The Merrifield solid-phase peptide synthesis technique has been adapted to the synthesis of homo- and heterometallic metal−organic complex arrays (MOCAs). A terpyridine-appended and Fmoc-protected L-tyrosine derivative was metalated with Pt(II), Rh(III), or Ru(II) ions in solution and sequentially coupled at the surface of functionalized polymeric resin to give a metal complex triad (Rh−Pt−Ru), tetrad (Ru−Rh−Pt−Pt), pentad (Rh−Pt−Ru−Pt−Rh), and hexad (Rh−Pt−Ru−Pt−Rh−Pt) with specific metal sequence arrangements. These were cleaved from the resin, and their character was confirmed by mass spectrometry.
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