Abstract
The heterometallic Sb(III)/Li cage complex [{Sb(P-t-Bu)3}2Li6 6THF] (1) is obtained by the low-temperature (<0 deg C) reaction of Sb(NMe2)3 with t-BuPHLi (1:3 equiv) in THF. Thermolysis of this reaction solution leads to the formation of the bicyclic distibane [(t-BuP)3Sb]2 (2). 31P NMR spectroscopic studies reveal that this process involves initial formation of [(t-BuP)3Sb]- and [t-Bu(H)PP-t-Bu]- anions. Complexes 1 and 2 have been characterized in the solid state by X-ray diffraction studies.