Synthesis of the first anionic derivatives of Hf(CO)7: [(C5h5)Hf(CO)4]- and [(C5Me5)Hf(CO)4]-

摘要: Potassium naphthalenide reductions of [(C5R5)HfCl3] (R  H, Me) in 1,2-dimethoxyethane at −60°C followed by carbonylation atmospheric pressure provide 25–50% isolated yields the first examples carbonyl anions hafnium(0), [(C5H5)Hf(Co)4]− and [(C5Me5)Hf(CO)4]−. These were as tetraethylammonium salts well K(cryptand-2.2.2) K(15-Crown-5)2+ for latter anion now represent two only four presently known Hf0 carbonyls. They characterized elemental analyses, IR 1H 13C NMR spectra.