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To achieve high activity and selectivity, various building blocks containing heteroatoms and groups linked by imine bonds were used to create catalytic COFs. However, the roles of linkages of COFs in ORR have not been investigated. In this work, the catalytic linkage engineering has been employed to modulate the catalytic behaviors. To create single catalytic sites while avoiding other possible catalytic sites, we synthesized COFs from benzene units linked by various bonds, such as imine, amide, azine, and oxazole bonds. Among these COFs, the oxazole\u2010linkage in COFs enables to catalyze the ORR with the highest activity, which achieved a half\u2010wave potential of 0.75\u2005V and a limited current density of 5.5\u2005mA\u2009cm<jats:sup>\u22122<\/jats:sup>. Moreover, the oxazole\u2010linked COF achieved a conversion frequency (TOF) value of 0.0133\u2005S<jats:sup>\u22121<\/jats:sup>, which were 1.9, 1.3, and 7.4\u2010times that of <jats:italic>azine\u2010<\/jats:italic>, <jats:italic>amide\u2010<\/jats:italic> and <jats:italic>imine<\/jats:italic>\u2010COFs, respectively. The theoretical calculation showed that the carbon atoms in oxazole linkages facilitated the formation of OOH* and promoted protonation of O* to form the OH*, thus advancing the catalytic activity. This work guides us on which linkages in COFs are suitable for ORR.<\/jats:p>","DOI":"10.1002\/anie.202304356","type":"journal-article","created":{"date-parts":[[2023,4,28]],"date-time":"2023-04-28T18:34:39Z","timestamp":1682706879000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":90,"title":["Catalytic Linkage Engineering of Covalent Organic Frameworks for the Oxygen Reduction Reaction"],"prefix":"10.1002","volume":"62","author":[{"given":"Xuewen","family":"Li","sequence":"first","affiliation":[{"name":"Shanghai Institute of Applied Physics Chinese Academy of Science  Shanghai 201210 P. R. China"},{"name":"University of Chinese Academy of Sciences  Beijing 100049 P. R. China"},{"name":"CAS Key Laboratory of Low-Carbon Conversion Science and Engineering Shanghai Advanced Research Institute (SARI) Chinese Academy of Sciences (CAS)  Shanghai 201210 P. R. 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