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However, the structural reconstruction of NiFe catalysts during OER is not fully understood. Most existing studies implicitly assume the formation of a homogeneous NiFe (oxy)hydroxide lattice; however, the actual reconstruction process is more likely to generate structurally heterogeneous (oxy)hydroxide phases with local distortions due to the intrinsic mismatch between Fe3+\u2013O and Ni3+\u2013O bond lengths in the bulk NiFe compounds. By constructing atomically dispersed Ni and Fe active sites as precatalysts and combining them with operando spectroelectrochemical studies, we observed an unusual reconstruction pathway in which isolated Ni2+ and Fe atoms can adaptively evolve into a short-range mixed NiFe (oxy)hydroxide local structure through the formation of interconnected M-O-M\u2032 (M\/M\u2032 = Ni3+\u03b4, Fe3+) motifs during the OER. At 1.6 V vs RHE, the reconstructed \u03b3-Fe3+OOH clusters are induced to integrate into the high-valent \u03b3-Ni3+\u03b4OOH lattice, resulting in a short-range mixed NixFe1\u2013xOOH structure. This new structure is characterized by an unusually short Fe3+\u2013Ni3+\u03b4 distance of \u223c2.86 \u00c5, which is significantly shorter than the typical Fe3+-Fe3+ distance in Fe3+ (oxy)hydroxides (2.95\u20133.25 \u00c5). Interestingly, this \u201cinduction effect\u201d is absent in Co3+\u2013Fe3+ catalysts, as atomically dispersed Co3+ sites directly transition into \u03b3-Co3+OOH, which lacks structural compatibility with \u03b3-Fe3+OOH. DFT calculations reveal that the unusually short Fe3+-O bond leads to a moderate *O adsorption strength at the Fe site in the catalyst, thereby creating the most favorable conditions for the oxygen evolution reaction (OER).<\/jats:p>","DOI":"10.1021\/jacs.6c05060","type":"journal-article","created":{"date-parts":[[2026,8,4]],"date-time":"2026-08-04T13:15:47Z","timestamp":1785849347000},"page":"33089-33103","source":"Crossref","is-referenced-by-count":1,"title":["Local\nCoordination Motif Compatibility Induces the\nFormation of Shortened Fe3+\u2013O\u2013Ni3+\u03b4 Moieties as Active Sites for Highly Efficient Oxygen Evolution Reaction"],"prefix":"10.1021","volume":"148","author":[{"given":"Wenchao","family":"Wan","sequence":"first","affiliation":[{"name":"Max Planck Institute for Chemical Energy Conversion , Stiftstra\u00dfe 34\u221236 , ,","place":["Mu\u0308lheim an der Ruhr, Germany, 45470"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2100-4310","authenticated-orcid":true,"given":"Liqun","family":"Kang","sequence":"additional","affiliation":[{"name":"Max Planck Institute for Chemical Energy Conversion , Stiftstra\u00dfe 34\u221236 , ,","place":["Mu\u0308lheim an der Ruhr, Germany, 45470"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Shiqian","family":"Wei","sequence":"additional","affiliation":[{"name":"Leshan West Silicon Materials Photovoltaic New Energy Industry Technology Research Institute , ,","place":["Leshan, China, 614000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-2362-0638","authenticated-orcid":true,"given":"Alexander","family":"Schnegg","sequence":"additional","affiliation":[{"name":"Max Planck Institute for Chemical Energy Conversion , Stiftstra\u00dfe 34\u221236 , ,","place":["Mu\u0308lheim an der Ruhr, Germany, 45470"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Kaltum","family":"Abdiaziz","sequence":"additional","affiliation":[{"name":"Max Planck Institute for Chemical Energy Conversion , Stiftstra\u00dfe 34\u221236 , ,","place":["Mu\u0308lheim an der Ruhr, Germany, 45470"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3867-1910","authenticated-orcid":true,"given":"Longxiang","family":"Liu","sequence":"additional","affiliation":[{"name":"University College London , , 20 Gordon St , ,","place":["London, United Kingdom, WC1H 0AJ"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Fei","family":"Guo","sequence":"additional","affiliation":[{"name":"University College London , , 20 Gordon St , ,","place":["London, United Kingdom, WC1H 0AJ"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Christopher S.","family":"Allen","sequence":"additional","affiliation":[{"name":"Diamond Light Source Ltd , , , ,","place":["Didcot, Oxfordshire, United Kingdom, OX11 0DE"]},{"name":"University of Oxford , , Parks Road , ,","place":["Oxford, United Kingdom, OX1 3HP"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-5196-3400","authenticated-orcid":true,"given":"Serena","family":"DeBeer","sequence":"additional","affiliation":[{"name":"Max Planck Institute for Chemical Energy Conversion , Stiftstra\u00dfe 34\u221236 , ,","place":["Mu\u0308lheim an der Ruhr, Germany, 45470"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3594-6392","authenticated-orcid":true,"given":"Saskia","family":"Heumann","sequence":"additional","affiliation":[{"name":"Max Planck Institute for Chemical Energy Conversion , Stiftstra\u00dfe 34\u221236 , ,","place":["Mu\u0308lheim an der Ruhr, Germany, 45470"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,7,29]]},"reference":[{"issue":"4","key":"2026081210070601900_cit1","doi-asserted-by":"publisher","first-page":"2306108","DOI":"10.1002\/adma.202306108","article-title":"Recent Advancements\nin Electrochemical Hydrogen Production via Hybrid Water Splitting","volume":"36","author":"Qian","year":"2024","journal-title":"Adv. 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