Alternating transition metal-organic bi- and multilayers composed of dicationic (ethylenediamine)palladium(II) and platinum(II) complexes and N-alkyl-4,4’-bipyridinium, [(η3−C3H5)Pd{(4,4’-bpy-N-(CH2)12OC6H3-3,5-(OMe)2)} (OAc)]NO3 and [M{(4,4’-bpy-N-(CH2)12OC6H3-3,5-(OMe)2)}2(en)](NO3)4 (M = Pd, Pt, en = 1,2-ethylenediamine), were synthesized on mica surface by simple casting method from aqueous solution.