in methanol mixing solns. of (C6H5)SH and AgNO3 under vigorously stirring; filtration of ppt.; rinsing with methanol and water successively; drying at 150°C (vac.);

1: tri-n-butylamine; AgNO3 / acetonitrile; methanol; propan-1-ol 2: acetonitrile View Scheme

tri-n-butylamine; AgNO3 in methanol; propan-1-ol; acetonitrile AgNO3 in MeCN was added to a soln. of C6H5SH, N(C4H9)3 and Me4NCl in MeCN (50 ml) and MeOH (50 ml), addition of 1-propanol (150 ml) and storageat 0°C caused crystn. of (Me4N)2(Ag6(SPh)8) and (Me4N)2(Ag5(SPh)7), when this mixt. was heated to; 60°C, much of the (Me4N)2(Ag6(SPh)8) redissolved, after additionof MeCN (AgSPh)n crystd. from this soln. when it was heated to 80°C and redissolved when mixt. was cooled to ambient temp. and (Me4N)2(Ag6(SPh)8) slowly grew for 4 weeks;

in acetonitrile byproducts: PhS(1-); complex was dissolved in MeCN, product ppt. slowly at room temp. and rapidly on heating;

in acetonitrile Electrolysis; under N2 atmosphere, initial voltage 20 V, 1 h, Ag anode, presence of Et4NClO4; washed with acetonitrile and then n-pentane, dried in vacuo; elem. anal.;

in 1,4-dioxane 20°C, 36 h;

1: in ethanol 6 h; Reflux; 2: With sodium hydroxide in ethanol 2 h; Reflux;