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Accurate control of the layer number of orderly stacked 2D polymers has been an unsettled challenge in self‐assembly. Herein we describe the fabrication of a bilayer 2D supramolecular organic framework from a monolayer 2D supramolecular organic framework in water by utilizing the cooperative coordination of a rod‐like bipyridine ligands to zinc porphyrin subunits of the monolayer network. The monolayer...
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