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In this work, we design and synthesize a series of three\u2010dimensional (3D) COFs with different \u03c0\u2010extended dihydrophenazine cores to achieve superior photocatalytic performance. These 3D COFs exhibit excellent crystallinity, high surface areas, and remarkable chemical stability. More importantly, they can work as highly efficient and recyclable catalysts for photocatalytic tandem polymerization reactions using styrene and fluoroalkyl anhydrides as substrates, yielding fluoroalkylated polystyrene polymers with narrow dispersity. These COFs constitute the first examples as tandem photocatalysts toward polymerization reactions. Moreover, optimal energy level alignment and enhanced photophysical properties are identified as key factors contributing to their high efficacy. This work not only provides a viable design strategy for multifunctional COF catalysts, but also expands their utility in complex synthetic sequences involving tandem catalytic processes.<\/jats:p>","DOI":"10.1002\/anie.202523520","type":"journal-article","created":{"date-parts":[[2026,1,7]],"date-time":"2026-01-07T11:46:13Z","timestamp":1767786373000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":11,"title":["Energy Level Engineering of Dihydrophenazine\u2010Based Covalent Organic Frameworks Through \u03c0\u2010Expansion of Cores Toward Tandem Photocatalytic Polymerization"],"prefix":"10.1002","volume":"65","author":[{"given":"Sheng","family":"Niu","sequence":"first","affiliation":[{"name":"State Key Laboratory of Silicon and Advanced Semiconductor Materials Department of Polymer Science of Engineering Zhejiang University  Hangzhou 310058 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