Abstract

AbstractThe double‐ or triple‐decker 3D metallo‐hexagons were obtained by self‐assembly of multitopic tris‐terpyridines with Cd2+ ions in near‐quantitative yield. Comprising up to 72 ionic pairs, the multiple spoked wheels display characteristic reversible gelation properties under thermodynamic conditions. The supramolecular metallo‐nanoarchitectures were characterized by 1H NMR, 2D NMR (COSY and NOESY), and diffusion‐ordered spectroscopy (DOSY) and HR‐ESI‐MS, traveling‐wave ion mobility mass spectrometry (TWIM‐MS), TEM, and AFM. For the first time, the self‐assembly of 45 units at once was demonstrated to yield exceptional giant triple‐decker hexagons of up to circa 42 000 Da.

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