Inorganic Syntheses (Volume 21) by John P. Fackler

By John P. Fackler

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5. C. Kowala and J . M. Swan, Aust. J. , 19,547 (1966). 6. B. P. Block,Inorg. , 4, 14 (1953). 9. TETRANUCLEAR IRON-SULFUR AND IRON-SELENIUM CLUSTERS Submitted by GEORGE CHRISTOU,* C. DAVID GARNER,* A. BALASUBRAMANIAM,? BRIAN RIDGE,? and H. N. R Y D O d Checked by EDWARD I. STIEFEL* and WIE-HIN PAN* 4FeC13 + 14Na(Li)SR -+ 4 ; [Fe(SR),] + 12Na(Li)Cl i- 2Na(Li)SR 4 + 4X i- 2Na(Li)SR n [Fe(SR)3] -+ Na2(Li2)[Fe4X4(SR)4]i- SRSSR (X = S or Se) Tetrakis(thio1ato)tetra-p3-thio-tetrairon,[Fe4S4(SR),] *-, complexes involve a distorted cubane-type structure with a thiolato group completing an essentially tetrahedral array of sulfur atoms about each iron.

A. Stein, P. E. Ellis, R. C. Elder, and E. Deutsch,Inorg. , 15,1618 (1976). 3. Concentrated perchloric acid is an oxidant, and contact with organic materials can lead to explosion or fire. A. A. Schilt, Perchloric Acid and Perchlorates, G. , Columbus, OH, 1979. 6. Terrakis(benzenethiolato)metallate(2-) Complexes 23 4. R. C. Elder, L. K. Florian, R. E. Lake, and A. M. Yacynych, Inorg. , 12, 2690 (1973). 5. J . D. Lydon, D. L. Nosco, and E. Deutsch, unpublished observations. 6. R. C. Elder, G. J.

The synthesis of the cubane-like cluster Cp4Fe4S6 is similar to that reported for [CpFeS] 4,3a in which Cp4Fe4S, is undoubtedly a minor reaction product also. (In the preparation of [CpFeSI4 given in Reference 3a, the crude reaction product was extracted with hot bromobenzene. ) 8 Caution. The syntheses described below should be carried out in a wellventilated hood because of the release of CO and the strong stench of mercaptides. Schlenk-typeglassware should be used for most procedures. , Pittsburgh, PA 15201.

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