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However, weak inter\u2010cage interactions, such as van der Waals forces and hydrogen bonding can cause solid\u2010state MOCs to lose structural integrity during desolvation, leading to the loss of porosity. In this work, a novel strategy to retain the permanent porosity of Cu\u2010paddlewheel\u2010based MOCs, enabling their use as heterogeneous catalysts is presented. Post\u2010synthetic solvothermal treatments in non\u2010coordinating solvents, mesitylene, and <jats:italic>p<\/jats:italic>\u2010xylene, effectively preserve the packing structures of solvent\u2010evacuated MOCs while preventing cage agglomeration. The resulting MOCs exhibit an exceptional N<jats:sub>2<\/jats:sub> sorption capacity, with a high surface area (S<jats:sub>BET<\/jats:sub>\u00a0=\u00a01934\u00a0m<jats:sup>2<\/jats:sup>\u00a0g<jats:sup>\u22121<\/jats:sup> for MOP\u201023), which is among the highest reported for porous MOCs. Intriguingly, while the solvothermal treatment reduced Cu(II) to Cu(I) in the Cu\u2010paddlewheel clusters, the MOCs with mixed\u2010valenced Cu(I)\/Cu(II) maintained their crystallinity and permanent porosity. The catalytic activities of these MOCs are successfully examined in copper(I)\u2010catalyzed hydrative amide synthesis, highlighting the prospect of MOCs as versatile reaction platforms.<\/jats:p>","DOI":"10.1002\/smll.202308393","type":"journal-article","created":{"date-parts":[[2023,12,27]],"date-time":"2023-12-27T20:52:40Z","timestamp":1703710360000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":20,"title":["Unlocking High Porosity: Post\u2010Synthetic Solvothermal Treatment of Cu\u2010Paddlewheel Based Metal\u2013Organic Cages"],"prefix":"10.1002","volume":"20","author":[{"given":"Byeongchan","family":"Lee","sequence":"first","affiliation":[{"name":"Department of Physics and Chemistry Daegu Gyeongbuk Institute of Science and Technology (DGIST)  333 Techno Jungang\u2010daero Dalseong\u2010gun Daegu 42988 Republic of 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