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Volume 69 
Part 4 
Page m181  
April 2013  

Received 12 February 2013
Accepted 26 February 2013
Online 2 March 2013

Key indicators
Single-crystal X-ray study
T = 296 K
Mean [sigma](C-C) = 0.004 Å
R = 0.030
wR = 0.080
Data-to-parameter ratio = 20.1
Details
Open access

Bis[1,2-bis(ethoxycarbonyl)ethene-1,2-dithiolato-[kappa]2S,S']bis([eta]5-pentamethylcyclopentadienyl)tetra-[mu]3-sulfido-diiron(IV)diiron(III)(3 Fe-Fe)

aFaculty of Symbiotic Systems Science, Fukushima University, 1 Kanayagawa, Fukushima 960-1296, Japan, and bCenter for Practical and Project-Based Learning, Cluster of Science and Technology, Fukushima University, 1 Kanayagawa, Fukushima 960-1296, Japan
Correspondence e-mail: inomata@sss.fukushima-u.ac.jp

The title compound, [Fe4(C10H15)2(C8H10O4S2)2S4], contains a twisted Fe4S4 cubane-like core. A twofold rotation axis passes through the Fe4S4 core, completing the coordination of the four Fe atoms with two pentamethylcyclopentadienyl ligands and two chelating dithiolate ligands. There are three short Fe-Fe and three long Fe...Fe contacts in the Fe4S4 core, suggesting bonding and non-bonding interactions, respectively. The Fe-S bonds in the Fe4S4 core range from 2.1523 (5) to 2.2667 (6) Å and are somewhat longer than the Fe-S bonds involving the dithiolate ligand.

Related literature

For details of the synthesis, see: Inomata et al. (1995[Inomata, S., Takano, H., Hiyama, K., Tobita, H. & Ogino, H. (1995). Organometallics, 14, 2112-2114.]). For related structures, see: Inomata et al. (1990[Inomata, S., Tobita, H. & Ogino, H. (1990). J. Am. Chem. Soc. 112, 6145-6146.], 1994[Inomata, S., Hiyama, K., Tobita, H. & Ogino, H. (1994). Inorg. Chem. 33, 5337-5342.]). For general background to compounds with iron-sulfur cubane-type clusters, see: Holm (1977[Holm, R. H. (1977). Acc. Chem. Res. 12, 427-434.]); Holm et al. (1990[Holm, R. H., Ciurli, S. & Weigel, J. A. (1990). Prog. Inorg. Chem. 38, 1-74.]).

[Scheme 1]

Experimental

Crystal data
  • [Fe4(C10H15)2(C8H10O4S2)2S4]

  • Mr = 1090.65

  • Monoclinic, C 2/c

  • a = 23.4532 (5) Å

  • b = 10.4466 (2) Å

  • c = 18.3113 (3) Å

  • [beta] = 90.6186 (7)°

  • V = 4486.14 (15) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 1.69 mm-1

  • T = 296 K

  • 0.30 × 0.20 × 0.20 mm

Data collection
  • Rigaku R-AXIS RAPID diffractometer

  • Absorption correction: multi-scan (REQAB; Jacobson, 1998[Jacobson, R. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.560, Tmax = 0.714

  • 21429 measured reflections

  • 5111 independent reflections

  • 4694 reflections with I > 2[sigma](I)

  • Rint = 0.044

Refinement
  • R[F2 > 2[sigma](F2)] = 0.030

  • wR(F2) = 0.080

  • S = 1.06

  • 5111 reflections

  • 254 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.50 e Å-3

  • [Delta][rho]min = -0.33 e Å-3

Table 1
Selected bond lengths (Å)

Fe1-Fe1i 3.3743 (3)
Fe1-Fe2 2.7253 (4)
Fe1-Fe2i 3.2683 (3)
Fe1-S1 2.1956 (5)
Fe1-S1i 2.2551 (5)
Fe1-S2 2.1749 (5)
Fe2-Fe2i 2.7619 (3)
Fe2-S1 2.2736 (5)
Fe2-S2 2.1523 (5)
Fe2-S2i 2.2667 (6)
Fe2-S3 2.1541 (5)
Fe2-S4 2.1934 (6)
Symmetry code: (i) [-x+1, y, -z+{\script{1\over 2}}].

Data collection: RAPID-AUTO (Rigaku, 2006[Rigaku (2006). CrystalStructure and RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.]); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SIR97 (Altomare et al., 1999[Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]); software used to prepare material for publication: CrystalStructure (Rigaku, 2006[Rigaku (2006). CrystalStructure and RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2725 ).


References

Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.  [ISI] [CrossRef] [ChemPort] [details]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [ISI] [CrossRef] [ChemPort] [details]
Holm, R. H. (1977). Acc. Chem. Res. 12, 427-434.  [CrossRef] [ISI]
Holm, R. H., Ciurli, S. & Weigel, J. A. (1990). Prog. Inorg. Chem. 38, 1-74.  [CrossRef] [ChemPort]
Inomata, S., Hiyama, K., Tobita, H. & Ogino, H. (1994). Inorg. Chem. 33, 5337-5342.  [CrossRef] [ChemPort] [ISI]
Inomata, S., Takano, H., Hiyama, K., Tobita, H. & Ogino, H. (1995). Organometallics, 14, 2112-2114.  [CrossRef] [ChemPort]
Inomata, S., Tobita, H. & Ogino, H. (1990). J. Am. Chem. Soc. 112, 6145-6146.  [CrossRef] [ChemPort] [ISI]
Jacobson, R. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan.
Rigaku (2006). CrystalStructure and RAPID-AUTO. Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]


Acta Cryst (2013). E69, m181  [ doi:10.1107/S1600536813005564 ]

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