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It is still of great difficulty to develop highly efficient catalysts toward the degradation of POPs. Herein, it is reported that regulating electronic structure of quasi\u2010single atomic ferric iron (Fe(III)) in the VO<jats:sub>2<\/jats:sub> support through the electronic metal\u2010support interaction (EMSI) is a versatile strategy to enhance the catalytic activity. Activated Fe(III) can react with peroxydisulfate (PDS) to produce both radicals and high\u2010valent iron (HVFe) simultaneously for the efficient and fast degradation of POPs. Density functional theory (DFT) calculations prove that the influence of EMSI promotes the electrons on Fe(III) 3<jats:italic>d<\/jats:italic>\u2010bond center moving close to the Fermi level, facilitating the charge transfer from Fe(III) to the adsorbate. Through the control experiments, both the radical path by PDS and the HVFe path aroused by the EMSI are confirmed in the POP degradation process. Consequently, the Fe\/VO<jats:sub>2<\/jats:sub> catalyst exhibits record\u2010breaking catalytic activity with the <jats:italic>k<\/jats:italic>\u2010value as high as 56.7, 43.3\u00a0\u00b5mol s<jats:sup>\u22121<\/jats:sup> g<jats:sup>\u22121<\/jats:sup> for p\u2010chlorophenol and 2,4\u2010dichlorophenol degradation, respectively.<\/jats:p>","DOI":"10.1002\/smll.202203269","type":"journal-article","created":{"date-parts":[[2022,7,25]],"date-time":"2022-07-25T01:25:09Z","timestamp":1658712309000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":12,"title":["Electronic Metal\u2010Support Interaction Directing the Design of Fe(III)\u2010Based Catalysts for Efficient Advanced Oxidation Processes by Dual Reaction Paths"],"prefix":"10.1002","volume":"18","author":[{"given":"Mingsen","family":"Xie","sequence":"first","affiliation":[{"name":"Tianjin Key Laboratory of Molecular Optoelectronic Sciences Department of Chemistry School of Science Tianjin University  Tianjin 300072 P. 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