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Three-dimensional (3D) covalent organic frameworks (COFs) are rare because there is a limited choice of organic building blocks that offer multiple reactive sites in a polyhedral geometry. Here, we synthesized an organic cage molecule ( Cage-6-NH   2  ) that was used as a triangular prism node to yield the first cage-based 3D COF, 3D-CageCOF-1 . This COF adopts an unreported 2-fold interpenetrated acs topology and exhibits reversible dynamic behavior, switching between a small-pore ( sp ) structure and a large-pore ( lp ) structure. It also shows high CO 2 uptake and captures water at low humidity (&lt;40%). This demonstrates the potential for expanding the structural complexity of 3D COFs by using organic cages as the building units.

3D Cage COFs: A Dynamic Three-Dimensional Covalent Organic Framework with High-Connectivity Organic Cage Nodes