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Abstract
Spectroscopic analysis of lithiated cyclic phospho-nates belonging to the 1,3,2-dioxaphosphorinane 2-oxide class have been examined by NMR spectroscopy in THF and by single-crystal X-ray crystallography. Lithio P-benzyl-1,3,2-dioxaphosphorinane 2-oxide (Li+7−) and lithio P-isopropyl-1,3,2-dioxaphosphorinane 2-oxide (Li+8−) are characterized by freely rotating, sp2-hybridized anions devoid of lithium–carbon contacts. The anions are most likely dimers linked through oxygen-lithium bridges. The P-isopropyl compound crystallized from TMEDA/THF as a C-lithiated dimer in which each lithium bridges a carbon and an oxygen and is solvated by one TMEDA molecule. © 1998 John Wiley & Sons, Inc. Heteroatom Chem 9:209–218, 1998
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