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Chapter 4 introduces programmable metal array fabrication based on metalated amino acids and peptides, where various transition-metal complexes are covalently conjugated to the α-side chains of amino acids and peptides. It starts by explaining what metalated amino acids and peptides are including a brief history, classification, and their application. It then presents syntheses of a series of Pd- and Pt-complex bound glutamines and Pd- and Ru- complex bound norvalines and their sonication-induced self-assembly properties into a supramolecular gel along with the formation of well-regulated metal arrays. By the end of this chapter, applications of the supramolecular aggregates of metalated amino acids toward a cyclization reaction of alkynes, a cross-coupling reaction, and oxidations of alcohols and methoxybenzenes in aqueous conditions are explained. A detailed discussion of the mechanism of sonication-induced self-assembly and precise structural study of the supramolecular aggregates are included to show the effectiveness of metalated amino acids- and peptide-based metal array fabrication to design advanced smart materials based on bioorganometallic compounds.