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This work addresses this challenge by anchoring Fe(IV) on an iron\u2010phthalocyanine\u2010based conjugated organic framework (FePPC) featuring multi\u2010layered reticular structures and strong \u03c0\u2212Fe3d\u2212O2p orbital overlapping. The two\u2010dimensional planar structures provided easily accessible active sites and the extended in\u2010plane conjugation fine\u2010tunes the redox reactivity of surface\u2010confined Fe(IV) species, suppressing unproductive decay while preserving selectivity toward diverse pollutants, yielding a 3.2\u2010fold enhancement in Fe(IV) utilization efficiency. Combined experimental and computational results show that the enhanced orbital overlapping delocalizes electrons at the Fe(IV)\u2550O bond and reduces occupancy of its anti\u2010bonding \u03c0* orbital, thereby strengthening the bond against nucleophilic attack by peroxymonosulfate, suppressing O\n                    <jats:sub>2<\/jats:sub>\n                    evolution, and improving both pollutant selectivity and peroxide stoichiometric efficiency. When integrated into a scale\u2010up membrane reactor, FePPC achieved over 95% micropollutant removal during 72\u00a0h of continuous operation. This work fills an important knowledge gap in understanding Fe(IV) redox properties and selectivity, addressing technical bottlenecks in Fe(IV)\u2010based AOP systems toward low\u2010chemical consumption and high\u2010efficiency wastewater treatment.\n                  <\/jats:p>","DOI":"10.1002\/anie.5511823","type":"journal-article","created":{"date-parts":[[2026,7,13]],"date-time":"2026-07-13T17:33:07Z","timestamp":1783963987000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Tailoring High\u2010Valent Iron\u2010Oxo Species Redox via Extended \u03c0\u2010Fe3d\u2013O2p Orbital Overlapping Toward Chemical\u2010Efficient Water Purification"],"prefix":"10.1002","volume":"65","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-1117-1422","authenticated-orcid":false,"given":"Hongyu","family":"Zhou","sequence":"first","affiliation":[{"name":"School of Chemical Engineering Adelaide University  Adelaide South Australia Australia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Junwen","family":"Chen","sequence":"additional","affiliation":[{"name":"School of Chemical Engineering Adelaide University  Adelaide South Australia Australia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jiuyi","family":"Wang","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Catalysis Dalian Institute of Chemical Physics Chinese Academy of Sciences  Dalian P.R. 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