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Here, we successfully designed a series of mortise\u2010and\u2010tenon molecular joint COFs by rationally engineering a twisted tetraphthaldehyde ligand bearing \u03c0\u2010conjugated \u201cclips\u201d. Stepwise extension of the \u201cclips\u201d enables topological evolution from 2D to twofold interpenetrated 3D, and ultimately to noninterpenetrated 3D structure. Notably, DHP\u2010CuPor\u2010COF with noninterpenetrated 3D structure amplifies light\u2010harvesting efficiency and substrate accessibility, enabling superior photothermal conversion and catalytic performance over its 2D and twofold interpenetrated 3D counterparts. To the best of our knowledge, it delivers highly efficient photothermal\u2010catalytic C\u2500X (X = O, S) bond formation for selective transformation of phenolic compounds via cross\u2010dehydrogenative coupling (CDC) reactions (conv., &gt;90% and yield, &gt;80%), markedly outperforming conventional thermal catalysis. The high efficiency arises from the synergistic of open 3D channels, abundant Cu\u2010porphyrin active sites and strong photothermal effect. This work provides an innovative strategy to tune the topological chemistry of COFs for advanced photocatalytic applications.<\/jats:p>","DOI":"10.1002\/anie.7484294","type":"journal-article","created":{"date-parts":[[2026,10,10]],"date-time":"2026-10-10T02:59:32Z","timestamp":1791601172000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Mortise\u2010and\u2010Tenon Molecular Joint Covalent Organic Frameworks With Tunable Topology for Photothermal\u2010Catalytic Cross\u2010Dehydrogenative Coupling"],"prefix":"10.1002","author":[{"given":"Xiaofei","family":"Chen","sequence":"first","affiliation":[{"name":"Guangdong Provincial Key Laboratory of Carbon Dioxide Resource Utilization School of Chemistry South China Normal University  P.R. China"},{"name":"Department Key Laboratory for Special Functional Materials of Ministry of Education, National &amp; Local Joint Engineering Research Center for High\u2010efficiency Display and Lighting Technology, School of Nanoscience and Materials Engineering Henan University  Zhengzhou P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Qianqian","family":"Li","sequence":"additional","affiliation":[{"name":"Department Key Laboratory for Special Functional Materials of Ministry of Education, National &amp; Local Joint Engineering Research Center for High\u2010efficiency Display and Lighting Technology, School of Nanoscience and Materials Engineering Henan University  Zhengzhou P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0000-8647-6517","authenticated-orcid":false,"given":"Wenhai","family":"Feng","sequence":"additional","affiliation":[{"name":"Guangdong Provincial Key Laboratory of Carbon Dioxide Resource Utilization School of Chemistry South China Normal University  P.R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jiayong","family":"Weng","sequence":"additional","affiliation":[{"name":"Guangdong Provincial Key Laboratory of Carbon Dioxide Resource Utilization School of Chemistry South China Normal University  P.R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Haotao","family":"Yang","sequence":"additional","affiliation":[{"name":"Guangdong Provincial Key Laboratory of Carbon Dioxide Resource Utilization School of Chemistry South China Normal University  P.R. 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