Polymerization of the complexes [Ru(bpy)2(vinyl-py)2]2+ (I), [Ru(vinyl-bpy)3]2+ (II), [Ru(bpy)2(vinyl-bpy)]2+ (III),[Ru(bpy)2(vinyl-py)Cl]+ (IV), and [Fe(vinyl-bpy)3]2+ (V) can be initiated by electrochemical reduction in CH3CN solvent to produce stable, adherent, electrochemically active films on Pt, vitreous carbon, Sn02, and Ti02 electrodes. Randomly site-mixed copolymer (one-layer) and spatially segregated two-layer films of the pairs I and IV and II and V can be prepared by simultaneous and sequential polymerization of the appropriate monomers, respectively. The spatial features were confirmed by variable-angle X-ray photoelectron spectroscopy. Cyclic voltammetry of the copolymers is the additive response of the two redox components. In the two-layer films, however, oxidation state changes of the outer polymer films are constrained to occur via electron-transfer

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