期刊
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
卷 126, 期 37, 页码 11612-11620出版社
AMER CHEMICAL SOC
DOI: 10.1021/ja0472230
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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.
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