Department of Chemistry, B. N. College, Patna University, Patna-800 004, Bihar, India Manuscript received 8 August 2007, revised 7 January 2008, accepted 8 January 2008 The complexes of palladium(II) and platinum(ll) with triphenylphosphine sulphide (Ph3PS) and triphenylstibine (Ph3Sb) of composition [ML2X2] (M = PdII, PtII ; L = Ph3PS or Ph3Sb and X = CI, Br, I or SCN) have been prepared and characterized. The triphenylstibine sulphide complexes like former ligand could not be isolated as the ligand get desulphurized in aqueous medium and the complexes of desulphurized ligand triphenylstibine have only been isolated in pure form. The complexes have been characterized by UV, IR, 1H NMR spectroscopic methods and resembles with square planar geometry.