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Electrochemical H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    synthesis via the two\u2010electron oxygen reduction reaction (2e\n                    <jats:sup>\u2212<\/jats:sup>\n                    ORR) provides a sustainable alternative but is often hindered by sluggish charge transport and insufficient O\n                    <jats:sub>2<\/jats:sub>\n                    activation. Here, we develop a bond\u2010hybridization strategy by incorporating sp\u2010hybridized acetylene units into the vertex or linker of covalent organic frameworks (COFs). The resulting COFs feature extended \u03c0\u2010conjugation, enhanced charge delocalization, and electronically polarized pores, thereby strengthening O\n                    <jats:sub>2<\/jats:sub>\n                    adsorption and activation. Compared with sp\n                    <jats:sup>2<\/jats:sup>\n                    \u2010dominated analogues, these sp\u2010hybridized COFs show faster charge\u2010transfer kinetics, higher H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    selectivity, and improved 2e\n                    <jats:sup>\u2212<\/jats:sup>\n                    ORR activity. In a flow cell, the optimized catalyst delivers an H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    production rate of 27.8 mol g\n                    <jats:sup>\u22121<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    and a peak Faradaic efficiency of 91.7% at 150 mA cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    . Mechanistic analyses combining electronic\u2010structure calculations and in situ vibrational spectroscopy reveal that sp hybridization reshapes frontier\u2010orbital distributions and local charge density, thereby coupling framework\u2010wide charge delocalization with favorable O\n                    <jats:sub>2<\/jats:sub>\n                    adsorption and *OOH stabilization. These results establish bond hybridization as a molecular\u2010level design parameter for catalytic selectivity in COFs, extending framework engineering beyond conventional functional\u2010group and building\u2010block modification.\n                  <\/jats:p>","DOI":"10.1002\/anie.3570658","type":"journal-article","created":{"date-parts":[[2026,10,13]],"date-time":"2026-10-13T05:40:16Z","timestamp":1791870016000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Charge\u2010Delocalizing sp\u2010Hybridized COFs for Selective H\n                    <sub>2<\/sub>\n                    O\n                    <sub>2<\/sub>\n                    Electrosynthesis"],"prefix":"10.1002","author":[{"given":"Changqing","family":"Li","sequence":"first","affiliation":[{"name":"Key Laboratory of Automobile Materials of MOE and School of Materials Science and Engineering Jilin University  Changchun P.R. China"},{"name":"Department of Energy and Chemical Engineering\/Center for Dimension\u2010Controllable Organic Frameworks Ulsan National Institute of Science and Technology (UNIST)  Ulsan Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yuqiang","family":"Huang","sequence":"additional","affiliation":[{"name":"Key Laboratory of Automobile Materials of MOE and School of Materials Science and Engineering Jilin University  Changchun P.R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0001-7776-4020","authenticated-orcid":false,"given":"Zilin","family":"Lu","sequence":"additional","affiliation":[{"name":"Hubei Key Laboratory of Automotive Power Train and Electronics, School of Automotive Engineering Hubei University of Automotive Technology  Shiyan China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zhao","family":"Qiao","sequence":"additional","affiliation":[{"name":"Key Laboratory of Automobile Materials of MOE and School of Materials Science and Engineering Jilin University  Changchun P.R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yongxuan","family":"Jiang","sequence":"additional","affiliation":[{"name":"Key Laboratory of Automobile Materials of MOE and School of Materials Science and Engineering Jilin University  Changchun P.R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0002-3578-993X","authenticated-orcid":false,"given":"Zhongping","family":"Li","sequence":"additional","affiliation":[{"name":"Key Laboratory of Automobile Materials of MOE and School of Materials Science and Engineering Jilin University  Changchun P.R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7008-4938","authenticated-orcid":false,"given":"Yucheng","family":"Jin","sequence":"additional","affiliation":[{"name":"Department of Energy and Chemical Engineering\/Center for Dimension\u2010Controllable Organic Frameworks Ulsan National Institute of Science and Technology (UNIST)  Ulsan Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0005-1231-5290","authenticated-orcid":false,"given":"Siliu","family":"Lyu","sequence":"additional","affiliation":[{"name":"Hubei Key Laboratory of Automotive Power Train and Electronics, School of Automotive Engineering Hubei University of Automotive Technology  Shiyan China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0132-5611","authenticated-orcid":false,"given":"Lipeng","family":"Zhai","sequence":"additional","affiliation":[{"name":"College of Chemistry and Molecular Sciences Henan University  Kaifeng P.R. 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