A homotelechelic macroligand bearing two 2,2′:6′,2″-terpyridin-4′-yl units, as chain ends, is used as building block for the preparation of a linear metallo-supramolecular chain-extended polymer. The macroligand has been prepared by nitroxide-mediated polymerization (NMP) of styrene using a bis-terpyridine-functionalized NMP initiator. The controlled character of the NMP process has been confirmed by detailed characterization of the polymer by size-exclusion chromatography, nuclear magnetic resonance spectroscopy as well as mass spectrometry. Subsequently, the self-assembly with FeII ions into the chain-extended metallopolymer and the disassembly thereof, in the presence of a strong competitive ligand, has been studied by UV–vis absorption spectroscopy and diffusion-ordered NMR spectroscopy. The reversibility of the formation of the metallo-supramolecular material, when addressed by external stimuli, could be proven. © 2013 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2013
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