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Here, we report a simple, one\u2010pot, inexpensive, regioselective synthesis of highly porous poly(aryl thioether)s through polycondensation of perfluoroaromatic compounds with sodium sulfide. The unprecedented temperature\u2010dependent para\u2010directing formation of thioether linkages leads to a stepwise transition of the polymer extension into a network, thereby allowing fine control of the porosity and optical band gaps. The obtained porous organic polymers with ultra\u2010microporosity (&lt;1\u2005nm) and sulfur as the surface functional groups show size\u2010dependent separation of organic micropollutants and selective removal of mercury ions from water. Our findings offer easy access to poly(aryl thioether)s with accessible sulfur functionalities and higher complexity, which will help in realizing advanced synthetic designs in applications such as adsorption, (photo)catalysis, and (opto)electronics.<\/jats:p>","DOI":"10.1002\/anie.202304378","type":"journal-article","created":{"date-parts":[[2023,4,12]],"date-time":"2023-04-12T10:31:20Z","timestamp":1681295480000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":6,"title":["Covalent Scrambling in Porous Polyarylthioethers through a Stepwise S<sub>N<\/sub>Ar for Tunable Bandgap and Porosity"],"prefix":"10.1002","volume":"62","author":[{"given":"Doyun","family":"Kim","sequence":"first","affiliation":[{"name":"Department of Chemical and Biomolecular Engineering Korea Advanced Institute of Science and Technology (KAIST)  291 Daehak-ro Yuseong-gu, Daejeon 34141 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Thien S.","family":"Nguyen","sequence":"additional","affiliation":[{"name":"Advanced Membranes and Porous Materials Center (AMPMC) Physical Science and Engineering (PSE) King Abdullah University of Science and Technology (KAUST)  Thuwal 23955-6900 Saudi Arabia"},{"name":"KAUST Catalysis Center (KCC) Physical Science &amp; 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