Halo Carbonyls of the Group 4 Elements. Synthesis and Structural Characterization of Hf(CO)2(Me2PCH2CH2PMe2)2I2, the First Stable Derivative of the Unknown Hf(CO)6I2

John E Ellis, Scott R. Frerichs, Kai Ming Chi

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Abstract

Treatment of HfI4(Me2PCH2CH2PMe2)2 with potassium naphthalenide at -60 °C in 1,2-dimethoxyethane followed by a low-temperature, atmospheric pressure carbonylation provided Hf(CO)2(dmpe)2I2 in 60-70% yield as a yellow-green crystalline substance. This material represents the first stable derivative of the unknown Hf(CO)6I2 and has been characterized by a single-crystal X-ray structure. The latter establishes the eight-coordinate nature of the hafnium in the complex. Much less thermally stable compounds, presumed to be Hf(CO)2(dmpe)2Cl2and Zr(CO)2(dmpe)2I2, have also been prepared by analogous procedures and are formulated on the basis of their infrared spectra in the ν(CO) region.

Original languageEnglish (US)
Pages (from-to)2858-2859
Number of pages2
JournalOrganometallics
Volume9
Issue number11
DOIs
StatePublished - Jan 1 1990

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