# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2015

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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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data_CompoundI

_vrf_PLAT041_ALERT_1_C           
;
PROBLEM: 
PLAT041_ALERT_1_C Calc. and Reported SumFormula Strings  Differ 
Please Check
FORMU01_ALERT_1_G  There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum:   C4 H16.86 Fe2 N12 O8.43 S5
Atom count from _chemical_formula_moiety:
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
_chemical_formula_sum and the formula from the _atom_site* data.
Atom count from _chemical_formula_sum:C4 H16.86 Fe2 N12 O8.43 S5'
Atom count from the _atom_site data:  C4 H16 Fe2 N12 O8.43 S5'
CELLZ01_ALERT_1_G Difference between formula and atom_site contents 
detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. 
Is this intentional?
From the CIF: _cell_formula_units_Z    8'
From the CIF: _chemical_formula_sum  C4 H16.86 Fe2 N12 O8.43 S5'
PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ 
Please Check
PLAT311_ALERT_2_G Isolated Disordered Oxygen Atom (No H's ?) Ow1 Check

RESPONSE:  Ow1 atom is oxygen atoms of disordered solvent 
water molecule in which hydrogen atoms were not localized but included 
into chemical formula of the compound.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C2 H8 Fe N6 O2 S2), O4 S, 0.43(O1 H2)'
_chemical_formula_sum            'C4 H16.86 Fe2 N12 O8.43 S5'
_chemical_formula_weight         639.15

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'

loop_
_symmetry_equiv_pos_as_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'

_cell_length_a                   12.6104(2)
_cell_length_b                   10.35013(19)
_cell_length_c                   37.1231(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4845.27(16)
_cell_formula_units_Z            8
_cell_measurement_temperature    100.01(10)
_cell_measurement_reflns_used    18675
_cell_measurement_theta_min      2.9422
_cell_measurement_theta_max      37.4190

_exptl_crystal_description       prizm
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2587.5
_exptl_absorpt_coefficient_mu    1.685
_exptl_absorpt_correction_T_min  0.89325
_exptl_absorpt_correction_T_max  1.00000
_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.
;

_diffrn_ambient_temperature      100.01(10)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector_area_resol_mean 16.2060
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            77356
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         34.00
_reflns_number_total             9877
_reflns_number_gt                8318
_reflns_threshold_expression     >2sigma(I)

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL (Sheldrick, 2000)'


_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0155P)²+8.5604P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9877
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0583
_refine_ls_wR_factor_ref         0.0945
_refine_ls_wR_factor_gt          0.0908
_refine_ls_goodness_of_fit_ref   1.245
_refine_ls_restrained_S_all      1.245
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.15275(3) -0.04585(3) 0.213522(9) 0.01352(7) Uani 1 1 d . . .
N1 N 0.09411(17) -0.1752(2) 0.23250(6) 0.0216(4) Uani 1 1 d . . .
O1 O 0.03865(18) -0.2528(2) 0.24518(8) 0.0449(7) Uani 1 1 d . . .
N2 N 0.07562(17) 0.0556(2) 0.18905(6) 0.0185(4) Uani 1 1 d . . .
O2 O 0.00593(16) 0.1185(2) 0.17795(6) 0.0294(4) Uani 1 1 d . . .
S1 S 0.30635(5) -0.12937(5) 0.187867(17) 0.01669(11) Uani 1 1 d . . .
C1 C 0.37632(19) 0.0054(2) 0.17307(6) 0.0153(4) Uani 1 1 d . . .
N3 N 0.4786(2) 0.0095(3) 0.17825(9) 0.0504(9) Uani 1 1 d . . .
H3A H 0.5146 0.0746 0.1706 0.060 Uiso 1 1 calc R . .
H3B H 0.5099 -0.0528 0.1893 0.060 Uiso 1 1 calc R . .
N4 N 0.33165(19) 0.1012(2) 0.15630(8) 0.0330(6) Uani 1 1 d . . .
H4A H 0.3694 0.1652 0.1489 0.040 Uiso 1 1 calc R . .
H4B H 0.2643 0.1006 0.1526 0.040 Uiso 1 1 calc R . .
S2 S 0.19903(5) 0.09829(5) 0.257629(16) 0.01729(11) Uani 1 1 d . . .
C2 C 0.26929(18) 0.0136(2) 0.29022(6) 0.0136(4) Uani 1 1 d . . .
N5 N 0.32856(17) -0.08764(19) 0.28221(6) 0.0181(4) Uani 1 1 d . . .
H5A H 0.3640 -0.1262 0.2988 0.022 Uiso 1 1 calc R . .
H5B H 0.3317 -0.1150 0.2604 0.022 Uiso 1 1 calc R . .
N6 N 0.26452(17) 0.0555(2) 0.32378(5) 0.0190(4) Uani 1 1 d . . .
H6A H 0.3000 0.0168 0.3404 0.023 Uiso 1 1 calc R . .
H6B H 0.2260 0.1213 0.3290 0.023 Uiso 1 1 calc R . .
Fe2 Fe 0.35925(3) 0.11397(3) 0.036661(9) 0.01521(7) Uani 1 1 d . . .
N7 N 0.42643(18) 0.0252(2) 0.06726(6) 0.0212(4) Uani 1 1 d . . .
O3 O 0.48568(18) -0.0285(2) 0.08621(6) 0.0341(5) Uani 1 1 d . . .
N8 N 0.41701(19) 0.2432(2) 0.01703(7) 0.0279(5) Uani 1 1 d . . .
O4 O 0.4667(2) 0.3279(3) 0.00531(9) 0.0580(8) Uani 1 1 d . . .
S3 S 0.32409(5) -0.04110(6) -0.006069(16) 0.01829(11) Uani 1 1 d . . .
C3 C 0.2537(2) 0.0362(2) -0.03998(6) 0.0174(4) Uani 1 1 d . . .
N9 N 0.19493(19) 0.1395(2) -0.03370(6) 0.0243(5) Uani 1 1 d . . .
H9A H 0.1597 0.1746 -0.0510 0.029 Uiso 1 1 calc R . .
H9B H 0.1919 0.1716 -0.0124 0.029 Uiso 1 1 calc R . .
N10 N 0.2573(2) -0.0115(2) -0.07283(6) 0.0240(5) Uani 1 1 d . . .
H10B H 0.2217 0.0245 -0.0899 0.029 Uiso 1 1 calc R . .
H10A H 0.2952 -0.0787 -0.0773 0.029 Uiso 1 1 calc R . .
S4 S 0.20372(5) 0.20635(5) 0.058124(16) 0.01565(11) Uani 1 1 d . . .
C4 C 0.13069(18) 0.0899(2) 0.08062(6) 0.0139(4) Uani 1 1 d . . .
N11 N 0.0385(2) 0.1234(2) 0.09410(8) 0.0347(6) Uani 1 1 d . . .
H11A H 0.0011 0.0677 0.1057 0.042 Uiso 1 1 calc R . .
H11B H 0.0155 0.2009 0.0913 0.042 Uiso 1 1 calc R . .
N12 N 0.16409(19) -0.0287(2) 0.08519(7) 0.0273(5) Uani 1 1 d . . .
H12B H 0.1258 -0.0832 0.0969 0.033 Uiso 1 1 calc R . .
H12A H 0.2243 -0.0521 0.0765 0.033 Uiso 1 1 calc R . .
S5 S 0.57070(4) 0.29688(5) 0.125507(14) 0.01120(9) Uani 1 1 d . . .
O8 O 0.59828(14) 0.24165(16) 0.16101(5) 0.0177(3) Uani 1 1 d . . .
O7 O 0.59936(13) 0.43621(15) 0.12485(4) 0.0140(3) Uani 1 1 d . . .
O5 O 0.45615(14) 0.28326(17) 0.11964(5) 0.0214(4) Uani 1 1 d . . .
O6 O 0.63027(19) 0.23091(18) 0.09722(6) 0.0325(5) Uani 1 1 d . . .
OW1 O 0.6361(5) -0.2096(6) 0.1196(2) 0.0549(18) Uani 0.43 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.01182(14) 0.01440(14) 0.01434(14) -0.00044(11) -0.00025(12) -0.00269(11)
N1 0.0156(10) 0.0220(10) 0.0272(11) 0.0042(8) -0.0008(8) -0.0035(8)
O1 0.0235(11) 0.0431(13) 0.0681(18) 0.0299(12) 0.0000(11) -0.0129(10)
N2 0.0174(9) 0.0212(9) 0.0169(9) -0.0001(7) -0.0051(7) -0.0044(8)
O2 0.0237(10) 0.0314(10) 0.0332(11) 0.0061(9) -0.0145(8) -0.0008(8)
S1 0.0178(3) 0.0108(2) 0.0214(3) -0.00058(19) 0.0052(2) -0.00193(19)
C1 0.0179(11) 0.0145(9) 0.0135(10) -0.0011(7) 0.0008(8) -0.0028(8)
N3 0.0230(13) 0.0516(17) 0.077(2) 0.0462(17) -0.0183(14) -0.0166(12)
N4 0.0180(11) 0.0270(12) 0.0540(17) 0.0234(11) 0.0076(11) 0.0003(9)
S2 0.0213(3) 0.0138(2) 0.0168(3) -0.00329(19) -0.0057(2) 0.0058(2)
C2 0.0110(9) 0.0122(9) 0.0175(10) -0.0021(7) -0.0015(8) 0.0008(7)
N5 0.0203(10) 0.0152(8) 0.0188(9) -0.0028(7) -0.0042(8) 0.0068(7)
N6 0.0198(10) 0.0210(9) 0.0163(9) -0.0023(7) -0.0038(8) 0.0082(8)
Fe2 0.01205(14) 0.01740(15) 0.01617(15) 0.00018(12) 0.00091(12) -0.00218(12)
N7 0.0184(10) 0.0241(10) 0.0211(10) -0.0026(8) -0.0027(8) -0.0022(8)
O3 0.0286(11) 0.0404(12) 0.0334(11) 0.0032(10) -0.0154(9) 0.0028(10)
N8 0.0176(11) 0.0283(11) 0.0377(14) 0.0070(10) 0.0050(10) -0.0047(9)
O4 0.0299(13) 0.0489(15) 0.095(2) 0.0325(15) 0.0111(14) -0.0153(11)
S3 0.0231(3) 0.0172(2) 0.0146(2) -0.0007(2) -0.0040(2) 0.0074(2)
C3 0.0195(11) 0.0179(10) 0.0149(10) -0.0003(8) -0.0019(9) 0.0051(8)
N9 0.0333(12) 0.0247(10) 0.0149(10) -0.0023(8) -0.0044(9) 0.0150(9)
N10 0.0324(12) 0.0260(11) 0.0137(9) -0.0030(8) -0.0064(9) 0.0169(9)
S4 0.0171(3) 0.0115(2) 0.0184(3) 0.00114(19) 0.0052(2) -0.00171(19)
C4 0.0144(10) 0.0143(9) 0.0130(9) 0.0005(7) 0.0007(8) -0.0022(8)
N11 0.0302(13) 0.0202(10) 0.0537(17) 0.0101(11) 0.0284(12) 0.0053(10)
N12 0.0201(11) 0.0151(9) 0.0467(15) 0.0100(9) 0.0144(10) 0.0014(8)
S5 0.0114(2) 0.0112(2) 0.0110(2) 0.00073(17) 0.00099(18) 0.00026(18)
O8 0.0177(8) 0.0175(7) 0.0178(8) 0.0061(6) -0.0059(7) -0.0013(6)
O7 0.0139(7) 0.0116(7) 0.0166(7) 0.0005(6) -0.0017(6) -0.0017(6)
O5 0.0168(8) 0.0195(8) 0.0279(10) 0.0109(7) -0.0096(7) -0.0052(7)
O6 0.0528(14) 0.0177(8) 0.0270(10) -0.0004(7) 0.0248(10) 0.0072(9)
OW1 0.033(3) 0.048(4) 0.083(5) 0.014(3) -0.008(3) -0.015(3)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 1.684(2) . ?
Fe1 N2 1.695(2) . ?
Fe1 S2 2.2907(7) . ?
Fe1 S1 2.3250(7) . ?
N1 O1 1.165(3) . ?
N2 O2 1.169(3) . ?
S1 C1 1.739(2) . ?
C1 N4 1.299(3) . ?
C1 N3 1.304(3) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
S2 C2 1.737(2) . ?
C2 N6 1.320(3) . ?
C2 N5 1.321(3) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
N6 H6A 0.8600 . ?
N6 H6B 0.8600 . ?
Fe2 N8 1.688(2) . ?
Fe2 N7 1.689(2) . ?
Fe2 S3 2.2997(7) . ?
Fe2 S4 2.3228(7) . ?
N7 O3 1.168(3) . ?
N8 O4 1.162(3) . ?
S3 C3 1.736(2) . ?
C3 N10 1.317(3) . ?
C3 N9 1.321(3) . ?
N9 H9A 0.8600 . ?
N9 H9B 0.8600 . ?
N10 H10B 0.8600 . ?
N10 H10A 0.8600 . ?
S4 C4 1.732(2) . ?
C4 N12 1.309(3) . ?
C4 N11 1.312(3) . ?
N11 H11A 0.8600 . ?
N11 H11B 0.8600 . ?
N12 H12B 0.8600 . ?
N12 H12A 0.8600 . ?
S5 O6 1.4606(19) . ?
S5 O5 1.4676(18) . ?
S5 O8 1.4782(17) . ?
S5 O7 1.4869(16) . ?

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 117.68(10) . . ?
N1 Fe1 S2 109.30(8) . . ?
N2 Fe1 S2 97.24(7) . . ?
N1 Fe1 S1 103.98(8) . . ?
N2 Fe1 S1 119.26(8) . . ?
S2 Fe1 S1 108.83(3) . . ?
O1 N1 Fe1 168.9(2) . . ?
O2 N2 Fe1 164.9(2) . . ?
C1 S1 Fe1 104.71(8) . . ?
N4 C1 N3 118.3(2) . . ?
N4 C1 S1 122.9(2) . . ?
N3 C1 S1 118.8(2) . . ?
C1 N3 H3A 120.0 . . ?
C1 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C1 N4 H4A 120.0 . . ?
C1 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
C2 S2 Fe1 107.40(8) . . ?
N6 C2 N5 119.9(2) . . ?
N6 C2 S2 117.92(17) . . ?
N5 C2 S2 122.16(18) . . ?
C2 N5 H5A 120.0 . . ?
C2 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C2 N6 H6A 120.0 . . ?
C2 N6 H6B 120.0 . . ?
H6A N6 H6B 120.0 . . ?
N8 Fe2 N7 120.31(12) . . ?
N8 Fe2 S3 109.77(10) . . ?
N7 Fe2 S3 100.44(8) . . ?
N8 Fe2 S4 100.74(9) . . ?
N7 Fe2 S4 114.63(8) . . ?
S3 Fe2 S4 111.17(3) . . ?
O3 N7 Fe2 170.3(2) . . ?
O4 N8 Fe2 172.7(3) . . ?
C3 S3 Fe2 106.09(8) . . ?
N10 C3 N9 119.1(2) . . ?
N10 C3 S3 118.76(18) . . ?
N9 C3 S3 122.12(18) . . ?
C3 N9 H9A 120.0 . . ?
C3 N9 H9B 120.0 . . ?
H9A N9 H9B 120.0 . . ?
C3 N10 H10B 120.0 . . ?
C3 N10 H10A 120.0 . . ?
H10B N10 H10A 120.0 . . ?
C4 S4 Fe2 109.15(8) . . ?
N12 C4 N11 118.9(2) . . ?
N12 C4 S4 122.97(19) . . ?
N11 C4 S4 118.12(18) . . ?
C4 N11 H11A 120.0 . . ?
C4 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C4 N12 H12B 120.0 . . ?
C4 N12 H12A 120.0 . . ?
H12B N12 H12A 120.0 . . ?
O6 S5 O5 110.76(13) . . ?
O6 S5 O8 109.84(12) . . ?
O5 S5 O8 109.08(10) . . ?
O6 S5 O7 108.46(11) . . ?
O5 S5 O7 109.26(10) . . ?
O8 S5 O7 109.42(10) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        34.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.110
_database_code_depnum_ccdc_archive 'CCDC 1001729'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_CompoundII

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H16 Fe4 N16 O14 S8'
_chemical_formula_weight         992.21

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.2712(3)
_cell_length_b                   10.4132(5)
_cell_length_c                   12.1912(5)
_cell_angle_alpha                86.462(4)
_cell_angle_beta                 88.363(4)
_cell_angle_gamma                87.613(4)
_cell_volume                     793.65(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    99.9(2)
_cell_measurement_reflns_used    4289
_cell_measurement_theta_min      3.2458
_cell_measurement_theta_max      37.2837

_exptl_crystal_description       prizm
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             496
_exptl_absorpt_coefficient_mu    2.399
_exptl_absorpt_correction_T_min  0.97873
_exptl_absorpt_correction_T_max  1.00000
_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.
;

_diffrn_ambient_temperature      99.9(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13522
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.25
_diffrn_reflns_theta_max         36.09
_reflns_number_total             7581
_reflns_number_gt                5810
_reflns_threshold_expression     >2sigma(I)

_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_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_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL (Sheldrick, 2000)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0268P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7581
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.0915
_refine_ls_wR_factor_gt          0.0787
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.09609(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_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.00985(12) 0.01254(14) 0.00955(12) 0.00014(10) 0.00049(9) 0.00003(9)
Fe2 0.01201(12) 0.01360(15) 0.00949(12) 0.00012(10) -0.00136(9) -0.00206(9)
S1 0.00932(18) 0.0117(2) 0.0123(2) -0.00049(17) -0.00116(14) 0.00021(14)
S2 0.00978(18) 0.0119(2) 0.00937(19) 0.00068(16) 0.00012(14) -0.00014(15)
S3 0.0123(2) 0.0157(2) 0.0099(2) -0.00060(17) -0.00135(15) 0.00141(16)
S4 0.0134(2) 0.0172(3) 0.0105(2) 0.00047(18) -0.00036(15) 0.00135(16)
N1 0.0118(7) 0.0141(8) 0.0117(7) -0.0015(6) -0.0002(5) -0.0001(6)
N2 0.0135(7) 0.0193(10) 0.0130(8) 0.0003(7) 0.0007(6) -0.0010(6)
N3 0.0154(7) 0.0202(10) 0.0146(8) 0.0019(7) -0.0034(6) -0.0033(6)
N4 0.0167(7) 0.0146(9) 0.0127(8) -0.0007(6) -0.0016(6) -0.0008(6)
N5 0.0110(7) 0.0190(9) 0.0133(8) 0.0017(6) -0.0004(5) -0.0015(6)
N6 0.0115(7) 0.0304(11) 0.0116(8) 0.0035(7) -0.0009(6) -0.0034(6)
N7 0.0124(7) 0.0214(10) 0.0107(7) 0.0021(6) 0.0001(5) 0.0008(6)
N8 0.0147(7) 0.0176(9) 0.0118(7) 0.0009(6) 0.0010(6) 0.0006(6)
O1 0.0118(6) 0.0250(9) 0.0211(8) -0.0033(7) 0.0018(5) 0.0006(6)
O2 0.0298(9) 0.0437(13) 0.0136(8) 0.0073(8) -0.0075(6) -0.0020(8)
O3 0.0196(7) 0.0355(12) 0.0281(9) 0.0035(8) -0.0066(6) -0.0135(7)
O4 0.0276(8) 0.0189(9) 0.0234(8) 0.0045(7) -0.0082(6) 0.0002(6)
O5 0.0140(6) 0.0182(8) 0.0121(6) 0.0033(6) 0.0023(5) 0.0013(5)
O6 0.0105(6) 0.0172(8) 0.0176(7) 0.0021(6) -0.0023(5) -0.0024(5)
O7 0.0159(6) 0.0144(8) 0.0130(7) -0.0027(5) -0.0009(5) 0.0024(5)
C1 0.0129(8) 0.0132(9) 0.0104(8) -0.0020(7) -0.0012(6) -0.0002(6)
C2 0.0159(8) 0.0111(9) 0.0102(8) -0.0016(7) -0.0008(6) -0.0004(6)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 1.6751(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) . ?

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 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) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        36.09
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.708
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.146
_database_code_depnum_ccdc_archive 'CCDC 1001730'
