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Abstract A porous molecular crystal (PMC) assembled by macrocyclic cyclotetrabenzoin acetate is an efficient adsorbent for CO₂separations. The 7.1×7.1 Å square pore of PMC and its ester C=O groups play important roles in improving its affinity for CO₂molecules. The benzene walls of macrocycle engage in an apparent [π⋅⋅⋅π] interaction with the molecule of CO₂at low pressure. In addition, the polar carbonyl groups pointing inward the square channels reduce the size of aperture to a 5.0×5.0 Å square, which offers kinetic selectivity for CO₂capture. The PMC features water tolerance and high structural stability under vacuum and various gas adsorption conditions, which are rare among intrinsically porous organic molecules. Most importantly, the moderate adsorbate‐adsorbent interaction allows the PMC to be readily regenerated, and therefore applied to pressure swing adsorption processes. The eluted N₂and CH₄are obtained with over 99.9 % and 99.8 % purity, respectively, and the separation performance is stable for 30 cycles. Coupled with its easy synthesis, cyclotetrabenzoin acetate is a promising adsorbent for CO₂separations from flue and natural gases.