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Herein, we present a novel dual\u2010vacancy defective hollow heterostructure derived from Metal\u2013Organic Frameworks, featuring abundant surface hydroxyl groups and S\/O vacancies, for photothermal\u2010promoted methanol solution reforming into hydrogen. The [In<jats:sub>2<\/jats:sub>S<jats:sub>3\u2010x<\/jats:sub>\/In<jats:sub>2<\/jats:sub>O<jats:sub>3\u2010x<\/jats:sub>](OH)<jats:sub>y<\/jats:sub> exhibits exceptional photothermal H<jats:sub>2<\/jats:sub> evolution activity, achieving a production rate of 215.2 mmolg<jats:sub>cat<\/jats:sub><jats:sup>\u22121<\/jats:sup>h<jats:sup>\u22121<\/jats:sup>, 16\u2010fold higher than its thermocatalytic activity, with an apparent quantum efficiency of 66.8\u2009% at 365\u2005nm and solar\u2010to\u2010hydrogen efficiency (STH) of 1.1\u2009% under AM 1.5G simulated solar illumination, and excellent durability over 82\u2005h, cumulating 2.61\u00d710<jats:sup>3<\/jats:sup> mmolg<jats:sub>cat<\/jats:sub><jats:sup>\u22121<\/jats:sup>. The synergistic effects of dual\u2010vacancies and the hollow heterostructure significantly enhance the photothermal effect, lowering the activation energy barrier for methanol\/water, enabling H<jats:sub>2<\/jats:sub> production at temperatures even as 80\u2009\u00b0C under non\u2010alkaline conditions. Furthermore, the incorporated surface hydroxyl groups facilitate the generation of active surface hydroxyls from water, further driving activation and cleavage of C\u2212H bonds in methanol, thereby markedly reducing the apparent reaction activation energy by 12.5\u2009%. This work provides a new strategy for effective H<jats:sub>2<\/jats:sub> production from aqueous methanol reforming under mild conditions, holding great promise for energy\u2010demanding industrial applications.<\/jats:p>","DOI":"10.1002\/anie.202423269","type":"journal-article","created":{"date-parts":[[2025,1,27]],"date-time":"2025-01-27T05:08:06Z","timestamp":1737954486000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":23,"title":["Surface Hydroxylated S\/O Dual\u2010Vacancy S\u2010Scheme Hollow [In<sub>2<\/sub>S<sub>3\u2010x<\/sub>\/In<sub>2<\/sub>O<sub>3\u2010x<\/sub>](OH)<sub>y<\/sub> Heterojunction for Photothermal\u2010promoted Low\u2010Temperature Methanol\/Water Reforming into Hydrogen"],"prefix":"10.1002","volume":"64","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-6362-6479","authenticated-orcid":false,"given":"Yunhong","family":"Pi","sequence":"first","affiliation":[{"name":"School of Chemical Engineering and Light Industry and Guangzhou Key Laboratory of Clean Transportation Energy and Chemistry Guangdong University of Technology  Guangzhou 510006 P. 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