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A Homologous Series of Regioselectively Tetradeprotonated Group 8 Metallocenes: New Inverse Crown Ring Compounds Synthesized via a Mixed Sodium-Magnesium Tris(diisopropylamide) Synergic Base

Lookup NU author(s): Professor William Clegg, Duncan Tooke

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Abstract

Subjecting ferrocene, ruthenocene, or osmocene to the synergic amide base sodium-magnesium tris(diisopropylamido) affords a unique homologous series of metallocene derivatives of general formula [{M(C5H3) 2}Na4Mg4(i-Pr2N)8] (where M = Fe (1), Ru (2), or Os (3)). X-ray crystallographic studies of 1-3 reveal a common molecular "inverse crown" structure comprising a 16-membered [(NaNMgN)4]4+ "host" ring and a metallocenetetraide [M(C5H3)2]4- "guest" core, the cleaved protons of which are lost selectively from the 1, 1′, 3, and 3′-positions. Variable-temperature NMR spectroscopic studies indicate that 1, 2, and 3 each exist as two distinct interconverting conformers in arene solution, the rates of exchange of which have been calculated using coalescence and EXSY NMR measurements.

Publication metadata

Author(s): Andrikopoulos PC, Armstrong DR, Clegg W, Gilfillan CJ, Hevia E, Kennedy AR, Mulvey RE, O'Hara CT, Parkinson JA, Tooke DM

Publication type: Article

Publication status: Published

Journal: Journal of the American Chemical Society

Year: 2004

Volume: 126

Issue: 37

Pages: 11612-11620

Print publication date: 22/09/2004

ISSN (print): 0002-7863

ISSN (electronic): 1520-5126

Publisher: American Chemical Society

URL: http://dx.doi.org/10.1021/ja0472230

DOI: 10.1021/ja0472230

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