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Here, the <jats:italic>e<jats:sub>g<\/jats:sub><\/jats:italic> fillings of Ni<jats:sub>Oh<\/jats:sub> and Fe<jats:sub>Oh<\/jats:sub> in NiFe<jats:sub>2<\/jats:sub>O<jats:sub>4<\/jats:sub>\u2010based spinel are controllably regulated by introducing an external radical of catalytically inactive MoS<jats:italic><jats:sub>x<\/jats:sub><\/jats:italic> as an electron acceptor via a novel ultrasonic anchored pyrolysis strategy. The electron occupied in <jats:italic>e<jats:sub>g<\/jats:sub><\/jats:italic> orbit of M<jats:sub>Oh<\/jats:sub> emigrates with the amount of Mo\uf8ffS hanging on the apical of octahedral sites, and results in a salutary transition from high to medium <jats:italic>e<jats:sub>g<\/jats:sub><\/jats:italic> occupancy state, as confirmed by the X\u2010ray absorption spectroscopy and X\u2010ray photoelectron spectroscopy. In addition, benefiting from the abundant unsaturated S atoms in amorphous MoS<jats:italic><jats:sub>x<\/jats:sub><\/jats:italic>, the M<jats:sub>Oh<\/jats:sub> at the surface furthest activates and consequently shows a superior water oxidation performance. Density functional theory also reveals that the <jats:italic>e<jats:sub>g<\/jats:sub><\/jats:italic> fillings of Ni and Fe decrease to 1.4 and 1.2 after MoS<jats:italic><jats:sub>x<\/jats:sub><\/jats:italic> modification, which can effectively reduce the free energy of the OOH* intermediates in the oxygen evolution reaction process. This work opens an avenue for further releasing the electrocatalytic activity of octahedral sites through bridging external phases with rational electron\u2010capturing\/donating capability.<\/jats:p>","DOI":"10.1002\/smtd.202201550","type":"journal-article","created":{"date-parts":[[2023,3,17]],"date-time":"2023-03-17T11:07:42Z","timestamp":1679051262000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":17,"title":["Activating Octahedral Center in Co\u2010Doped NiFe<sub>2<\/sub>O<sub>4<\/sub> via Bridging Amorphous MoS<i><sub>x<\/sub><\/i> for Electrocatalytic Water Oxidation: A Case for <i>e<sub>g<\/sub><\/i> Orbital Regulation in Spinel Oxide"],"prefix":"10.1002","volume":"7","author":[{"given":"Lu","family":"Yao","sequence":"first","affiliation":[{"name":"State Key Laboratory of Inorganic Synthesis and Preparative Chemistry Jilin Provincial International Cooperation Key Laboratory of Advanced Inorganic Solid Functional Materials College of Chemistry Jilin University  Changchun 130012 P. 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