Treatment of an overcrowded triselenatribismane, yl)methyl)phenyl-1,3,
5-triselena-2,4,6-tribismane, with hexamethylphosphorous triamide in t
oluene at 100 degrees C resulted in the quantitative formation of a st
able dibismuthene [TbtBi = BiTbt, where Tbt is 2,4,6-tris(bis(trimethy
lsilyl)methyl)phenyl], a compound containing a double bond formed betw
een two bismuth atoms. The compound formed as deep purple crystals upo
n cooling. Ultraviolet-visible and Raman spectra, x-ray crystallograph
ic structural analysis, and theoretical calculations provided evidence
for the double bond character of the Bi-Bi bond.