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Acta Cryst. (2007). E63, m1996    [ doi:10.1107/S160053680702524X ]

Bis([mu]-9-anthrylmethylthiolato)bis[tricarbonyliron(I)](Fe-Fe)

S. Gao and X.-J. Peng

Abstract top

The title compound, [Fe2(C15H11S)2(CO)6], has been prepared as a structural model for the iron hydrogenase active site. The asymmetric unit consists of two molecules. The Fe2S2 units in both molecules exhibit a butterfly conformation.

Comment top

Since the crystal structure of iron hydrogenases ([Fe]H2ases) was solved (Peters et al., 1998), the classical organometallic diiron dithiolate complexes again became hot research topics for chemists alover due to their structural resemblance of the active site of the [Fe]H2ases (H-Cluster). Title compound (I) was prepared with the ambitious aim of helping to solve the mystery of the chemical reactivity of the H-Cluster. Here we report the crystal structure of (I).

There are two molecules in the asymmetric unit, with essentially identical geometries. Including the Fe—Fe bond each Fe atom is hexacoordinated and exhibits a heavily distorted octahedral geometry. The bond lengths (Fe—Fe, Fe—S and Fe—C) and angles (C—Fe—Fe and Fe—S—Fe) in each molecule are indistinguishable from those in the other and are within the expected range (Lyon et al., 1999, Li et al., 2002, Ott et al., 2003). The C atoms of the anthracene rings in each molecule are almost coplanar, the planes formed have r.m.s. deviations from the mean plane of only 0.038 Å for A (C8–C21), 0.030 Å for B (C23–C36), 0.022 Å for C (C44–C57), and 0.057 Å for D (C59–C72), respectively. The dihedral angles between the anthracene planes in each molecule are 59.449° for A/B and 78.175° for C/D.

Selected bond distances and angles are summarized in Table 1, ORTEP representations of both crystallographically independent molecules are depicted in Figures 1 and 2.

Related literature top

For related literature, see: Lan et al. (2003); Li & Rauchfuss (2002); Lyon et al. (1999); Ott et al. (2003); Peters et al. (1998).

Experimental top

The starting compound 9-bromomethylanthracene was prepared from 9-hydroxymethylanthracene according to the literature procedure (Lan et al., 2003). Super hydride (LiEt3BH, 1 M solution in THF, 3 ml, 3 mmol) was added to a degassed solution of [(µ-S2)Fe2(CO)6] (516 mg, 1.5 mmol) in dry THF (35 ml) at −78 °C over 30 min. 9-Bromomethylanthracene (813 mg, 3 mmol) was added to the dark emerald green solution, causing an immediate change in color to red. The reaction mixture was allowed to warm to room temperature and stirred for an additional hour. The solvent was removed on a rotary evaporator. The crude product was purified by column chromatography with silica using CH2Cl2/hexanes (1:10) as the eluent to give compound (I) as a red solid (893 mg, 82%). A single-crystal of (I) was obtained by slow evaporation of the dichloromethane/hexane (5:1, v/v) solution at room temperature.

Refinement top

One of the anthracene moieties (C59 to C71) shows large anistropic displacement parameters due to pronounced thermal motion (back and forth rocking of the anthracene around the S3—C58 bond). Restraining the anisotropic displacement parameters of atoms closer than 1.7 Å to each other to have similar Uij components did not significantely improve the quality of the model and was thus omitted in the final refinement cycles. The H atoms attached to C were placed in geometrically calculated positions (C—H = 0.93–0.97 Å) and refined as riding, with Uiso(H) = 1.2Ueq(C).

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SMART (Bruker, 1997); data reduction: SAINT-Plus (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The molecular structure of the first molecule in the asymmetric unit of (I), with displacement ellipsoids drawn at 30% probability level.
[Figure 2] Fig. 2. The molecular structure of the second molecule in the asymmetric unit of (I), with displacement ellipsoids drawn at 30% probability level.
Bis(µ-9-anthrylmethylthiolato)bis[tricarbonyliron(I)](Fe—Fe) top
Crystal data top
[Fe2(C30H22S2)(CO)6]Z = 4
Mr = 726.36F000 = 1480
Triclinic, P1Dx = 1.490 Mg m−3
Hall symbol: -P 1Mo Kα radiation
λ = 0.71073 Å
a = 11.471 (4) ÅCell parameters from 3698 reflections
b = 16.990 (6) Åθ = 2.3–22.7º
c = 17.698 (6) ŵ = 1.07 mm−1
α = 70.218 (4)ºT = 273 (2) K
β = 88.973 (4)ºBlock, red
γ = 86.239 (5)º0.45 × 0.29 × 0.10 mm
V = 3239 (2) Å3
Data collection top
Bruker APEXII CCD area-detector
diffractometer		11208 independent reflections
Radiation source: fine-focus sealed tube7705 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.024
T = 273(2) Kθmax = 25.0º
φ and ω scansθmin = 1.8º
Absorption correction: multi-scan
(SADABS; Bruker, 1997)		h = −13→13
Tmin = 0.645, Tmax = 0.904k = −12→20
16289 measured reflectionsl = −20→21
Refinement top
Refinement on F2H-atom parameters constrained
Least-squares matrix: full  w = 1/[σ2(Fo2) + (0.0432P)2]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.045(Δ/σ)max = 0.001
wR(F2) = 0.102Δρmax = 0.34 e Å−3
S = 1.01Δρmin = −0.27 e Å−3
11208 reflectionsExtinction correction: none
829 parameters
Crystal data top
[Fe2(C30H22S2)(CO)6]γ = 86.239 (5)º
Mr = 726.36V = 3239 (2) Å3
Triclinic, P1Z = 4
a = 11.471 (4) ÅMo Kα
b = 16.990 (6) ŵ = 1.07 mm−1
c = 17.698 (6) ÅT = 273 (2) K
α = 70.218 (4)º0.45 × 0.29 × 0.10 mm
β = 88.973 (4)º
Data collection top
Bruker APEXII CCD area-detector
diffractometer		11208 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 1997)		7705 reflections with I > 2σ(I)
Tmin = 0.645, Tmax = 0.904Rint = 0.024
16289 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.045829 parameters
wR(F2) = 0.102H-atom parameters constrained
S = 1.01Δρmax = 0.34 e Å−3
11208 reflectionsΔρmin = −0.27 e Å−3
Special details top

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

Refinement. 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 > σ(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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.56624 (4)0.30124 (3)0.08483 (3)0.04097 (14)
Fe20.71838 (4)0.18116 (3)0.12968 (3)0.04349 (14)
Fe30.44492 (4)0.86636 (3)0.44222 (3)0.04723 (15)
Fe40.37153 (4)0.73358 (3)0.53846 (3)0.04643 (15)
S10.56929 (7)0.18750 (6)0.04441 (5)0.0410 (2)
S20.74699 (7)0.30516 (5)0.03247 (5)0.0403 (2)
S30.30760 (8)0.79305 (6)0.41106 (5)0.0460 (2)
S40.31290 (7)0.86388 (6)0.53965 (5)0.0462 (2)
C10.4843 (3)0.3829 (2)0.0091 (2)0.0516 (9)
C20.4504 (3)0.2546 (3)0.1509 (2)0.0532 (10)
C30.6040 (3)0.3621 (2)0.1453 (2)0.0500 (9)
C40.6514 (3)0.0976 (3)0.2038 (2)0.0655 (12)
C50.7848 (3)0.2103 (3)0.2062 (2)0.0554 (10)
C60.8363 (3)0.1186 (2)0.1049 (2)0.0500 (9)
C70.8453 (3)0.3749 (2)0.0567 (2)0.0482 (9)
H7A0.80240.42660.05510.058*
H7B0.87750.34800.11030.058*
C80.9419 (3)0.3934 (2)−0.0040 (2)0.0434 (8)
C91.0409 (3)0.3361 (2)0.0082 (2)0.0459 (9)
C101.0527 (3)0.2596 (3)0.0741 (2)0.0570 (10)
H10A0.99370.24690.11220.068*
C111.1469 (3)0.2045 (3)0.0833 (3)0.0733 (13)
H11A1.15130.15490.12700.088*
C121.2373 (4)0.2223 (3)0.0271 (3)0.0802 (14)
H12A1.30050.18350.03280.096*
C131.2341 (3)0.2946 (3)−0.0350 (3)0.0713 (13)
H13A1.29650.3064−0.07040.086*
C141.1358 (3)0.3534 (3)−0.0471 (2)0.0547 (10)
C151.1282 (4)0.4271 (3)−0.1120 (2)0.0666 (12)
H15A1.19090.4396−0.14720.080*
C161.0316 (4)0.4830 (3)−0.1266 (2)0.0631 (12)
C171.0251 (5)0.5572 (3)−0.1945 (3)0.0905 (16)
H17A1.08780.5692−0.22970.109*
C180.9300 (7)0.6107 (4)−0.2091 (3)0.112 (2)
H18A0.92830.6595−0.25370.134*
C190.8336 (6)0.5938 (3)−0.1581 (4)0.1052 (19)
H19A0.76800.6311−0.16960.126*
C200.8342 (4)0.5229 (3)−0.0913 (3)0.0755 (13)
H20A0.76900.5124−0.05820.091*
C210.9339 (3)0.4653 (2)−0.0721 (2)0.0534 (10)
C220.6230 (3)0.2023 (2)−0.05877 (18)0.0437 (8)
H22A0.68810.2381−0.06990.052*
H22B0.65130.1484−0.06180.052*
C230.5296 (3)0.2407 (2)−0.12195 (19)0.0427 (8)
C240.5369 (3)0.3243 (2)−0.1743 (2)0.0513 (10)
C250.6283 (4)0.3762 (3)−0.1727 (2)0.0687 (12)
H25A0.68650.3557−0.13380.082*
C260.6331 (5)0.4550 (3)−0.2265 (3)0.0916 (16)
H26A0.69460.4872−0.22430.110*
C270.5455 (6)0.4879 (3)−0.2854 (3)0.1047 (19)
H27A0.54940.5420−0.32180.126*
C280.4570 (5)0.4427 (3)−0.2896 (3)0.0902 (16)
H28A0.40000.4658−0.32900.108*
C290.4474 (4)0.3593 (3)−0.2350 (2)0.0618 (11)
C300.3580 (4)0.3110 (3)−0.2407 (2)0.0667 (12)
H30A0.30060.3345−0.27970.080*
C310.3504 (3)0.2281 (3)−0.1904 (2)0.0535 (10)
C320.2575 (3)0.1790 (3)−0.1969 (3)0.0699 (12)
H32A0.19980.2027−0.23560.084*
C330.2518 (4)0.0997 (3)−0.1485 (3)0.0803 (14)
H33A0.18970.0690−0.15300.096*
C340.3397 (4)0.0625 (3)−0.0907 (3)0.0731 (12)
H34A0.33640.0067−0.05830.088*
C350.4287 (3)0.1067 (2)−0.0818 (2)0.0567 (10)
H35A0.48510.0806−0.04270.068*
C360.4394 (3)0.1921 (2)−0.1301 (2)0.0459 (9)
C370.4056 (4)0.9648 (3)0.3649 (3)0.0666 (12)
C380.5612 (4)0.8249 (3)0.3958 (2)0.0640 (11)
C390.5495 (3)0.8992 (2)0.4969 (3)0.0607 (11)
C400.4635 (4)0.6573 (3)0.5143 (2)0.0688 (12)
C410.4593 (3)0.7249 (3)0.6237 (2)0.0597 (11)
C420.2565 (4)0.6679 (3)0.5887 (2)0.0681 (12)
C430.1693 (3)0.9094 (2)0.4939 (2)0.0505 (9)
H43A0.17220.96970.47060.061*
H43B0.15390.88820.45080.061*
C440.0708 (3)0.8894 (2)0.5531 (2)0.0483 (9)
C450.0546 (3)0.9341 (3)0.6074 (2)0.0530 (10)
C460.1298 (4)0.9949 (3)0.6119 (2)0.0630 (11)
H46A0.19541.00490.57920.076*
C470.1097 (4)1.0394 (3)0.6627 (3)0.0837 (15)
H47A0.16171.07860.66420.100*
C480.0123 (5)1.0268 (4)0.7123 (3)0.0991 (19)
H48A−0.00171.05850.74570.119*
C49−0.0619 (4)0.9686 (4)0.7121 (3)0.0848 (17)
H49A−0.12590.95990.74630.102*
C50−0.0444 (4)0.9199 (3)0.6604 (2)0.0681 (13)
C51−0.1196 (4)0.8617 (4)0.6573 (3)0.0841 (17)
H51A−0.18280.85200.69220.101*
C52−0.1074 (3)0.8164 (3)0.6056 (3)0.0733 (14)
C53−0.1882 (5)0.7581 (4)0.6017 (4)0.109 (2)
H53A−0.25290.74950.63520.131*
C54−0.1737 (5)0.7150 (4)0.5507 (5)0.126 (3)
H54A−0.22780.67670.55050.151*
C55−0.0771 (5)0.7267 (3)0.4970 (4)0.111 (2)
H55A−0.06840.69680.46170.133*
C560.0019 (4)0.7823 (3)0.4984 (3)0.0812 (14)
H56A0.06490.79000.46340.097*
C57−0.0082 (3)0.8298 (3)0.5521 (2)0.0595 (11)
C580.3526 (3)0.7409 (2)0.3382 (2)0.0553 (10)
H58A0.41220.77140.30270.066*
H58B0.38420.68420.36600.066*
C590.2460 (3)0.7397 (3)0.2910 (2)0.0621 (11)
C600.1765 (4)0.6703 (4)0.3161 (3)0.0821 (14)
C610.1979 (5)0.6009 (4)0.3877 (4)0.1090 (19)
H61A0.26090.60090.42010.131*
C620.1293 (8)0.5344 (5)0.4107 (5)0.165 (3)
H62A0.14600.48960.45760.199*
C630.0338 (11)0.5341 (8)0.3630 (8)0.208 (6)
H63A−0.01330.48880.37950.250*
C640.0079 (9)0.5959 (8)0.2951 (7)0.178 (5)
H64A−0.05500.59260.26410.214*
C650.0768 (5)0.6684 (6)0.2689 (5)0.119 (2)
C660.0527 (5)0.7352 (7)0.2007 (5)0.139 (4)
H66A−0.00880.73230.16840.167*
C670.1138 (5)0.8065 (5)0.1768 (3)0.109 (2)
C680.0829 (8)0.8789 (7)0.1093 (5)0.168 (5)
H68A0.01930.87740.07810.201*
C690.1395 (9)0.9478 (7)0.0887 (5)0.171 (6)
H69A0.11600.99330.04390.205*
C700.2379 (6)0.9524 (4)0.1357 (3)0.129 (3)
H70A0.27731.00140.12200.155*
C710.2737 (5)0.8844 (4)0.2008 (3)0.0930 (18)
H71A0.33870.88740.23020.112*
C720.2140 (4)0.8105 (4)0.2239 (3)0.0746 (14)
O10.4307 (3)0.43621 (19)−0.03723 (18)0.0804 (9)
O20.3786 (2)0.2228 (2)0.19443 (17)0.0766 (9)
O30.6322 (3)0.39878 (19)0.18440 (17)0.0751 (8)
O40.6111 (3)0.0426 (2)0.2508 (2)0.1122 (13)
O50.8250 (3)0.23076 (19)0.25447 (17)0.0798 (9)
O60.9113 (2)0.07995 (19)0.08964 (17)0.0758 (9)
O70.3758 (3)1.0255 (2)0.3152 (2)0.1025 (12)
O80.6386 (3)0.7966 (2)0.3698 (2)0.1035 (12)
O90.6178 (3)0.9199 (2)0.5311 (2)0.0962 (11)
O100.5247 (3)0.6095 (2)0.4982 (2)0.1114 (13)
O110.5177 (3)0.7201 (2)0.67673 (17)0.0894 (10)
O120.1870 (3)0.6244 (2)0.6217 (2)0.1164 (14)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0363 (3)0.0441 (3)0.0424 (3)0.0005 (2)0.0025 (2)−0.0152 (2)
Fe20.0388 (3)0.0451 (3)0.0420 (3)0.0010 (2)−0.0001 (2)−0.0094 (2)
Fe30.0474 (3)0.0471 (3)0.0470 (3)−0.0075 (3)0.0075 (2)−0.0152 (3)
Fe40.0535 (3)0.0473 (3)0.0363 (3)−0.0061 (3)−0.0004 (2)−0.0107 (2)
S10.0366 (4)0.0424 (5)0.0440 (5)−0.0038 (4)0.0028 (4)−0.0145 (4)
S20.0352 (4)0.0431 (5)0.0434 (5)−0.0047 (4)0.0024 (4)−0.0152 (4)
S30.0519 (5)0.0518 (6)0.0368 (5)−0.0036 (5)−0.0003 (4)−0.0183 (4)
S40.0455 (5)0.0545 (6)0.0423 (5)−0.0027 (5)0.0017 (4)−0.0211 (5)
C10.048 (2)0.047 (2)0.060 (2)0.0003 (19)−0.0002 (19)−0.018 (2)
C20.047 (2)0.066 (3)0.050 (2)0.003 (2)0.0013 (18)−0.025 (2)
C30.048 (2)0.057 (3)0.049 (2)0.0027 (19)0.0053 (18)−0.023 (2)
C40.045 (2)0.073 (3)0.061 (3)0.001 (2)0.0050 (19)−0.001 (2)
C50.058 (2)0.057 (3)0.043 (2)0.002 (2)−0.0007 (19)−0.008 (2)
C60.047 (2)0.043 (2)0.056 (2)−0.0029 (19)−0.0017 (18)−0.0114 (19)
C70.0431 (19)0.051 (2)0.057 (2)−0.0094 (18)0.0038 (17)−0.0249 (19)
C80.0415 (19)0.049 (2)0.048 (2)−0.0111 (18)0.0019 (16)−0.0258 (19)
C90.0408 (19)0.053 (2)0.050 (2)−0.0131 (18)0.0043 (16)−0.023 (2)
C100.039 (2)0.065 (3)0.066 (3)−0.008 (2)0.0034 (18)−0.020 (2)
C110.053 (3)0.072 (3)0.088 (3)−0.001 (2)−0.004 (2)−0.019 (3)
C120.055 (3)0.082 (4)0.113 (4)0.001 (3)0.000 (3)−0.046 (3)
C130.045 (2)0.096 (4)0.094 (4)−0.018 (3)0.020 (2)−0.057 (3)
C140.049 (2)0.069 (3)0.058 (2)−0.021 (2)0.0078 (19)−0.034 (2)
C150.073 (3)0.083 (3)0.054 (3)−0.031 (3)0.018 (2)−0.032 (3)
C160.094 (3)0.053 (3)0.041 (2)−0.035 (3)−0.005 (2)−0.009 (2)
C170.135 (5)0.076 (4)0.063 (3)−0.041 (4)0.001 (3)−0.020 (3)
C180.183 (7)0.070 (4)0.072 (4)−0.035 (5)−0.038 (4)−0.004 (3)
C190.137 (5)0.055 (4)0.121 (5)0.003 (4)−0.052 (4)−0.026 (4)
C200.090 (3)0.051 (3)0.087 (3)−0.002 (3)−0.021 (3)−0.025 (3)
C210.066 (2)0.045 (2)0.055 (2)−0.019 (2)−0.005 (2)−0.021 (2)
C220.0431 (19)0.046 (2)0.046 (2)−0.0005 (17)0.0029 (16)−0.0215 (18)
C230.050 (2)0.040 (2)0.042 (2)0.0026 (18)0.0051 (16)−0.0192 (17)
C240.071 (3)0.048 (2)0.038 (2)0.001 (2)0.0071 (19)−0.0198 (19)
C250.103 (3)0.056 (3)0.049 (2)−0.018 (3)0.000 (2)−0.018 (2)
C260.150 (5)0.063 (3)0.066 (3)−0.039 (3)0.007 (3)−0.022 (3)
C270.185 (6)0.051 (3)0.068 (3)−0.017 (4)−0.012 (4)−0.004 (3)
C280.145 (5)0.055 (3)0.061 (3)0.010 (3)−0.018 (3)−0.008 (3)
C290.085 (3)0.051 (3)0.049 (2)0.012 (2)−0.001 (2)−0.019 (2)
C300.070 (3)0.079 (3)0.053 (2)0.016 (3)−0.013 (2)−0.028 (2)
C310.054 (2)0.062 (3)0.048 (2)0.006 (2)−0.0054 (18)−0.025 (2)
C320.053 (2)0.095 (4)0.065 (3)0.003 (3)−0.013 (2)−0.032 (3)
C330.064 (3)0.095 (4)0.089 (3)−0.025 (3)−0.005 (3)−0.038 (3)
C340.072 (3)0.067 (3)0.082 (3)−0.018 (3)−0.010 (3)−0.024 (3)
C350.055 (2)0.053 (3)0.061 (2)−0.004 (2)−0.0081 (19)−0.019 (2)
C360.043 (2)0.050 (2)0.045 (2)0.0072 (18)−0.0023 (16)−0.0192 (19)
C370.061 (3)0.064 (3)0.070 (3)−0.013 (2)0.018 (2)−0.016 (2)
C380.058 (2)0.080 (3)0.062 (3)−0.010 (2)0.005 (2)−0.033 (2)
C390.052 (2)0.050 (3)0.086 (3)−0.006 (2)0.008 (2)−0.031 (2)
C400.093 (3)0.059 (3)0.049 (2)0.007 (3)−0.010 (2)−0.014 (2)
C410.063 (3)0.061 (3)0.049 (2)−0.008 (2)0.004 (2)−0.010 (2)
C420.074 (3)0.061 (3)0.059 (3)−0.017 (2)−0.003 (2)−0.004 (2)
C430.051 (2)0.054 (2)0.044 (2)0.0002 (19)−0.0009 (17)−0.0127 (18)
C440.041 (2)0.051 (2)0.041 (2)0.0050 (18)−0.0025 (16)−0.0017 (18)
C450.050 (2)0.060 (3)0.035 (2)0.019 (2)−0.0023 (17)−0.0018 (19)
C460.066 (3)0.068 (3)0.053 (2)0.011 (2)0.001 (2)−0.022 (2)
C470.085 (3)0.100 (4)0.075 (3)0.023 (3)−0.011 (3)−0.047 (3)
C480.105 (4)0.126 (5)0.065 (3)0.048 (4)−0.016 (3)−0.041 (4)
C490.075 (3)0.115 (5)0.049 (3)0.043 (3)0.009 (2)−0.016 (3)
C500.052 (2)0.082 (3)0.046 (2)0.021 (3)0.004 (2)0.004 (2)
C510.052 (3)0.094 (4)0.070 (3)0.019 (3)0.014 (2)0.015 (3)
C520.037 (2)0.069 (3)0.085 (3)0.003 (2)−0.004 (2)0.012 (3)
C530.054 (3)0.082 (5)0.150 (6)−0.007 (3)−0.007 (3)0.014 (4)
C540.069 (4)0.077 (5)0.206 (8)−0.022 (4)−0.036 (5)−0.010 (5)
C550.078 (4)0.088 (4)0.163 (6)−0.008 (3)−0.029 (4)−0.037 (4)
C560.056 (3)0.073 (3)0.109 (4)−0.006 (3)−0.019 (3)−0.022 (3)
C570.050 (2)0.052 (3)0.065 (3)0.004 (2)−0.010 (2)−0.004 (2)
C580.065 (2)0.064 (3)0.044 (2)0.008 (2)−0.0052 (18)−0.029 (2)
C590.064 (3)0.090 (3)0.049 (2)0.012 (3)−0.008 (2)−0.047 (2)
C600.083 (3)0.113 (4)0.080 (3)−0.017 (3)0.006 (3)−0.069 (3)
C610.135 (5)0.106 (5)0.107 (5)−0.039 (4)0.017 (4)−0.059 (4)
C620.217 (9)0.125 (6)0.183 (8)−0.079 (6)0.042 (7)−0.080 (6)
C630.204 (11)0.249 (15)0.265 (15)−0.132 (11)0.066 (12)−0.190 (12)
C640.123 (6)0.290 (16)0.219 (11)−0.077 (9)0.029 (8)−0.202 (11)
C650.085 (4)0.207 (8)0.126 (5)−0.029 (5)0.010 (4)−0.132 (6)
C660.070 (4)0.290 (13)0.112 (6)0.022 (6)−0.024 (4)−0.145 (8)
C670.078 (4)0.197 (8)0.068 (4)0.060 (4)−0.018 (3)−0.079 (5)
C680.128 (7)0.300 (14)0.066 (6)0.134 (9)−0.031 (5)−0.075 (7)
C690.189 (11)0.225 (12)0.058 (4)0.150 (9)0.005 (5)−0.024 (6)
C700.190 (7)0.114 (5)0.069 (4)0.077 (5)0.026 (4)−0.029 (4)
C710.126 (5)0.096 (4)0.054 (3)0.045 (4)0.006 (3)−0.032 (3)
C720.074 (3)0.114 (4)0.046 (3)0.035 (3)−0.007 (2)−0.048 (3)
O10.085 (2)0.060 (2)0.083 (2)0.0111 (17)−0.0246 (17)−0.0093 (17)
O20.0613 (17)0.099 (2)0.0689 (19)−0.0230 (18)0.0235 (15)−0.0260 (17)
O30.090 (2)0.082 (2)0.0690 (19)−0.0119 (18)0.0029 (16)−0.0458 (18)
O40.085 (2)0.102 (3)0.103 (3)−0.019 (2)0.017 (2)0.027 (2)
O50.103 (2)0.081 (2)0.0537 (18)−0.0003 (19)−0.0225 (17)−0.0210 (17)
O60.0639 (18)0.077 (2)0.090 (2)0.0180 (17)0.0015 (16)−0.0376 (18)
O70.089 (2)0.076 (3)0.104 (3)0.005 (2)0.018 (2)0.017 (2)
O80.070 (2)0.158 (4)0.109 (3)0.005 (2)0.0222 (19)−0.082 (3)
O90.073 (2)0.085 (2)0.151 (3)−0.0081 (19)−0.025 (2)−0.064 (2)
O100.145 (3)0.092 (3)0.093 (3)0.054 (3)−0.015 (2)−0.037 (2)
O110.091 (2)0.115 (3)0.0603 (19)−0.014 (2)−0.0231 (17)−0.0236 (19)
O120.103 (3)0.110 (3)0.109 (3)−0.058 (2)0.012 (2)0.007 (2)
Geometric parameters (Å, °) top
Fe1—C21.794 (4)C29—C301.381 (6)
Fe1—C11.795 (4)C30—C311.396 (6)
Fe1—C31.796 (4)C30—H30A0.9300
Fe1—S22.2517 (11)C31—C321.424 (5)
Fe1—S12.2745 (12)C31—C361.439 (5)
Fe1—Fe22.5148 (9)C32—C331.335 (6)
Fe2—C41.781 (4)C32—H32A0.9300
Fe2—C51.788 (4)C33—C341.406 (6)
Fe2—C61.805 (4)C33—H33A0.9300
Fe2—S22.2634 (11)C34—C351.349 (5)
Fe2—S12.2743 (11)C34—H34A0.9300
Fe3—C381.783 (4)C35—C361.424 (5)
Fe3—C391.784 (4)C35—H35A0.9300
Fe3—C371.802 (5)C37—O71.142 (5)
Fe3—S32.2560 (12)C38—O81.145 (4)
Fe3—S42.2659 (11)C39—O91.140 (4)
Fe3—Fe42.5092 (9)C40—O101.143 (5)
Fe4—C401.777 (5)C41—O111.140 (4)
Fe4—C411.788 (4)C42—O121.136 (5)
Fe4—C421.804 (4)C43—C441.503 (4)
Fe4—S32.2502 (12)C43—H43A0.9700
Fe4—S42.2780 (13)C43—H43B0.9700
S1—C221.857 (3)C44—C571.406 (5)
S2—C71.843 (3)C44—C451.416 (5)
S3—C581.845 (3)C45—C461.411 (5)
S4—C431.850 (3)C45—C501.440 (5)
C1—O11.145 (4)C46—C471.365 (6)
C2—O21.148 (4)C46—H46A0.9300
C3—O31.140 (4)C47—C481.391 (6)
C4—O41.138 (5)C47—H47A0.9300
C5—O51.141 (4)C48—C491.347 (7)
C6—O61.132 (4)C48—H48A0.9300
C7—C81.502 (4)C49—C501.430 (6)
C7—H7A0.9700C49—H49A0.9300
C7—H7B0.9700C50—C511.370 (6)
C8—C211.395 (5)C51—C521.381 (7)
C8—C91.416 (5)C51—H51A0.9300
C9—C101.422 (5)C52—C531.420 (7)
C9—C141.429 (5)C52—C571.446 (6)
C10—C111.357 (5)C53—C541.341 (8)
C10—H10A0.9300C53—H53A0.9300
C11—C121.400 (6)C54—C551.426 (8)
C11—H11A0.9300C54—H54A0.9300
C12—C131.341 (6)C55—C561.357 (6)
C12—H12A0.9300C55—H55A0.9300
C13—C141.424 (5)C56—C571.439 (6)
C13—H13A0.9300C56—H56A0.9300
C14—C151.382 (5)C58—C591.498 (5)
C15—C161.380 (6)C58—H58A0.9700
C15—H15A0.9300C58—H58B0.9700
C16—C171.416 (6)C59—C601.407 (6)
C16—C211.445 (5)C59—C721.409 (6)
C17—C181.343 (7)C60—C611.420 (7)
C17—H17A0.9300C60—C651.436 (7)
C18—C191.397 (8)C61—C621.362 (8)
C18—H18A0.9300C61—H61A0.9300
C19—C201.373 (6)C62—C631.397 (12)
C19—H19A0.9300C62—H62A0.9300
C20—C211.422 (5)C63—C641.324 (14)
C20—H20A0.9300C63—H63A0.9300
C22—C231.510 (4)C64—C651.445 (12)
C22—H22A0.9700C64—H64A0.9300
C22—H22B0.9700C65—C661.367 (10)
C23—C361.404 (5)C66—C671.375 (10)
C23—C241.416 (5)C66—H66A0.9300
C24—C251.421 (5)C67—C681.425 (10)
C24—C291.446 (5)C67—C721.451 (7)
C25—C261.358 (6)C68—C691.314 (14)
C25—H25A0.9300C68—H68A0.9300
C26—C271.407 (7)C69—C701.436 (12)
C26—H26A0.9300C69—H69A0.9300
C27—C281.331 (7)C70—C711.373 (7)
C27—H27A0.9300C70—H70A0.9300
C28—C291.428 (6)C71—C721.402 (7)
C28—H28A0.9300C71—H71A0.9300
C2—Fe1—C1100.16 (16)C26—C25—C24121.8 (4)
C2—Fe1—C392.67 (17)C26—C25—H25A119.1
C1—Fe1—C397.63 (17)C24—C25—H25A119.1
C2—Fe1—S2155.19 (12)C25—C26—C27120.3 (5)
C1—Fe1—S2103.31 (12)C25—C26—H26A119.9
C3—Fe1—S292.11 (11)C27—C26—H26A119.9
C2—Fe1—S186.37 (13)C28—C27—C26120.8 (5)
C1—Fe1—S1105.34 (13)C28—C27—H27A119.6
C3—Fe1—S1156.82 (12)C26—C27—H27A119.6
S2—Fe1—S179.80 (4)C27—C28—C29121.6 (5)
C2—Fe1—Fe298.82 (12)C27—C28—H28A119.2
C1—Fe1—Fe2152.62 (12)C29—C28—H28A119.2
C3—Fe1—Fe2101.02 (11)C30—C29—C28121.9 (4)
S2—Fe1—Fe256.37 (3)C30—C29—C24119.6 (4)
S1—Fe1—Fe256.43 (3)C28—C29—C24118.4 (4)
C4—Fe2—C590.72 (19)C29—C30—C31122.7 (4)
C4—Fe2—C697.14 (18)C29—C30—H30A118.7
C5—Fe2—C6101.29 (17)C31—C30—H30A118.7
C4—Fe2—S2162.42 (12)C30—C31—C32122.0 (4)
C5—Fe2—S293.68 (13)C30—C31—C36118.4 (4)
C6—Fe2—S298.66 (12)C32—C31—C36119.6 (4)
C4—Fe2—S188.73 (13)C33—C32—C31121.2 (4)
C5—Fe2—S1152.53 (12)C33—C32—H32A119.4
C6—Fe2—S1106.03 (12)C31—C32—H32A119.4
S2—Fe2—S179.55 (4)C32—C33—C34120.1 (4)
C4—Fe2—Fe1106.62 (13)C32—C33—H33A120.0
C5—Fe2—Fe197.68 (12)C34—C33—H33A120.0
C6—Fe2—Fe1149.27 (12)C35—C34—C33120.8 (4)
S2—Fe2—Fe155.93 (3)C35—C34—H34A119.6
S1—Fe2—Fe156.44 (3)C33—C34—H34A119.6
C38—Fe3—C3989.57 (18)C34—C35—C36122.3 (4)
C38—Fe3—C37101.71 (19)C34—C35—H35A118.8
C39—Fe3—C37100.1 (2)C36—C35—H35A118.8
C38—Fe3—S394.55 (14)C23—C36—C35124.2 (3)
C39—Fe3—S3161.87 (14)C23—C36—C31120.0 (3)
C37—Fe3—S396.31 (14)C35—C36—C31115.9 (3)
C38—Fe3—S4155.51 (14)O7—C37—Fe3176.6 (4)
C39—Fe3—S488.66 (13)O8—C38—Fe3176.4 (4)
C37—Fe3—S4102.64 (13)O9—C39—Fe3178.8 (4)
S3—Fe3—S480.29 (4)O10—C40—Fe4178.3 (5)
C38—Fe3—Fe4100.53 (14)O11—C41—Fe4178.1 (4)
C39—Fe3—Fe4105.84 (14)O12—C42—Fe4177.6 (4)
C37—Fe3—Fe4145.68 (13)C44—C43—S4112.9 (2)
S3—Fe3—Fe456.05 (3)C44—C43—H43A109.0
S4—Fe3—Fe456.71 (3)S4—C43—H43A109.0
C40—Fe4—C4191.94 (19)C44—C43—H43B109.0
C40—Fe4—C4298.8 (2)S4—C43—H43B109.0
C41—Fe4—C4299.21 (18)H43A—C43—H43B107.8
C40—Fe4—S392.62 (13)C57—C44—C45120.1 (3)
C41—Fe4—S3155.07 (13)C57—C44—C43120.5 (4)
C42—Fe4—S3104.28 (13)C45—C44—C43119.3 (3)
C40—Fe4—S4156.18 (15)C46—C45—C44123.5 (3)
C41—Fe4—S485.87 (14)C46—C45—C50116.6 (4)
C42—Fe4—S4104.95 (15)C44—C45—C50119.9 (4)
S3—Fe4—S480.15 (4)C47—C46—C45122.3 (4)
C40—Fe4—Fe3100.89 (15)C47—C46—H46A118.9
C41—Fe4—Fe398.80 (13)C45—C46—H46A118.9
C42—Fe4—Fe3152.71 (13)C46—C47—C48120.7 (5)
S3—Fe4—Fe356.27 (3)C46—C47—H47A119.6
S4—Fe4—Fe356.25 (3)C48—C47—H47A119.6
C22—S1—Fe2111.55 (11)C49—C48—C47120.0 (5)
C22—S1—Fe1116.60 (12)C49—C48—H48A120.0
Fe2—S1—Fe167.13 (3)C47—C48—H48A120.0
C7—S2—Fe1116.02 (11)C48—C49—C50121.5 (5)
C7—S2—Fe2116.99 (12)C48—C49—H49A119.3
Fe1—S2—Fe267.69 (3)C50—C49—H49A119.3
C58—S3—Fe4117.90 (12)C51—C50—C49122.9 (5)
C58—S3—Fe3115.48 (13)C51—C50—C45118.2 (5)
Fe4—S3—Fe367.67 (3)C49—C50—C45118.9 (5)
C43—S4—Fe3109.89 (11)C50—C51—C52124.0 (4)
C43—S4—Fe4117.34 (13)C50—C51—H51A118.0
Fe3—S4—Fe467.04 (3)C52—C51—H51A118.0
O1—C1—Fe1177.6 (4)C51—C52—C53123.2 (5)
O2—C2—Fe1177.9 (4)C51—C52—C57118.4 (4)
O3—C3—Fe1177.2 (3)C53—C52—C57118.4 (5)
O4—C4—Fe2178.1 (4)C54—C53—C52121.7 (6)
O5—C5—Fe2178.1 (4)C54—C53—H53A119.2
O6—C6—Fe2179.1 (3)C52—C53—H53A119.2
C8—C7—S2108.4 (2)C53—C54—C55121.5 (6)
C8—C7—H7A110.0C53—C54—H54A119.3
S2—C7—H7A110.0C55—C54—H54A119.3
C8—C7—H7B110.0C56—C55—C54118.7 (6)
S2—C7—H7B110.0C56—C55—H55A120.6
H7A—C7—H7B108.4C54—C55—H55A120.6
C21—C8—C9120.3 (3)C55—C56—C57122.4 (5)
C21—C8—C7120.7 (3)C55—C56—H56A118.8
C9—C8—C7119.0 (3)C57—C56—H56A118.8
C8—C9—C10123.5 (3)C44—C57—C56123.4 (4)
C8—C9—C14120.2 (3)C44—C57—C52119.4 (4)
C10—C9—C14116.3 (3)C56—C57—C52117.2 (4)
C11—C10—C9122.4 (4)C59—C58—S3107.1 (2)
C11—C10—H10A118.8C59—C58—H58A110.3
C9—C10—H10A118.8S3—C58—H58A110.3
C10—C11—C12120.0 (4)C59—C58—H58B110.3
C10—C11—H11A120.0S3—C58—H58B110.3
C12—C11—H11A120.0H58A—C58—H58B108.5
C13—C12—C11120.9 (4)C60—C59—C72121.0 (4)
C13—C12—H12A119.6C60—C59—C58120.1 (4)
C11—C12—H12A119.6C72—C59—C58118.9 (4)
C12—C13—C14120.6 (4)C59—C60—C61123.4 (5)
C12—C13—H13A119.7C59—C60—C65119.6 (6)
C14—C13—H13A119.7C61—C60—C65116.9 (6)
C15—C14—C13122.0 (4)C62—C61—C60122.3 (7)
C15—C14—C9118.3 (4)C62—C61—H61A118.9
C13—C14—C9119.8 (4)C60—C61—H61A118.9
C16—C15—C14122.8 (4)C61—C62—C63119.4 (9)
C16—C15—H15A118.6C61—C62—H62A120.3
C14—C15—H15A118.6C63—C62—H62A120.3
C15—C16—C17121.6 (5)C64—C63—C62122.3 (13)
C15—C16—C21119.5 (4)C64—C63—H63A118.8
C17—C16—C21118.9 (5)C62—C63—H63A118.8
C18—C17—C16121.3 (6)C63—C64—C65120.3 (11)
C18—C17—H17A119.4C63—C64—H64A119.8
C16—C17—H17A119.4C65—C64—H64A119.8
C17—C18—C19120.6 (6)C66—C65—C60118.2 (7)
C17—C18—H18A119.7C66—C65—C64123.1 (8)
C19—C18—H18A119.7C60—C65—C64118.7 (8)
C20—C19—C18121.0 (6)C65—C66—C67124.0 (7)
C20—C19—H19A119.5C65—C66—H66A118.0
C18—C19—H19A119.5C67—C66—H66A118.0
C19—C20—C21120.5 (5)C66—C67—C68124.0 (8)
C19—C20—H20A119.7C66—C67—C72118.9 (6)
C21—C20—H20A119.7C68—C67—C72117.0 (8)
C8—C21—C20123.6 (4)C69—C68—C67123.5 (11)
C8—C21—C16118.8 (4)C69—C68—H68A118.2
C20—C21—C16117.6 (4)C67—C68—H68A118.2
C23—C22—S1112.6 (2)C68—C69—C70119.7 (10)
C23—C22—H22A109.1C68—C69—H69A120.2
S1—C22—H22A109.1C70—C69—H69A120.2
C23—C22—H22B109.1C71—C70—C69119.9 (8)
S1—C22—H22B109.1C71—C70—H70A120.1
H22A—C22—H22B107.8C69—C70—H70A120.1
C36—C23—C24120.9 (3)C70—C71—C72121.2 (6)
C36—C23—C22119.6 (3)C70—C71—H71A119.4
C24—C23—C22119.5 (3)C72—C71—H71A119.4
C23—C24—C25124.4 (3)C71—C72—C59123.3 (4)
C23—C24—C29118.5 (4)C71—C72—C67118.7 (6)
C25—C24—C29117.1 (4)C59—C72—C67118.0 (6)
C2—Fe1—Fe2—C42.68 (19)C8—C9—C14—C13−179.0 (3)
C1—Fe1—Fe2—C4−130.8 (3)C10—C9—C14—C131.0 (5)
C3—Fe1—Fe2—C497.17 (19)C13—C14—C15—C16177.1 (4)
S2—Fe1—Fe2—C4−177.68 (16)C9—C14—C15—C16−2.1 (6)
S1—Fe1—Fe2—C4−76.96 (16)C14—C15—C16—C17−178.5 (4)
C2—Fe1—Fe2—C5−90.39 (17)C14—C15—C16—C210.7 (6)
C1—Fe1—Fe2—C5136.2 (3)C15—C16—C17—C18178.9 (4)
C3—Fe1—Fe2—C54.10 (17)C21—C16—C17—C18−0.3 (7)
S2—Fe1—Fe2—C589.26 (13)C16—C17—C18—C19−1.1 (8)
S1—Fe1—Fe2—C5−170.03 (13)C17—C18—C19—C201.0 (9)
C2—Fe1—Fe2—C6141.8 (3)C18—C19—C20—C210.5 (7)
C1—Fe1—Fe2—C68.3 (4)C9—C8—C21—C20175.7 (3)
C3—Fe1—Fe2—C6−123.7 (3)C7—C8—C21—C20−3.2 (5)
S2—Fe1—Fe2—C6−38.6 (2)C9—C8—C21—C16−4.5 (5)
S1—Fe1—Fe2—C662.1 (2)C7—C8—C21—C16176.6 (3)
C2—Fe1—Fe2—S2−179.64 (12)C19—C20—C21—C8178.0 (4)
C1—Fe1—Fe2—S246.9 (3)C19—C20—C21—C16−1.8 (6)
C3—Fe1—Fe2—S2−85.16 (12)C15—C16—C21—C82.7 (5)
S1—Fe1—Fe2—S2100.72 (5)C17—C16—C21—C8−178.1 (3)
C2—Fe1—Fe2—S179.64 (12)C15—C16—C21—C20−177.5 (3)
C1—Fe1—Fe2—S1−53.8 (3)C17—C16—C21—C201.7 (5)
C3—Fe1—Fe2—S1174.13 (12)Fe2—S1—C22—C23−156.9 (2)
S2—Fe1—Fe2—S1−100.72 (5)Fe1—S1—C22—C23−82.5 (3)
C38—Fe3—Fe4—C40−2.55 (19)S1—C22—C23—C36−73.4 (4)
C39—Fe3—Fe4—C40−95.12 (19)S1—C22—C23—C24109.1 (3)
C37—Fe3—Fe4—C40127.1 (3)C36—C23—C24—C25−176.8 (3)
S3—Fe3—Fe4—C4085.84 (14)C22—C23—C24—C250.7 (5)
S4—Fe3—Fe4—C40−172.69 (14)C36—C23—C24—C291.7 (5)
C38—Fe3—Fe4—C4191.15 (18)C22—C23—C24—C29179.2 (3)
C39—Fe3—Fe4—C41−1.42 (18)C23—C24—C25—C26177.5 (4)
C37—Fe3—Fe4—C41−139.2 (3)C29—C24—C25—C26−1.0 (6)
S3—Fe3—Fe4—C41179.55 (13)C24—C25—C26—C270.8 (7)
S4—Fe3—Fe4—C41−78.99 (13)C25—C26—C27—C28−0.2 (8)
C38—Fe3—Fe4—C42−138.1 (3)C26—C27—C28—C29−0.1 (8)
C39—Fe3—Fe4—C42129.4 (3)C27—C28—C29—C30−177.7 (5)
C37—Fe3—Fe4—C42−8.4 (4)C27—C28—C29—C24−0.1 (7)
S3—Fe3—Fe4—C42−49.7 (3)C23—C24—C29—C30−0.2 (5)
S4—Fe3—Fe4—C4251.8 (3)C25—C24—C29—C30178.3 (4)
C38—Fe3—Fe4—S3−88.40 (13)C23—C24—C29—C28−177.9 (3)
C39—Fe3—Fe4—S3179.03 (13)C25—C24—C29—C280.7 (5)
C37—Fe3—Fe4—S341.3 (3)C28—C29—C30—C31176.9 (4)
S4—Fe3—Fe4—S3101.46 (5)C24—C29—C30—C31−0.7 (6)
C38—Fe3—Fe4—S4170.14 (13)C29—C30—C31—C32179.9 (4)
C39—Fe3—Fe4—S477.57 (13)C29—C30—C31—C360.1 (6)
C37—Fe3—Fe4—S4−60.2 (3)C30—C31—C32—C33179.6 (4)
S3—Fe3—Fe4—S4−101.46 (5)C36—C31—C32—C33−0.6 (6)
C4—Fe2—S1—C22−138.18 (19)C31—C32—C33—C34−1.2 (7)
C5—Fe2—S1—C22132.7 (3)C32—C33—C34—C351.9 (7)
C6—Fe2—S1—C22−41.11 (17)C33—C34—C35—C36−0.6 (7)
S2—Fe2—S1—C2254.99 (13)C24—C23—C36—C35177.6 (3)
Fe1—Fe2—S1—C22110.85 (13)C22—C23—C36—C350.1 (5)
C4—Fe2—S1—Fe1110.97 (14)C24—C23—C36—C31−2.2 (5)
C5—Fe2—S1—Fe121.8 (3)C22—C23—C36—C31−179.7 (3)
C6—Fe2—S1—Fe1−151.96 (12)C34—C35—C36—C23179.0 (4)
S2—Fe2—S1—Fe1−55.86 (4)C34—C35—C36—C31−1.1 (6)
C2—Fe1—S1—C22153.35 (16)C30—C31—C36—C231.3 (5)
C1—Fe1—S1—C2253.80 (17)C32—C31—C36—C23−178.4 (3)
C3—Fe1—S1—C22−118.3 (3)C30—C31—C36—C35−178.5 (3)
S2—Fe1—S1—C22−47.33 (12)C32—C31—C36—C351.7 (5)
Fe2—Fe1—S1—C22−103.56 (12)C38—Fe3—C37—O7107 (7)
C2—Fe1—S1—Fe2−103.09 (12)C39—Fe3—C37—O7−161 (7)
C1—Fe1—S1—Fe2157.37 (12)S3—Fe3—C37—O711 (7)
C3—Fe1—S1—Fe2−14.8 (3)S4—Fe3—C37—O7−70 (7)
S2—Fe1—S1—Fe256.23 (4)Fe4—Fe3—C37—O7−22 (7)
C2—Fe1—S2—C7−109.4 (3)C39—Fe3—C38—O844 (7)
C1—Fe1—S2—C789.98 (18)C37—Fe3—C38—O8144 (7)
C3—Fe1—S2—C7−8.38 (18)S3—Fe3—C38—O8−118 (7)
S1—Fe1—S2—C7−166.51 (14)S4—Fe3—C38—O8−42 (7)
Fe2—Fe1—S2—C7−110.22 (14)Fe4—Fe3—C38—O8−62 (7)
C2—Fe1—S2—Fe20.8 (3)C38—Fe3—C39—O912 (21)
C1—Fe1—S2—Fe2−159.81 (13)C37—Fe3—C39—O9−89 (21)
C3—Fe1—S2—Fe2101.84 (12)S3—Fe3—C39—O9116 (21)
S1—Fe1—S2—Fe2−56.29 (4)S4—Fe3—C39—O9168 (100)
C4—Fe2—S2—C7116.2 (5)Fe4—Fe3—C39—O9113 (21)
C5—Fe2—S2—C712.07 (17)C41—Fe4—C40—O10−71 (13)
C6—Fe2—S2—C7−89.95 (17)C42—Fe4—C40—O10−171 (100)
S1—Fe2—S2—C7165.22 (13)S3—Fe4—C40—O1084 (13)
Fe1—Fe2—S2—C7108.85 (13)S4—Fe4—C40—O1013 (14)
C4—Fe2—S2—Fe17.4 (5)Fe3—Fe4—C40—O1028 (13)
C5—Fe2—S2—Fe1−96.79 (12)C40—Fe4—C41—O1163 (12)
C6—Fe2—S2—Fe1161.19 (12)C42—Fe4—C41—O11162 (12)
S1—Fe2—S2—Fe156.36 (4)S3—Fe4—C41—O11−37 (13)
C40—Fe4—S3—C586.6 (2)S4—Fe4—C41—O11−93 (12)
C41—Fe4—S3—C58106.9 (3)Fe3—Fe4—C41—O11−38 (12)
C42—Fe4—S3—C58−93.1 (2)C40—Fe4—C42—O1244 (11)
S4—Fe4—S3—C58163.79 (15)C41—Fe4—C42—O12−49 (11)
Fe3—Fe4—S3—C58107.99 (15)S3—Fe4—C42—O12139 (11)
C40—Fe4—S3—Fe3−101.35 (15)S4—Fe4—C42—O12−138 (11)
C41—Fe4—S3—Fe3−1.1 (3)Fe3—Fe4—C42—O12180 (100)
C42—Fe4—S3—Fe3158.86 (15)Fe3—S4—C43—C44164.5 (2)
S4—Fe4—S3—Fe355.80 (4)Fe4—S4—C43—C4490.8 (3)
C38—Fe3—S3—C58−11.74 (19)S4—C43—C44—C57−105.8 (3)
C39—Fe3—S3—C58−114.4 (4)S4—C43—C44—C4577.4 (4)
C37—Fe3—S3—C5890.60 (19)C57—C44—C45—C46−179.9 (3)
S4—Fe3—S3—C58−167.60 (14)C43—C44—C45—C46−3.1 (5)
Fe4—Fe3—S3—C58−111.38 (14)C57—C44—C45—C50−1.3 (5)
C38—Fe3—S3—Fe499.64 (14)C43—C44—C45—C50175.5 (3)
C39—Fe3—S3—Fe4−3.0 (4)C44—C45—C46—C47177.5 (4)
C37—Fe3—S3—Fe4−158.02 (13)C50—C45—C46—C47−1.2 (6)
S4—Fe3—S3—Fe4−56.22 (4)C45—C46—C47—C48−0.4 (7)
C38—Fe3—S4—C43−136.1 (3)C46—C47—C48—C491.7 (7)
C39—Fe3—S4—C43137.85 (19)C47—C48—C49—C50−1.3 (7)
C37—Fe3—S4—C4337.8 (2)C48—C49—C50—C51−178.4 (4)
S3—Fe3—S4—C43−56.59 (14)C48—C49—C50—C45−0.3 (6)
Fe4—Fe3—S4—C43−112.16 (14)C46—C45—C50—C51179.7 (3)
C38—Fe3—S4—Fe4−24.0 (3)C44—C45—C50—C511.0 (5)
C39—Fe3—S4—Fe4−109.99 (13)C46—C45—C50—C491.5 (5)
C37—Fe3—S4—Fe4149.92 (15)C44—C45—C50—C49−177.2 (3)
S3—Fe3—S4—Fe455.57 (3)C49—C50—C51—C52177.1 (4)
C40—Fe4—S4—C43119.4 (3)C45—C50—C51—C52−1.0 (6)
C41—Fe4—S4—C43−155.19 (17)C50—C51—C52—C53−178.1 (4)
C42—Fe4—S4—C43−56.75 (19)C50—C51—C52—C571.2 (6)
S3—Fe4—S4—C4345.53 (13)C51—C52—C53—C54−179.9 (5)
Fe3—Fe4—S4—C43101.36 (13)C57—C52—C53—C540.8 (8)
C40—Fe4—S4—Fe318.0 (3)C52—C53—C54—C55−1.0 (10)
C41—Fe4—S4—Fe3103.46 (12)C53—C54—C55—C560.6 (9)
C42—Fe4—S4—Fe3−158.10 (14)C54—C55—C56—C570.0 (7)
S3—Fe4—S4—Fe3−55.82 (4)C45—C44—C57—C56179.5 (3)
C2—Fe1—C1—O162 (8)C43—C44—C57—C562.7 (5)
C3—Fe1—C1—O1−32 (8)C45—C44—C57—C521.5 (5)
S2—Fe1—C1—O1−126 (8)C43—C44—C57—C52−175.2 (3)
S1—Fe1—C1—O1151 (8)C55—C56—C57—C44−178.2 (4)
Fe2—Fe1—C1—O1−165 (8)C55—C56—C57—C52−0.2 (6)
C1—Fe1—C2—O2169 (10)C51—C52—C57—C44−1.4 (6)
C3—Fe1—C2—O2−92 (10)C53—C52—C57—C44177.9 (4)
S2—Fe1—C2—O28(11)C51—C52—C57—C56−179.5 (4)
S1—Fe1—C2—O264 (10)C53—C52—C57—C56−0.2 (6)
Fe2—Fe1—C2—O29(10)Fe4—S3—C58—C59134.7 (3)
C2—Fe1—C3—O3113 (7)Fe3—S3—C58—C59−148.2 (3)
C1—Fe1—C3—O3−146 (7)S3—C58—C59—C60−92.3 (4)
S2—Fe1—C3—O3−43 (7)S3—C58—C59—C7284.7 (4)
S1—Fe1—C3—O326 (8)C72—C59—C60—C61−173.5 (4)
Fe2—Fe1—C3—O313 (8)C58—C59—C60—C613.4 (7)
C5—Fe2—C4—O4−98 (14)C72—C59—C60—C655.2 (6)
C6—Fe2—C4—O43(14)C58—C59—C60—C65−177.8 (4)
S2—Fe2—C4—O4157 (13)C59—C60—C61—C62−179.9 (5)
S1—Fe2—C4—O4109 (14)C65—C60—C61—C621.3 (8)
Fe1—Fe2—C4—O4163 (14)C60—C61—C62—C63−0.6 (12)
C4—Fe2—C5—O5−108 (11)C61—C62—C63—C641.0 (18)
C6—Fe2—C5—O5155 (11)C62—C63—C64—C65−2(2)
S2—Fe2—C5—O555 (11)C59—C60—C65—C66−0.3 (8)
S1—Fe2—C5—O5−19 (12)C61—C60—C65—C66178.6 (5)
Fe1—Fe2—C5—O5−1(11)C59—C60—C65—C64178.9 (6)
C4—Fe2—C6—O6−122 (26)C61—C60—C65—C64−2.2 (8)
C5—Fe2—C6—O6−30 (26)C63—C64—C65—C66−178.2 (11)
S2—Fe2—C6—O666 (26)C63—C64—C65—C602.7 (15)
S1—Fe2—C6—O6147 (26)C60—C65—C66—C67−4.1 (10)
Fe1—Fe2—C6—O697 (26)C64—C65—C66—C67176.8 (7)
Fe1—S2—C7—C8−160.2 (2)C65—C66—C67—C68−174.6 (6)
Fe2—S2—C7—C8122.8 (2)C65—C66—C67—C723.3 (9)
S2—C7—C8—C2194.4 (3)C66—C67—C68—C69177.5 (9)
S2—C7—C8—C9−84.5 (3)C72—C67—C68—C69−0.5 (12)
C21—C8—C9—C10−176.9 (3)C67—C68—C69—C70−0.2 (16)
C7—C8—C9—C102.1 (5)C68—C69—C70—C711.3 (13)
C21—C8—C9—C143.1 (5)C69—C70—C71—C72−1.6 (8)
C7—C8—C9—C14−178.0 (3)C70—C71—C72—C59−178.8 (4)
C8—C9—C10—C11178.1 (4)C70—C71—C72—C670.9 (6)
C14—C9—C10—C11−1.8 (5)C60—C59—C72—C71173.7 (4)
C9—C10—C11—C120.4 (6)C58—C59—C72—C71−3.3 (6)
C10—C11—C12—C132.0 (7)C60—C59—C72—C67−6.0 (6)
C11—C12—C13—C14−2.8 (7)C58—C59—C72—C67177.0 (3)
C12—C13—C14—C15−177.9 (4)C66—C67—C72—C71−177.9 (5)
C12—C13—C14—C91.3 (6)C68—C67—C72—C710.2 (7)
C8—C9—C14—C150.3 (5)C66—C67—C72—C591.8 (7)
C10—C9—C14—C15−179.8 (3)C68—C67—C72—C59179.8 (5)
Table 1
Selected geometric parameters (Å, °) top
Fe1—C21.794 (4)Fe3—C381.783 (4)
Fe1—C11.795 (4)Fe3—C391.784 (4)
Fe1—C31.796 (4)Fe3—C371.802 (5)
Fe1—S22.2517 (11)Fe3—S32.2560 (12)
Fe1—S12.2745 (12)Fe3—S42.2659 (11)
Fe1—Fe22.5148 (9)Fe3—Fe42.5092 (9)
Fe2—C41.781 (4)Fe4—C401.777 (5)
Fe2—C51.788 (4)Fe4—C411.788 (4)
Fe2—C61.805 (4)Fe4—C421.804 (4)
Fe2—S22.2634 (11)Fe4—S32.2502 (12)
Fe2—S12.2743 (11)Fe4—S42.2780 (13)
C1—Fe1—Fe2152.62 (12)Fe2—S1—Fe167.13 (3)
C6—Fe2—Fe1149.27 (12)Fe1—S2—Fe267.69 (3)
C37—Fe3—Fe4145.68 (13)Fe4—S3—Fe367.67 (3)
C42—Fe4—Fe3152.71 (13)Fe3—S4—Fe467.04 (3)
Acknowledgements top

This work was supported by the Ministry of Education of China and the National Natural Science Foundation of China (project Nos. 20128005, 20376010 and 20472012).

references
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