in neat (no solvent) under Ar, Cl2O6 added at -180°C to metal salt, allowed to warm slowly until react. started, temp. increased to 15°C, successive addns. made until react. completed (colour, change in weight, qualitativetests, and X-ray anal.); evolved gases analized by IR; elem. anal.;

in neat (no solvent) under Ar, Cl2O6 added at -180°C to metal salt, allowed to warm slowly until react. started, temp. increased to 15°C, successive addns. made until react. completed (colour, change in weight, qualitativetests, and X-ray anal.); evolved gases analized by IR; elem. anal.;

in neat (no solvent) byproducts: O2; mixing at the temp. of liquid air; heating at 5°C;; distillation;;