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In this work, we employed a photocatalytic anaerobic reaction pathway for directly synthesizing the targeted high\u2010value xylenol and H\n                    <jats:sub>2<\/jats:sub>\n                    from\n                    <jats:italic>m<\/jats:italic>\n                    \u2010xylene and water over a palladium single atom\u2010loaded TiO\n                    <jats:sub>2<\/jats:sub>\n                    with zinc modification (Pd\n                    <jats:sub>1<\/jats:sub>\n                    \u2010TiO\n                    <jats:sub>2<\/jats:sub>\n                    (Zn)). In situ infrared spectroscopy and electron paramagnetic resonance, in combination with first\u2010principles simulations, revealed that the photocatalytic anaerobic conversion of\n                    <jats:italic>m<\/jats:italic>\n                    \u2010xylene proceeds via surface lattice oxygen\u2010mediated hydroxylation. Lattice oxygen coordinated with Pd acts as a recyclable oxygen source for phenolic hydroxyl groups, regenerated by the rate\u2010determining water oxidation. Isotope labeling confirms hydroxyl hydrogen originates from the benzene ring, not water; water only provides oxygen. The zinc modification could significantly reduce the reaction barrier of the water\u2010oxidation step from 0.85 to 0.22\u00a0eV at the Pd\u2010O site. Therefore, the phenolic production rate over Pd\n                    <jats:sub>1<\/jats:sub>\n                    \u2010TiO\n                    <jats:sub>2<\/jats:sub>\n                    (Zn) reached 376.9\u00a0\u00b5mol g\n                    <jats:sup>\u22121<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    , accompanied by an exceptionally high phenolic selectivity of 98.5% and a hydrogen production rate of 380.6\u00a0\u00b5mol g\n                    <jats:sup>\u22121<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    , 2\u2010fold higher than that of unmodified Pd\n                    <jats:sub>1<\/jats:sub>\n                    \u2010TiO\n                    <jats:sub>2<\/jats:sub>\n                    .\n                  <\/jats:p>","DOI":"10.1002\/anie.6427054","type":"journal-article","created":{"date-parts":[[2026,7,7]],"date-time":"2026-07-07T15:03:06Z","timestamp":1783436586000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Photocatalytic Anaerobic Conversion of\n                    <i>m<\/i>\n                    \u2010Xylene to Xylenols With Co\u2010Production of Hydrogen"],"prefix":"10.1002","volume":"65","author":[{"given":"Zhuizhui","family":"Su","sequence":"first","affiliation":[{"name":"School of Environment and Energy Peking University Shenzhen Graduate School  Shenzhen Guangdong People's Republic of China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yonghua","family":"Tang","sequence":"additional","affiliation":[{"name":"School of Physics and Optoelectronics Xiangtan University  Xiangtan Hunan 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