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The well-known host molecule C-methylcalix[4]resorcinarene is shown to exist in two unique hexameric arrangements within the same crystal. These two hexameric assemblies are linked via a water molecule into a supra-heterodimer.

Solid-state isolation of a unique, small-molecule, supra-heterodimer of large hexameric assemblies of C-methylcalix[4]resorcinarene