The first members of a new class of supramolecular organometallic compounds with mixed-alkali-metal cluster cores, LiK5 and Li3K3, sandwiched between two four-fold reduced corannulene decks are prepared and fully characterized. The triple-decker supramolecular anions, [(C20H104−)(LiK5)6+(C20H104−)]2− and [(C20H104−)(Li3K3)6+(C20H104−)]2−, illustrate a record ability of bowl-shaped and highly charged corannulene to provide all its sites, five benzene rings fused to a central five-membered ring, for binding of six alkali-metal ions. The previously unseen engagement of the hub-site of C20H104− in lithium binding is accompanied by unprecedented shifts up to −24 ppm in 7Li NMR spectra. The discussion of product formation mechanism, augmented by calculations, is provided.
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