The reaction of (AlI·NEt
3)
4 withdonor-free
t-Bu
3SiNa in toluene at -78
C leads tothe generationand crystallization ofAl
4[Si(
t-Bu)
3]
4,which-after Al
4Cp*
4- is the second structurally characterizedAl
4R
4compound. The obtained experimental data were compared with results of
ab initio calculations.