School of Studies in Chemistry, Jiwaji University, Gwalior-474 011, Madhya Pradesh, India E-mail : sksrivas7@yahoo.com Manuscript received 28 June 2007, accepted 2 July 2007 Reactions of C6H5HgOH with CS2 and 2-alkyl amino ethanol at -20 oc yield neutral two coordinate unsymmetrically substituted phenylmercury(II) N-alkyl, N·hydroxyethyl dithiocarbamate complexes,[C6H5HgS(S)CN(R)CH2CH2OH] [R =CH3 (1), C2H5 (2), n-C4H9 (3)]. Few bimetallic derivatives of compound 1 and 2 with HgII, CdII and AgI salts have also been prepared. The products bave been characterised using analytical and spectroscopic (IR, UV, 1H an.d 13C NMR) data. The bimetallic adducts 4-13 are formed through the coordination of the sulfur atom of phenylmercury(ll) N-alkyl, N-hydroxyethyl dithiocarbamate to the soft metal acceptors.