(Et4N)(ClO4) in acetone Electrolysis; under flush of Ar; electrolytic oxidn. of the metal in a glass cell in the presence of an acetone soln. of the thiuram disulphide ((NEt4)(ClO4)as electrolyte), current flow at 50 V, 50 min; solvent is reduced in vac., petroleum ether is added, compd. is dried in vac.;

in toluene metal and S-compd. were refluxed in 1:1.5 molar ratio in toluene for 3 h; soln. was filtered, concd. to 1/3 of its original vol., cooled to room temp., solid was filtered off, washed with petroleum ether (b.p. 60-80 °C), dried in vac., elem. anal.;