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A unique lithium halide complex, [(LiBr)2·3HMPA·toluene]: synthesis from reaction of solid NH4Br with BunLi in HMPA (hexamethylphosphoramide)/toluene media, crystal structure showing two Li–Br units linked by three µ2-HMPA ligands, and detection of 7Li 31P coupling in solutions of the complex

BARR, D and DOYLE, M J and Mulvey, Robert and RAITHBY, P R and REED, D and SNAITH, R and WRIGHT, D S (1989) A unique lithium halide complex, [(LiBr)2·3HMPA·toluene]: synthesis from reaction of solid NH4Br with BunLi in HMPA (hexamethylphosphoramide)/toluene media, crystal structure showing two Li–Br units linked by three µ2-HMPA ligands, and detection of 7Li 31P coupling in solutions of the complex. Journal of the Chemical Society, Chemical Communications (5). pp. 318-319. ISSN 0022-4936

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Abstract

Reaction of solid NH4Br with BunLi and HMPA (hexamethylphosphoramide)(1 : 1 : 2 ratio) in toluene produces (LiBr)2·3HMPA·toluene, (1), shown by X-ray crystallography to contain (LiBr)2·3HMPA molecules whose two terminal Li–Br units are linked by three µ2-HMPA ligands and with toluene molecules lying between these units in the lattice; in arene solutions, the (LiBr)2·3HMPA units remain intact, giving rise in 7Li n.m.r. spectra to 1 : 3 : 3 : 1 quartets caused by through-bond (OP) coupling of each 7Li nucleus to three 31P(HMPA) centres.