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Utilizing active oxygen species (e.g., active hydroxyl (OH*) or lattice oxygen) generated at the anode during water electrolysis provides a sustainable solution to achieve electrochemical activation of the C(OH)\u2212C(OH) bond. However, elucidating the mechanisms of active oxygen species and their roles in enhancing product selectivity remains a challenge. Herein, we report a strategy to unravel the contribution of active oxygen species for C(OH)\u2212C(OH) bond cleavage during alcohols electrooxidation, revealing that lattice oxygen promotes C(OH)\u2212C(OH) bond cleavage and enhances product selectivity. We constructed NiAl\u2010LDH and Ni(Al)\u2010LDH as model catalysts, the latter derived through a \u201cnano\u2010tailoring\u201d Al\u2010leaching strategy. As a result, Ni(Al)\u2010LDH facilitates lattice oxygen formation more readily, which acts as the primary active species for C(OH)\u2212C(OH) bond cleavage and achieves \u223c90% selectivity for formic acid production in ethylene glycol oxidation reaction (EGOR). The intrinsic mechanism involves that lattice oxygen participates in EGOR via the Mars\u2010van\u2010Krevelen mechanism and specifically induces C(OH)\u2212C(OH) bond cleavage through an indirect pathway. This mechanistic insight into C(OH)\u2212C(OH) bond cleavage mediated by lattice oxygen provides a valuable reference for designing selective catalysts in alcohols electrooxidation.<\/jats:p>","DOI":"10.1002\/anie.202524156","type":"journal-article","created":{"date-parts":[[2026,1,16]],"date-time":"2026-01-16T13:17:26Z","timestamp":1768569446000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":13,"title":["Lattice Oxygen Mediated C(OH)\u2212C(OH) Bond Cleavage to Promote Alcohols Electrooxidation"],"prefix":"10.1002","volume":"65","author":[{"given":"Tian","family":"Xia","sequence":"first","affiliation":[{"name":"State Key Laboratory of Chemical Resource Engineering College of Chemistry Beijing University of Chemical Technology  Beijing 100029 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jiangrong","family":"Yang","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Chemical Resource Engineering College of Chemistry Beijing University of Chemical Technology  Beijing 100029 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yizhong","family":"Zou","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Chemical Resource Engineering College of Chemistry Beijing University of Chemical Technology  Beijing 100029 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zhenhua","family":"Li","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Chemical Resource Engineering College of Chemistry Beijing University of Chemical Technology  Beijing 100029 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6461-623X","authenticated-orcid":false,"given":"Mingfei","family":"Shao","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Chemical Resource Engineering College of Chemistry Beijing University of Chemical Technology  Beijing 100029 China"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2026,1,16]]},"reference":[{"key":"e_1_2_7_1_1","doi-asserted-by":"publisher","DOI":"10.1002\/aenm.202401061"},{"key":"e_1_2_7_2_1","doi-asserted-by":"publisher","DOI":"10.1002\/aenm.202301572"},{"key":"e_1_2_7_3_1","doi-asserted-by":"publisher","DOI":"10.1002\/adfm.202503193"},{"key":"e_1_2_7_4_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202400281"},{"key":"e_1_2_7_5_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202421240"},{"key":"e_1_2_7_6_1","doi-asserted-by":"publisher","DOI":"10.1021\/acscatal.3c05734"},{"key":"e_1_2_7_7_1","doi-asserted-by":"publisher","DOI":"10.1002\/cssc.201702075"},{"key":"e_1_2_7_8_1","first-page":"148","volume":"17","author":"Li Y.","year":"2025","journal-title":"Nanomicro. 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