in neat (no solvent) stirring complex salt in flask; evacuation; introduction of SO3 vapour in stages; keeping reactants in contact for 15-20 mins after addn. of last aliquot of SO3; cooling with liquid N2, then with alcohol bath at -50°C; apparatus described;; warming to room temp.; evacuation for about 6 h; filling with dry N2; repeated washing of solid fluorosulphate with dry ether; drying under vac.; detn. by IR, 19F-NMR; elem. anal.;;
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