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Herein, we engineered atomically exposed nickel molecular catalysts anchored on functional carbon black through tailored aromatic ligands coordination. This unique spatial coordination structure efficiently promotes the reconstruction of high\u2010valence Ni\n                    <jats:sup>III<\/jats:sup>\n                    \u2010OOH sites, which boost electrooxidation of 18 organic substrates with peak current density exceeding 800\u00a0mA cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    . Especially, the optimal electrocatalyst achieves record mass activities of 4.38 and 4.26 A mg\n                    <jats:sub>Ni<\/jats:sub>\n                    <jats:sup>\u22121<\/jats:sup>\n                    for methanol and ethylene glycol oxidation, respectively. In situ characterization and theoretical analyses elucidate that the atomically exposed Ni\n                    <jats:sup>III<\/jats:sup>\n                    \u2010OOH centers would directly adsorb organic substrates, thereby enhancing C\u2500C\/C\u2500H bonds cleavage efficiency. Meanwhile, the proton abstraction from C\u2500H bond would enable reversible redox cycling between Ni\n                    <jats:sup>II<\/jats:sup>\n                    \u2010OH and Ni\n                    <jats:sup>III<\/jats:sup>\n                    \u2010OOH, sustaining catalytic activity. This study advances the understanding of organic oxidation mechanisms and showcases the great potential of molecular complexes in electrocatalysis.\n                  <\/jats:p>","DOI":"10.1002\/anie.202509377","type":"journal-article","created":{"date-parts":[[2025,6,2]],"date-time":"2025-06-02T04:20:03Z","timestamp":1748838003000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":19,"title":["Tailoring Coordination Microenvironment of Nickel Molecular Complexes for Electrooxidation of Organic Nucleophiles"],"prefix":"10.1002","volume":"64","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-7019-677X","authenticated-orcid":false,"given":"Chengdong","family":"Yang","sequence":"first","affiliation":[{"name":"Key Laboratory for Colloid and Interface Chemistry Ministry of Education School of Chemistry and Chemical Engineering Shandong University  Jinan 250100 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Laboratory for Colloid and Interface Chemistry Ministry of Education School of Chemistry and Chemical Engineering Shandong University  Jinan 250100 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1029-3404","authenticated-orcid":false,"given":"Jintao","family":"Zhang","sequence":"additional","affiliation":[{"name":"Key Laboratory for Colloid and Interface Chemistry Ministry of Education School of Chemistry and Chemical Engineering Shandong University  Jinan 250100 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