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http://dx.doi.org/10.5012/bkcs.2007.28.11.1958

Synthesis and Characterization of Ir(H)(CO)(PEt3})2(η2-C60)  

Lee, Chang-Yeon (Department of Chemistry and School of Molecular Science (BK21), Korea Advanced Institute of Science and Technology)
Lee, Gae-Hang (Department of Chemistry and School of Molecular Science (BK21), Korea Advanced Institute of Science and Technology)
Kang, Hong-Kyu (Department of Chemistry and School of Molecular Science (BK21), Korea Advanced Institute of Science and Technology)
Park, Bo-Keun (Department of Chemistry and School of Molecular Science (BK21), Korea Advanced Institute of Science and Technology)
Park, Joon-T. (Department of Chemistry and School of Molecular Science (BK21), Korea Advanced Institute of Science and Technology)
Publication Information
Bulletin of the Korean Chemical Society / v.28, no.11, 2007 , pp. 1958-1962 More about this Journal
Abstract
The title complex, Ir(H)(CO)(PEt3)2(η 2-C60) (2), has been prepared by the reaction of excess C60 (4 equiv) with a tetrairidium complex Ir4(CO)8(PEt3)4 (1) in refluxing chlorobenzene in 40% yield as green crystals. Compound 2 has been characterized by cyclic voltammetry (CV), spectroscopic methods (mass, IR, 1H and 31P NMR), and a single crystal X-ray diffraction study. The molecular structure reveals that the iridium atom of 2 is coordinated by two axial ligands of a hydrogen atom and a carbonyl group, and three equatorial ligands of two phosphorus atoms and an η 2-C60 moiety. The CV study exhibits three reversible one-electron redox waves for the successive reductions of 2, together with additional four redox waves due to free C60 reductions, which was formed by decomposition of 2 in the reduced states. The three reversible redox waves of 2 are shifted to more negative potentials by ca. 270 mV compared to free C60, reflecting both metal-to-C60 π-back-donation and the electron-donating nature of the two phosphorus ligands.
Keywords
Metallofullerene; Iridium; Crystal structure; Cyclic voltammetry;
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