The formation of 3D fused 10-membered "bracelet" frameworks derived from the alkyl-substituted curcurbit[5]urils (SQ[5]s), 1,2,4-hexamethylcucurbit [5]uril (1,2,), and pentacyclopentanocucurbit[5]uril (PCyHQ[5]) and K þ ions is described. These remarkable catenated structures feature trigonal-planar branching units involving three SQ[5]s connected via their bound K þ ions in a triangular manner in which the coordination of each K þ ion to the five portal carbonyl oxygen atoms of one SQ [5] as well as to a bridging portal carbonyl oxygen from an adjacent SQ[5] draws the edges of three portals into close proximity. The corresponding offset angle at each junction provides the basis for the 3D assembly of the observed fused 10-membered SQ[5] bracelet frameworks.

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