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Here, we report a cage\u2010directed assembly strategy that enables the programmed introduction of topologically correlated defects and induces aperiodicity in HKUST\u20101\u2010type frameworks. Pre\u2010synthesised Rh(II) metal\u2013organic cages or polyhedra (MOPs) act as persistent cavities that template the formation of HKUST\u20101\u2010based networks containing linker\u2010induced Cu\u2010vacancy domains confined within discrete cuboctahedral cavities. The use of dicarboxylate linkers, in which one carboxylate group is missing compared to the original 1,3,5\u2010benzenetricarboxylate linker, gives rise to nine distinct local defect configurations that are independently distributed throughout the lattice. This results in an aperiodic framework with preserved long\u2010range crystallinity. The resulting materials exhibit hierarchical micro\u2013mesoporosity, reversible loss and recovery of crystallinity, and a pronounced solvent\u2010induced breathing response. This work demonstrates that combining pre\u2010formed cages with linkers with reduced connectivity can be a new strategy to localise defects and access aperiodic MOFs with emergent structural adaptability.<\/jats:p>","DOI":"10.1002\/anie.9270871","type":"journal-article","created":{"date-parts":[[2026,6,26]],"date-time":"2026-06-26T11:31:53Z","timestamp":1782473513000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Defect\u2010Guided Assembly of Aperiodic and Flexible Metal\u2013Organic Frameworks From Pre\u2010Formed Cages"],"prefix":"10.1002","volume":"65","author":[{"given":"Francisco","family":"S\u00e1nchez\u2010F\u00e9rez","sequence":"first","affiliation":[{"name":"Catalan Institute of Nanoscience and Nanotechnology (ICN2) CSIC and The Barcelona Institute of Science and Technology Campus UAB  Barcelona Spain"},{"name":"Department of Chemistry Faculty of Science Universitat Aut\u00f2noma de Barcelona (UAB)  Barcelona Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Akim","family":"Khobotov\u2010Bakishev","sequence":"additional","affiliation":[{"name":"Catalan Institute of Nanoscience and Nanotechnology (ICN2) CSIC and The Barcelona Institute of Science and Technology Campus UAB  Barcelona Spain"},{"name":"Department of Chemistry Faculty of Science Universitat Aut\u00f2noma de Barcelona (UAB)  Barcelona Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Borja","family":"Ort\u00edn\u2010Rubio","sequence":"additional","affiliation":[{"name":"Catalan Institute of Nanoscience and Nanotechnology (ICN2) CSIC and The Barcelona Institute of Science and Technology Campus UAB  Barcelona Spain"},{"name":"Department of Chemistry Faculty of Science Universitat Aut\u00f2noma de Barcelona (UAB)  Barcelona Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Cornelia","family":"von Baeckman","sequence":"additional","affiliation":[{"name":"Catalan Institute of Nanoscience and Nanotechnology (ICN2) CSIC and The Barcelona Institute of Science and Technology Campus UAB  Barcelona Spain"},{"name":"Department of Chemistry Faculty of Science Universitat Aut\u00f2noma de Barcelona (UAB)  Barcelona Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Laura","family":"Hern\u00e1ndez\u2010L\u00f3pez","sequence":"additional","affiliation":[{"name":"Catalan Institute of Nanoscience and Nanotechnology (ICN2) CSIC and The Barcelona Institute of Science and Technology Campus UAB  Barcelona Spain"},{"name":"Department of Chemistry Faculty of Science Universitat Aut\u00f2noma de Barcelona (UAB)  Barcelona Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Alba","family":"Cort\u00e9s\u2010Mart\u00ednez","sequence":"additional","affiliation":[{"name":"Catalan Institute of Nanoscience and Nanotechnology (ICN2) CSIC and The Barcelona Institute of Science and Technology Campus UAB  Barcelona Spain"},{"name":"Department of Chemistry Faculty of Science Universitat Aut\u00f2noma de Barcelona (UAB)  Barcelona Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Robert A. 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