The starting material used was tin (99% granular 20 mesh, J.T. Baker Chemical Co.) and the synthesized SnI 4 . Under vacuum, stoichiometric quantities of SnI 4 and Sn metal were enclosed in an evacuated silica ampoule (P = 10 mTorr), heated to 600 °C over 6 hours and held at 600 °C for 32 hours before cooling to ambient temperature in the muffle furnace.