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ABSTRACT Introduction: Copper deficiency is a common problem for ruminants. This can result from insufficient Cu intake (primary deficiency) or the presence of an antagonist that renders Cu unavailable for absorption (secondary deficiency). When Mo intake is sufficient, thiomolybdates, TMx, form in sufficient quantities in the rumen to significantly antagonize Cu. Aims: To synthesize the heterometallic sulphur assemblies that may be water soluble, which are kinetically inert and show relevance towards biological activities as Cu-Mo antagonism. Materials and methods: Various types of coinage metal hetrometallic sulphur systems have been synthesized using water soluble tetra-thiometallate anions for molybdenum and tungsten system. Resonance Ramam spectroscopy has been utilized to determine unambioguously the structure of the symmetrically coordinated trinuclear complexes for which the suitable single crystals for a crystal structure determination have been tried but got failed due to poor experimental environment. The genesis of the heteropolynuclear species have been correlated with the polynuclear Cu(?) complexes of different geometry. Results and discussion: The synthesized complexes in our study contain the stoichiometry between tetrathiomolybdate and copper in the ratio, 1:1, 1:2, 1:3 and 1:4, respectively. The tendency of iron in these complexes to enhance its coordination number has been demonstrated. Two equivalents of CuCl 2 H20 (2.8gm) and one equivalent of ammonium heptamolybdate (with respect to Mo) (1.8 gm) were dissolved in 40 ml aqueous NH3 (d, 0.7) to get a clear blue solution. Into this H2S gas was passed for an hour. Immediately, black precipitate of CuS appeared at the first Stage followed by the gradual red colouration of the solution. The formation of multinuclear species containing Cu and Mo through the dissolution of CuS with the concomitant reduction of Cu++ to Cu+ under the experimental condition. Conclusion: From various experiments it was concluded that high molybdenum and Sulphate intake disturb the metabolic efficiency of copper utilization and induce copper deficiency. Thus, �Cu-Mo antagonism� may be viewed as an interaction between Cu, Mo and S. Hence, the synthesis of Copper-Thiomolybdate-Protein Complex may shed some light on the chemical implication of this phenonmenon and may contribute quantitatively towards rationalizing the difference in its modus operendi in ruminants and monogastrics.