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The separation of xenon (Xe) and krypton (Kr) remains a significant industrial challenge. Adsorptive separation using porous solid adsorbents offers a promising avenue for efficient Xe/Kr purification; however, its practical implementation hinges on the development of materials with enhanced selectivity and adsorption capacity. A novel three‐dimensional microporous hydrogen‐bonded organic framework (HOF) was designed and synthesized for efficient Kr/Xe separation. The Xe/Kr separation performance was evaluated using sorption isotherms and dynamic breakthrough experiments as well as GCMC simulations. More details are discussed in the article by Bao et al . on pages 1303—1308. image