The aim of my research work was to carry out NMR and MS measurements using the newly synthesized ImEtHpH ligand to explore its [(η⁵-Cp*)Rh]²+ binding capabilities in an aqueous solution. Shedding light to the donor atom preference of the metal ion might provide valuable information on the forthcoming strategy of the synthesis of the Co/PGM heterobimetallic complexes. I have used NMR and ESI-MS methods during my work. In summary, our results indicate that this ligand also forms mainly (N,N) chelate with the rhodium cation but excess of the metal ion should be avoided when one is about to make the solid complexes. As previous results indicate, the synthesis should be started with the use of the Co(III) entity first that has high preference toward the (O,O) chelating set of these type of ambidentate ligands.