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The unprecedented infinite stacks of trans‐1,2‐bis(4‐pyridyl)ethylene (4,4′‐bpe) were prepared with a supramolecular YbIII–aqua complex that exhibited the stereospecific photocycloaddition of olefins within a single‐crystal‐to‐single‐crystal process and was confirmed by crystallographic methods (see figure). The supramolecular assistance of YbIII was observed in solution, in which the reaction proceeded catalytically.

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