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The traditional thermal catalysis, utilizing noble metal salts or toxic solvents, generally results in relatively low atom economy or unmet sustainable development prospect. The challenge of the CDC reactions lies in the simultaneous activation of C\u2500H bonds in terminal alkynes and formation of free radical activation of tertiary amines to achieve the C\u2500C coupling, which calls for novel catalytic techniques and powerful catalysts. For the first time, in exclusively green solvent (i.e., dimethyl carbonate), full light, and air, we have developed a series of molecular junction polyoxotungstate\u2010based copper\u2010organic frameworks (i.e., Cu\u2010POMOF\u20101, Cu\u2010POMOF\u20102, and Cu\u2010POMOF\u20103), each with unique topological dimension and well\u2010regulated charge transfer ability that can be utilized in efficient photocatalytic CDC reactions. Notably, the optimal Cu\u2010POMOF\u20103 with the combination of polyoxotungstate and Cu sites within the 3D POMOF topological structure enables the simultaneous activation and C\u2500C coupling of tertiary amines and terminal alkynes with 98% yield. In addition, the reaction system enables scale\u2010up production (2.06\u00a0g in a batch experiment) and operation under natural sunlight and air.<\/jats:p>","DOI":"10.1002\/anie.202516079","type":"journal-article","created":{"date-parts":[[2025,8,22]],"date-time":"2025-08-22T12:54:50Z","timestamp":1755867290000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":22,"title":["Molecular Junction Polyoxotungstate\u2010based Copper\u2010Organic Frameworks for Photocatalytic Cross\u2010Dehydrogenative Coupling"],"prefix":"10.1002","volume":"64","author":[{"given":"Zongyin","family":"Gao","sequence":"first","affiliation":[{"name":"Shandong Provincial Key Laboratory of Chemical Energy Storage and Novel Cell Technology School of Chemistry &amp; Chemical Engineering Liaocheng University  Liaocheng Shandong 252059 P.R. 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