
C9 C 1.0728(4) 0.2463(6) 0.4075(4) 0.0655(18) Uani 0.67 1 d P . .
H9A H 1.1191 0.3078 0.4677 0.098 Uiso 0.67 1 calc PR . .
H9B H 1.1050 0.2722 0.3565 0.098 Uiso 0.67 1 calc PR . .
H9C H 1.0925 0.1710 0.4181 0.098 Uiso 0.67 1 calc PR . .
C10 C 0.9093(7) 0.1446(8) 0.2719(6) 0.097(3) Uani 0.67 1 d P . .
H10A H 0.9671 0.0911 0.2824 0.146 Uiso 0.67 1 calc PR . .
H10B H 0.9347 0.1967 0.2302 0.146 Uiso 0.67 1 calc PR . .
H10C H 0.8139 0.0969 0.2406 0.146 Uiso 0.67 1 calc PR . .
O1 O 0.3406(2) 0.00758(18) 0.00422(14) 0.0406(5) Uani 1 1 d . . .
O2 O 0.3676(2) -0.19019(19) 0.26722(18) 0.0521(6) Uani 1 1 d . . .
O3 O 0.4473(3) 0.3165(3) 0.48735(17) 0.0676(8) Uani 1 1 d . . .
O4 O 0.4298(2) 0.40433(19) 0.17719(17) 0.0478(5) Uani 1 1 d . . .
O5 O 0.1817(2) 0.0766(2) 0.23487(16) 0.0462(5) Uani 1 1 d . . .
P1 P 0.12820(6) 0.40908(5) 0.84381(4) 0.02262(13) Uani 1 1 d . . .
C11 C 0.2028(2) 0.3373(2) 0.76852(17) 0.0292(5) Uani 1 1 d . . .
C12 C 0.2732(3) 0.4062(3) 0.7208(2) 0.0392(6) Uani 1 1 d . . .
H12 H 0.2795 0.4889 0.7273 0.047 Uiso 1 1 calc R . .
C13 C 0.3343(3) 0.3546(3) 0.6638(2) 0.0478(8) Uani 1 1 d . . .
H13 H 0.3815 0.4017 0.6307 0.057 Uiso 1 1 calc R . .
C14 C 0.3267(3) 0.2356(3) 0.6551(2) 0.0491(8) Uani 1 1 d . . .
H14 H 0.3698 0.2008 0.6166 0.059 Uiso 1 1 calc R . .
C15 C 0.2573(3) 0.1666(3) 0.7013(2) 0.0488(8) Uani 1 1 d . . .
H15 H 0.2526 0.0842 0.6946 0.059 Uiso 1 1 calc R . .
C16 C 0.1930(3) 0.2161(3) 0.7586(2) 0.0385(6) Uani 1 1 d . . .
H16 H 0.1437 0.1679 0.7900 0.046 Uiso 1 1 calc R . .
C17 C -0.0170(2) 0.4441(2) 0.77000(17) 0.0247(5) Uani 1 1 d . . .
C18 C -0.0583(3) 0.5370(2) 0.80789(19) 0.0319(5) Uani 1 1 d . . .
H18 H -0.0054 0.5864 0.8703 0.038 Uiso 1 1 calc R . .
C19 C -0.1781(3) 0.5566(3) 0.7531(2) 0.0389(6) Uani 1 1 d . . .
H19 H -0.2061 0.6210 0.7778 0.047 Uiso 1 1 calc R . .
C20 C -0.2563(3) 0.4838(3) 0.6637(2) 0.0410(7) Uani 1 1 d . . .
H20 H -0.3389 0.4971 0.6274 0.049 Uiso 1 1 calc R . .
C21 C -0.2152(3) 0.3915(3) 0.6264(2) 0.0398(6) Uani 1 1 d . . .
H21 H -0.2695 0.3413 0.5645 0.048 Uiso 1 1 calc R . .
C22 C -0.0947(3) 0.3716(2) 0.67926(19) 0.0318(5) Uani 1 1 d . . .
H22 H -0.0657 0.3087 0.6533 0.038 Uiso 1 1 calc R . .
C23 C 0.0748(2) 0.3099(2) 0.91525(17) 0.0253(5) Uani 1 1 d . . .
C24 C -0.0573(3) 0.2871(2) 0.91610(19) 0.0302(5) Uani 1 1 d . . .
H24 H -0.1192 0.3229 0.8784 0.036 Uiso 1 1 calc R . .
C25 C -0.0976(3) 0.2116(2) 0.9726(2) 0.0365(6) Uani 1 1 d . . .
H25 H -0.1874 0.1960 0.9737 0.044 Uiso 1 1 calc R . .
C26 C -0.0083(3) 0.1591(2) 1.0270(2) 0.0394(6) Uani 1 1 d . . .
H26 H -0.0368 0.1076 1.0656 0.047 Uiso 1 1 calc R . .
C27 C 0.1227(3) 0.1812(2) 1.0258(2) 0.0369(6) Uani 1 1 d . . .
H27 H 0.1837 0.1443 1.0632 0.044 Uiso 1 1 calc R . .
C28 C 0.1650(3) 0.2565(2) 0.97061(19) 0.0319(5) Uani 1 1 d . . .
H28 H 0.2552 0.2720 0.9702 0.038 Uiso 1 1 calc R . .
C29 C 0.2513(2) 0.5453(2) 0.92089(17) 0.0238(5) Uani 1 1 d . . .
C30 C 0.3203(3) 0.5500(2) 1.01751(18) 0.0319(5) Uani 1 1 d . . .
H30 H 0.2984 0.4828 1.0448 0.038 Uiso 1 1 calc R . .
C31 C 0.4215(3) 0.6533(2) 1.0742(2) 0.0370(6) Uani 1 1 d . . .
H31 H 0.4695 0.6565 1.1403 0.044 Uiso 1 1 calc R . .
C32 C 0.4526(3) 0.7513(2) 1.0347(2) 0.0340(6) Uani 1 1 d . . .
H32 H 0.5226 0.8216 1.0735 0.041 Uiso 1 1 calc R . .
C33 C 0.3824(3) 0.7477(2) 0.9391(2) 0.0317(5) Uani 1 1 d . . .
H33 H 0.4035 0.8158 0.9126 0.038 Uiso 1 1 calc R . .
C34 C 0.2815(2) 0.6457(2) 0.88167(18) 0.0276(5) Uani 1 1 d . . .
H34 H 0.2329 0.6435 0.8160 0.033 Uiso 1 1 calc R . .
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'
P P 0.1023 0.0942 '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
_geom_angle_publ_flag
N2 Fe1 N1 120.65(11) . . ?
N2 Fe1 C1 101.51(11) . . ?
N1 Fe1 C1 103.07(10) . . ?
N2 Fe1 S1 115.87(8) . . ?
N1 Fe1 S1 109.17(7) . . ?
C1 Fe1 S1 103.86(8) . . ?
N2 Fe1 Fe2 126.10(8) . . ?
N1 Fe1 Fe2 110.71(8) . . ?
C1 Fe1 Fe2 49.12(8) . . ?
S1 Fe1 Fe2 55.205(19) . . ?
N3 Fe2 N4 122.01(12) . . ?
N3 Fe2 C1 101.70(11) . . ?
N4 Fe2 C1 105.30(11) . . ?
N3 Fe2 S1 116.88(8) . . ?
N4 Fe2 S1 105.15(8) . . ?
C1 Fe2 S1 103.57(8) . . ?
N3 Fe2 Fe1 126.83(9) . . ?
N4 Fe2 Fe1 109.35(8) . . ?
C1 Fe2 Fe1 48.57(8) . . ?
S1 Fe2 Fe1 55.45(2) . . ?
C2 S1 Fe2 111.48(8) . . ?
C2 S1 Fe1 110.93(9) . . ?
Fe2 S1 Fe1 69.34(2) . . ?
O1 N1 Fe1 172.1(2) . . ?
O2 N2 Fe1 172.2(2) . . ?
O3 N3 Fe2 171.7(3) . . ?
O4 N4 Fe2 174.6(2) . . ?
C9 N5 C7 117.2(3) . . ?
C9 N5 C8 97.5(4) . . ?
C7 N5 C8 109.6(3) . . ?
C9 N5 C10 89.7(4) . . ?
C7 N5 C10 111.0(3) . . ?
C8 N5 C10 129.4(4) . . ?
O5 C1 Fe1 138.6(2) . . ?
O5 C1 Fe2 139.1(2) . . ?
Fe1 C1 Fe2 82.31(10) . . ?
C3 C2 C7 119.2(2) . . ?
C3 C2 S1 122.41(19) . . ?
C7 C2 S1 118.33(19) . . ?
C2 C3 C4 121.3(2) . . ?
C5 C4 C3 119.3(3) . . ?
C6 C5 C4 120.3(3) . . ?
C5 C6 C7 121.2(3) . . ?
C6 C7 C2 118.6(2) . . ?
C6 C7 N5 121.8(2) . . ?
C2 C7 N5 119.5(2) . . ?
C17 P1 C23 108.64(11) . . ?
C17 P1 C29 109.07(11) . . ?
C23 P1 C29 110.37(11) . . ?
C17 P1 C11 109.99(11) . . ?
C23 P1 C11 109.47(12) . . ?
C29 P1 C11 109.29(11) . . ?
C16 C11 C12 120.0(2) . . ?
C16 C11 P1 121.5(2) . . ?
C12 C11 P1 118.6(2) . . ?
C13 C12 C11 120.2(3) . . ?
C14 C13 C12 120.0(3) . . ?
C15 C14 C13 120.4(3) . . ?
C14 C15 C16 120.8(3) . . ?
C11 C16 C15 118.6(3) . . ?
C22 C17 C18 120.4(2) . . ?
C22 C17 P1 119.79(18) . . ?
C18 C17 P1 119.51(19) . . ?
C19 C18 C17 119.0(2) . . ?
C20 C19 C18 120.7(3) . . ?
C19 C20 C21 120.1(3) . . ?
C20 C21 C22 120.1(3) . . ?
C17 C22 C21 119.6(2) . . ?
C24 C23 C28 120.0(2) . . ?
C24 C23 P1 119.53(19) . . ?
C28 C23 P1 120.51(19) . . ?
C25 C24 C23 119.3(2) . . ?
C26 C25 C24 120.5(3) . . ?
C25 C26 C27 120.2(3) . . ?
C28 C27 C26 120.2(3) . . ?
C27 C28 C23 119.8(2) . . ?
C30 C29 C34 119.9(2) . . ?
C30 C29 P1 120.56(19) . . ?
C34 C29 P1 119.47(18) . . ?
C29 C30 C31 119.8(2) . . ?
C32 C31 C30 120.1(2) . . ?
C33 C32 C31 120.3(2) . . ?
C32 C33 C34 120.4(2) . . ?
C33 C34 C29 119.6(2) . . ?
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 N2 1.658(2) . ?
Fe1 N1 1.664(2) . ?
Fe1 C1 1.960(3) . ?
Fe1 S1 2.2805(7) . ?
Fe1 Fe2 2.5907(5) . ?
Fe2 N3 1.653(2) . ?
Fe2 N4 1.660(2) . ?
Fe2 C1 1.976(3) . ?
Fe2 S1 2.2737(7) . ?
S1 C2 1.782(3) . ?
N1 O1 1.186(3) . ?
N2 O2 1.177(3) . ?
N3 O3 1.177(3) . ?
N4 O4 1.180(3) . ?
N5 C9 1.418(5) . ?
N5 C7 1.420(3) . ?
N5 C8 1.521(6) . ?
N5 C10 1.677(9) . ?
C1 O5 1.156(3) . ?
C2 C3 1.385(4) . ?
C2 C7 1.403(3) . ?
C3 C4 1.387(4) . ?
C4 C5 1.376(4) . ?
C5 C6 1.374(4) . ?
C6 C7 1.395(4) . ?
P1 C17 1.787(2) . ?
P1 C23 1.792(2) . ?
P1 C29 1.799(2) . ?
P1 C11 1.800(2) . ?
C11 C16 1.390(4) . ?
C11 C12 1.391(4) . ?
C12 C13 1.384(4) . ?
C13 C14 1.370(5) . ?
C14 C15 1.369(5) . ?
C15 C16 1.404(4) . ?
C17 C22 1.385(3) . ?
C17 C18 1.391(3) . ?
C18 C19 1.389(4) . ?
C19 C20 1.374(4) . ?
C20 C21 1.380(4) . ?
C21 C22 1.388(4) . ?
C23 C24 1.393(3) . ?
C23 C28 1.396(3) . ?
C24 C25 1.387(4) . ?
C25 C26 1.377(4) . ?
C26 C27 1.384(4) . ?
C27 C28 1.379(4) . ?
C29 C30 1.387(3) . ?
C29 C34 1.399(3) . ?
C30 C31 1.388(4) . ?
C31 C32 1.381(4) . ?
C32 C33 1.379(4) . ?
C33 C34 1.381(4) . ?
