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Herein, by strategically balancing the solubility of aniline\u2010functionalized arsenic polyoxomolybdate (AsPOM) with the organic linker of 1,4\u2010bi(3\u2010dimethylamino\u20101\u2010oxoprop\u20102\u2010enyl)benzene (BDOEB), a new 3D covalent AsPOM\u2010organic polymer, termed POF\u20102, was successfully prepared. Its short\u2010 to medium\u2010range ordered structure was resolved using the advanced total scattering atomic pair distribution function (PDF). The unique architecture of POF\u20102 synergistically combines the strong oxidative capability of AsPOM with the tunable light absorption and oxygen activation ability of organic monomers, narrowing the bandgap from 3.13\u00a0eV (AsPOM) to 2.28\u00a0eV (POF\u20102) and extending light absorption to 575\u00a0nm. Under ambient conditions with low\u2010energy visible\u2010light irradiation (10\u00a0W LED), POF\u20102 exhibits exceptional photocatalytic performance in aromatic C\u2500H bromination and [3+2] cycloaddition reactions, achieving\u00a0&gt;99% conversion and\u00a0&gt;99% selectivity. Mechanistic studies reveal that the well\u2010defined donor\u2013acceptor (D\u2013A) structure of POF\u20102 facilitates rapid hole (h\n                    <jats:sup>+<\/jats:sup>\n                    )\u2010mediated C\u2500H activation on AsPOM nodes and selective\n                    <jats:sup>1<\/jats:sup>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    generation on BDOEB linkers, avoiding nonproductive substrate mineralization. This work not only demonstrates a new 3D covalent AsPOM\u2010organic polymer for C\u2500H functionalization but also provides a blueprint for designing molecularly precise, multifunctional photocatalysts for sustainable organic synthesis.\n                  <\/jats:p>","DOI":"10.1002\/anie.202513712","type":"journal-article","created":{"date-parts":[[2025,7,30]],"date-time":"2025-07-30T05:50:22Z","timestamp":1753854622000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":7,"title":["3D Covalent Arsenic Polyoxomolybdate\u2010Organic Polymer with Ultrahigh Photocatalytic Oxidative Ability for Aromatic C\u2500H Activation"],"prefix":"10.1002","volume":"64","author":[{"given":"Yingnan","family":"Zhao","sequence":"first","affiliation":[{"name":"Key Laboratory of Automobile Materials (Jilin University), Ministry of Education, School of Materials Science and Engineering Jilin University  Changchun 130012 China"},{"name":"Key Laboratory of Polyoxometalate and Reticular Material Chemistry of Ministry of Education, Faculty of Chemistry Northeast Normal University  Changchun 130024 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Liang","family":"Pang","sequence":"additional","affiliation":[{"name":"Key Laboratory of Automobile Materials (Jilin University), Ministry of Education, School of Materials Science and Engineering Jilin University  Changchun 130012 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Tianyu","family":"Qiu","sequence":"additional","affiliation":[{"name":"Key Laboratory of Polyoxometalate and Reticular Material Chemistry of Ministry of Education, Faculty of Chemistry Northeast Normal University  Changchun 130024 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Feiyang","family":"Yu","sequence":"additional","affiliation":[{"name":"Key Laboratory of Polyoxometalate and Reticular Material Chemistry of Ministry of Education, Faculty of Chemistry Northeast Normal University  Changchun 130024 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zhongling","family":"Lang","sequence":"additional","affiliation":[{"name":"Key Laboratory of Polyoxometalate and Reticular Material Chemistry of Ministry of Education, Faculty of Chemistry Northeast Normal University  Changchun 130024 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Gao\u2010Feng","family":"Han","sequence":"additional","affiliation":[{"name":"Key Laboratory of Automobile Materials (Jilin University), Ministry of Education, School of Materials Science and Engineering Jilin University  Changchun 130012 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yangguang","family":"Li","sequence":"additional","affiliation":[{"name":"Key Laboratory of Polyoxometalate and Reticular Material Chemistry of Ministry of Education, Faculty of Chemistry Northeast Normal University  Changchun 130024 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