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Owing to the finite building blocks and difficulty in structural identification, it remains a tremendous challenge to elaborately design and synthesize three‐dimensional covalent organic frameworks (3D COFs) with predetermined topologies. Herein, we report the first two cases of 3D COFs with the non‐interpenetrated hea net, termed JUC‐596 and JUC‐597, by using the combination of tetrahedral and triangular...
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