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Volume 69 
Part 4 
Pages m227-m228  
April 2013  

Received 8 March 2013
Accepted 19 March 2013
Online 23 March 2013

Key indicators
Single-crystal X-ray study
T = 93 K
Mean [sigma](C-C) = 0.007 Å
R = 0.075
wR = 0.186
Data-to-parameter ratio = 19.0
Details
Open access

Bis[1,2-bis(methoxycarbonyl)ethene-1,2-dithiolato-[kappa]2S,S']bis([eta]5-pentamethylcyclopentadienyl)tetra-[mu]3-sulfido-tetrairon(4 Fe-Fe) hexafluoridophosphate

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 asymmetric unit of the title compound, [Fe4(C6H6O4S2)2(C10H15)2S4]PF6, contains two different complex cations and two PF6- anions. The two complex cations have similar conformations with the butterfly-like Fe4S4 core surrounded by two pentamethylcyclopentadienyl ligands and the S atoms of two dithiolate ligands. In each Fe4S4 core, there are four short Fe-Fe and two long Fe...Fe contacts, suggesting bonding and non-bonding interactions, respectively. The Fe-S distances range from 2.1287 (13) to 2.2706 (16) Å for one and from 2.1233 (13) to 2.2650 (16) Å for the other Fe4S4 core. The Fe-S distances involving the dithiolate ligands are in a more narrow range [2.1764 (16)-2.1874 (13) Å for one and 2.1743 (14)-2.1779 (16) Å for the other cation]. There are no significant interactions between cations and anions.

Related literature

For background to polynuclear transition metal clusters, see: Geiger & Connelly (1985[Geiger, W. E. & Connelly, N. G. (1985). Adv. Organomet. Chem. 24, 87-130.]). For structural details of iron-sulfur cubane-type clusters, see: Blonk et al. (1992[Blonk, H. L., van der Linden, J. G. M., Steggerda, J. J., Geleyn, R. P., Smits, J. M. M., Beurskens, G., Beurskens, P. T. & Jordanov, J. (1992). Inorg. Chem. 31, 957-962.]); Inomata et al. (1994[Inomata, S., Hitomi, K., Tobita, H. & Ogino, H. (1994). Inorg. Chim. Acta, 225, 229-238.], 1995[Inomata, S., Takano, H., Hiyama, K., Tobita, H. & Ogino, H. (1995). Organometallics, 14, 2112-2114.]); Schunn et al. (1966[Schunn, R. A., Fritchie, C. J. Jr & Prewitt, C. T. (1966). Inorg. Chem. 5, 892-899.]); Toan et al. (1977a[Toan, T., Fehlhammer, W. P. & Dahl, L. F. (1977a). J. Am. Chem. Soc. 99, 402-407.],b[Toan, T., Teo, B. K., Ferguson, J. A., Meyer, T. J. & Dahl, L. F. (1977b). J. Am. Chem. Soc. 99, 408-416.]); Wei et al. (1966[Wei, C. H., Wilkes, G. R., Treichel, P. M. & Dahl, L. F. (1966). Inorg. Chem. 5, 900-905.]).

[Scheme 1]

Experimental

Crystal data
  • [Fe4(C6H6O4S2)2(C10H15)2S4]PF6

  • Mr = 1179.51

  • Monoclinic, P 21 /c

  • a = 15.546 (9) Å

  • b = 23.767 (13) Å

  • c = 24.872 (14) Å

  • [beta] = 102.209 (6)°

  • V = 8982 (9) Å3

  • Z = 8

  • Mo K[alpha] radiation

  • [mu] = 1.74 mm-1

  • T = 93 K

  • 0.20 × 0.20 × 0.15 mm

Data collection
  • Rigaku Saturn diffractometer

  • Absorption correction: multi-scan (REQAB; Jacobson, 1998[Jacobson, R. (1998). REQAB. Private communication to Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.634, Tmax = 0.770

  • 81617 measured reflections

  • 20169 independent reflections

  • 16442 reflections with I > 2[sigma](I)

  • Rint = 0.062

Refinement
  • R[F2 > 2[sigma](F2)] = 0.075

  • wR(F2) = 0.186

  • S = 1.14

  • 20169 reflections

  • 1064 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.94 e Å-3

  • [Delta][rho]min = -0.87 e Å-3

Table 1
Selected bond lengths (Å)

Fe1-Fe2 3.1989 (10)
Fe1-Fe3 2.7418 (10)
Fe1-Fe4 2.7306 (10)
Fe2-Fe3 2.7505 (9)
Fe2-Fe4 2.7601 (11)
Fe3-Fe4 3.2499 (11)
Fe5-Fe6 3.1960 (10)
Fe5-Fe7 2.7603 (9)
Fe5-Fe8 2.7619 (11)
Fe6-Fe7 2.7601 (10)
Fe6-Fe8 2.7223 (10)
Fe7-Fe8 3.2216 (11)

Data collection: CrystalClear (Rigaku, 2009[Rigaku (2009). CrystalClear. Rigaku Corporation, Tokyo, Japan.]); cell refinement: CrystalClear; data reduction: CrystalClear; 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. Rigaku Corporation, Tokyo, Japan.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2732 ).


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]
Blonk, H. L., van der Linden, J. G. M., Steggerda, J. J., Geleyn, R. P., Smits, J. M. M., Beurskens, G., Beurskens, P. T. & Jordanov, J. (1992). Inorg. Chem. 31, 957-962.  [CrossRef] [ChemPort] [ISI]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [ISI] [CrossRef] [ChemPort] [details]
Geiger, W. E. & Connelly, N. G. (1985). Adv. Organomet. Chem. 24, 87-130.  [CrossRef] [ChemPort]
Inomata, S., Hitomi, K., Tobita, H. & Ogino, H. (1994). Inorg. Chim. Acta, 225, 229-238.  [CrossRef] [ChemPort] [ISI]
Inomata, S., Takano, H., Hiyama, K., Tobita, H. & Ogino, H. (1995). Organometallics, 14, 2112-2114.  [CrossRef] [ChemPort]
Jacobson, R. (1998). REQAB. Private communication to Rigaku Corporation, Tokyo, Japan.
Rigaku (2006). CrystalStructure. Rigaku Corporation, Tokyo, Japan.
Rigaku (2009). CrystalClear. Rigaku Corporation, Tokyo, Japan.
Schunn, R. A., Fritchie, C. J. Jr & Prewitt, C. T. (1966). Inorg. Chem. 5, 892-899.  [CrossRef] [ChemPort] [ISI]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Toan, T., Fehlhammer, W. P. & Dahl, L. F. (1977a). J. Am. Chem. Soc. 99, 402-407.
Toan, T., Teo, B. K., Ferguson, J. A., Meyer, T. J. & Dahl, L. F. (1977b). J. Am. Chem. Soc. 99, 408-416.
Wei, C. H., Wilkes, G. R., Treichel, P. M. & Dahl, L. F. (1966). Inorg. Chem. 5, 900-905.  [CrossRef] [ChemPort] [ISI]


Acta Cryst (2013). E69, m227-m228   [ doi:10.1107/S1600536813007514 ]

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