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We present HOF\u2010ZJNU\u20103, a hydrogen\u2010bonded organic framework built from an expanded BTB (4,4\u2032,4\u2033\u2010benzene\u20101,3,5\u2010triyl\u2010tribenzoate) linker, featuring the highest catenation degree observed in BTB\u2010based HOFs. This unique architecture confers good stability under solvent, pH, and thermal conditions. With optimally sized pores and aromatic\u2010rich surfaces, HOF\u2010ZJNU\u20103 demonstrates excellent propylene\/ethylene separation potential, outperforming its parent frameworks (HOF\u2010BTB and HOF\u2010BTB\u2010NH\n                    <jats:sub>2<\/jats:sub>\n                    ) under ambient conditions. Notably, the material accomplishes single\u2010cycle purification of high\u2010purity ethylene (99.95%) and propylene (99.5%) from equimolar binary mixtures, achieving a record ethylene productivity of 3.22\u00a0mol\u00a0kg\n                    <jats:sup>\u22121<\/jats:sup>\n                    among HOF adsorbents. This study not only establishes HOF\u2010ZJNU\u20103 as a benchmark HOF material for MTO product separation but also advances the structural design of HOFs for industrial olefin purification.\n                  <\/jats:p>","DOI":"10.1002\/anie.202511773","type":"journal-article","created":{"date-parts":[[2025,6,20]],"date-time":"2025-06-20T02:05:02Z","timestamp":1750385102000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":32,"title":["Efficient Separation of Methanol\u2010to\u2010Olefins Products Using a Robust Polycatenated Hydrogen\u2010Bonded Organic Framework"],"prefix":"10.1002","volume":"64","author":[{"given":"Shengjie","family":"Lin","sequence":"first","affiliation":[{"name":"Key Laboratory of the Ministry of Education for Advanced Catalysis Materials, College of Chemistry and Materials Science Zhejiang Normal University  Jinhua 321004 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