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

Scott R. Frerichs; John E. Ellis

doi:10.1016/0022-328X(89)85439-7

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

Scott R. Frerichs, John E. Ellis

Chemistry (Twin Cities)

Research output: Contribution to journal › Article › peer-review

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Abstract

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

Original language	English (US)
Pages (from-to)	C41-C44
Journal	Journal of Organometallic Chemistry
Volume	359
Issue number	2
DOIs	https://doi.org/10.1016/0022-328X(89)85439-7
State	Published - Jan 10 1989

Bibliographical note

Funding Information:
Acknowledgement. We thank the National Science Foundation (U.S.) and the Donors of the Petroleum Research Fund, administered by the American Chemical Society for financial support.

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

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

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note = "Funding Information: Acknowledgement. We thank the National Science Foundation (U.S.) and the Donors of the Petroleum Research Fund, administered by the American Chemical Society for financial support.",

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T2 - [(C5h5)Hf(CO)4]- and [(C5Me5)Hf(CO)4]-

AU - Frerichs, Scott R.

AU - Ellis, John E.

N1 - Funding Information: Acknowledgement. We thank the National Science Foundation (U.S.) and the Donors of the Petroleum Research Fund, administered by the American Chemical Society for financial support.

PY - 1989/1/10

Y1 - 1989/1/10

N2 - Potassium naphthalenide reductions of [(C5R5)HfCl3] (R H, Me) in 1,2-dimethoxyethane at -60°C followed by carbonylation at atmospheric pressure provide 25-50% isolated yields of the first examples of carbonyl anions of hafnium(0), [(C5H5)Hf(Co)4]- and [(C5Me5)Hf(CO)4]-. These were isolated as tetraethylammonium salts as well as K(cryptand-2.2.2) and K(15-Crown-5)2+ salts for the latter anion and now represent two of only four presently known Hf0 carbonyls. They were characterized by elemental analyses, IR and 1H and 13C NMR spectra.

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

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