Synthesis, Isolation, and Characterization of [K(cryptand 2.2.2)]2[Hf(CO)6], the First Substance To Contain Hafnium in a Negative Oxidation State. Structural Characterization of [K(cryptand 2.2.2)]2[M(CO)6]·Pyridine (M = Ti, Zr, and Hf)

John E Ellis, Kai Ming Chi

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36 Scopus citations

Abstract

Reductive carbonylation of M(CO)4|CH3C(CH2PMe2)3], M = Ti, Zr, and Hf, by [K(cryptand 2.2.2)] [naphthalene] at -70 followed by warming provides practically quantitative yields of the thermally robust salts [K(cryptand 2.2.2)]2[M(CO)6], include previously inaccessible [Hf(CO)6]2-. X-ray crystal structure analyses show the presence of essentially unperturbed octahi nexacarbonyl metal units in all three salts. This study represents the first structural characterization of “pure” carbonyimetallates of the group 4 elements and establishes the existence of a compound containing hafnium in a negative (-2) oxidation state for the first time.

Original languageEnglish (US)
Pages (from-to)6022-6025
Number of pages4
JournalJournal of the American Chemical Society
Volume112
Issue number16
DOIs
StatePublished - Jan 1990

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