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Herein, we report a synergistic relay strategy that integrates phenoxyl\u2010radical\u2010mediated oligomerization and aromatic\u2010ring\u2010opening pathways for the highly efficient treatment of organic wastewater. This approach couples an initial high\u2010valence iron\u2010oxo species (HVIO)\u2010driven oligomerization via formal hydrogen atom transfer at one site with a subsequent singlet oxygen (\n                    <jats:sup>1<\/jats:sup>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    )\u2010mediated ring\u2010opening reaction at an adjacent site, enabled by a dual\u2010single\u2010atom Fe\n                    <jats:sub>1<\/jats:sub>\n                    Cu\n                    <jats:sub>1<\/jats:sub>\n                    \/TiO\n                    <jats:sub>2<\/jats:sub>\n                    photocatalyst. Under solar\u2010light irradiation, photoinduced electrons are transferred to peroxymonosulfate (PMS) at the Fe\n                    <jats:sub>1<\/jats:sub>\n                    site, which acts as a critical activator to generate HVIO for oligomerization\u2010based removal. Simultaneously, holes oxidize PMS at the Cu\n                    <jats:sub>1<\/jats:sub>\n                    site to produce\n                    <jats:sup>1<\/jats:sup>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    , leading to efficient aromatic\u2010ring\u2010opening. This sequential strategy achieved nearly 72% chemical oxygen demand removal with 23% carbon recovery into separable polymer products within 10 min for the phenol and ultimately reached complete removal with a rate constant of 1.21 min\n                    <jats:sup>\u22121<\/jats:sup>\n                    , significantly surpassing most reported values. Moreover, the system exhibited excellent stability and long\u2010term activity in a custom\u2010designed photo\u2010filter reactor, highlighting its practical potential. By coupling oligomerization and mineralization, this work provides a groundbreaking and versatile platform for treating complex organic wastewater.\n                  <\/jats:p>","DOI":"10.1002\/anie.2359022","type":"journal-article","created":{"date-parts":[[2026,7,17]],"date-time":"2026-07-17T05:30:54Z","timestamp":1784266254000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Synergetic Relay of Phenoxyl\u2010Radical\u2010Mediated Oligomerization and Aromatic\u2010Ring\u2010Opening Processes for Organic Wastewater Treatment"],"prefix":"10.1002","volume":"65","author":[{"given":"Xiaoru","family":"Huang","sequence":"first","affiliation":[{"name":"Institute of Photochemistry and Photofunctional Materials School of Materials and Chemistry University of Shanghai for Science and Technology  Shanghai 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