Supramolecular tessellation is a newly emerging and promising area in supramolecular chemistry because of its unique structural aesthetics and potential applications. Herein, we investigate the "exo-wall" interactions of pillar[]arenes and prepare fantastic hexagonal supramolecular tessellations based on perethylated pillar[6]arenes () with electron-deficient molecules 1,5-difluoro-2,4-dinitrobenzene () and tetrafluoro-1,4-benzoquinone (). The crystal structures clearly confirm that can form highly ordered hexagonal 2D tiling patterns with / as linkers through cocrystallization. Moreover, the self-assembled packing arrangements in the ultimate cocrystal superstructures can be adjusted under different crystallization conditions. This work not only explores the rare exo-wall interactions based on pillar[]arenes but also reports the fabrication of supramolecular tessellations based on pillararenes for the first time, showing a new perspective in supramolecular chemistry.
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