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However, the spatial confinement of the dehydrogenation and proton reduction processes generally induces strong Coulombic coupling of photoinduced charges, resulting in frustrated reaction kinetics. In this study, we develop a defect\u2010cluster synergistic strategy to overcome the above challenges. We construct Mo\n                    <jats:italic>\n                      <jats:sup>\u03b4<\/jats:sup>\n                    <\/jats:italic>\n                    <jats:sup>+<\/jats:sup>\n                    substitution\u2010Zn vacancy (Mo\n                    <jats:sub>Zn<\/jats:sub>\n                    <jats:italic>V<\/jats:italic>\n                    <jats:sub>Zn<\/jats:sub>\n                    ) defect clusters in Zn\n                    <jats:sub>0.3<\/jats:sub>\n                    Cd\n                    <jats:sub>0.7<\/jats:sub>\n                    S via in situ charge compensation. The quasi\u2010continuous defect states arising from these associated point defects enable the persistent decoupling of 56.3% of the photoinduced charges with a lifetime of 2542.9\u00a0ps. The Mo\n                    <jats:sub>Zn<\/jats:sub>\n                    <jats:italic>V<\/jats:italic>\n                    <jats:sub>Zn<\/jats:sub>\n                    defect clusters also serve as synergistic active sites, simultaneously facilitating hole\u2010mediated dehydrogenation and the entire electron\u2010mediated sequence from proton\u2010coupled electron transfer to surface\u2010adsorbed hydrogen transfer. Consequently, a lignin\u2010derived aromatic diol achieves 90.4% conversion in 1\u00a0h, yielding hydrogen and value\u2010added aromatic acyloin at rates of 7.4 and 7.3 mmol\u00b7g\n                    <jats:sup>\u22121<\/jats:sup>\n                    \u00b7h\n                    <jats:sup>\u22121<\/jats:sup>\n                    , respectively. This study offers an integrated strategy that simultaneously decouples photoinduced charges and engineers catalytic sites in spatially confined photoredox reactions, opening up an alternative avenue for the sustainable and versatile valorization of biomass resources.\n                  <\/jats:p>","DOI":"10.1002\/anie.5837873","type":"journal-article","created":{"date-parts":[[2026,10,2]],"date-time":"2026-10-02T07:41:38Z","timestamp":1790926898000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Dehydrogenation of Biomass\u2010Derived Aromatic Diol to Value\u2010Added Acyloin and Hydrogen Production Over Zn\n                    <sub>0.3<\/sub>\n                    Cd\n                    <sub>0.7<\/sub>\n                    S Solid Solution With Defect Clusters and Its Photocatalytic Mechanism"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0009-0005-1531-4891","authenticated-orcid":false,"given":"Sijie","family":"Wan","sequence":"first","affiliation":[{"name":"State Key Laboratory of Advanced Technology for Materials Synthesis and Processing Wuhan University of Technology  Wuhan Hubei P. 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