in neat (no solvent) stainless steel cylinder loaded with LiF and I2O5 in a glovebox, IF5 added at -196°C on the vacuum line, cylinder shaken for 20h at room temp. then kept at 50°C for 3d with occasional shaking; IF5 (volatile at 25°C) pumped off, white solid residue consisted of mainly LiIF4O, LiF and IF3O with a small amt. of IO2F. IF3O and IO2F found in bottom of reactor and essentially pure LiIF4O obtained from upper walls of the reactor;

in neat (no solvent) absence of air and moisture; distn. of excess of BrF5 on IO2F, warming to -48°C; product mixt. not sepd., detd. by (19)F-NMR spectroscopy;

in neat (no solvent) absence of air and moisture; distn. of excess of BrF5 on IO2F, warming to -48°C; product mixt. not sepd., detd. by (19)F-NMR spectroscopy;

in further solvent(s) absence of air and moisture; excess of BrF5, -48°C;