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However, the development of electroactive and stable MOFs for electrocatalysis still faces challenges. Here, a molecularly engineered MOF system featuring a 2D coordination network based on mercaptan\u2013metal links (e.g., nickel, as for Ni(DMBD)\u2010MOF) is designed. The crystal structure is solved from microcrystals by a continuous\u2010rotation electron diffraction (cRED) technique. Computational results indicate a metallic electronic structure of Ni(DMBD)\u2010MOF due to the Ni\u2013S coordination, highlighting the effective design of the thiol ligand for enhancing electroconductivity. Additionally, both experimental and theoretical studies indicate that (DMBD)\u2010MOF offers advantages in the electrocatalytic oxygen evolution reaction (OER) over non\u2010thiol (e.g., 1,4\u2010benzene dicarboxylic acid) analog (BDC)\u2010MOF, because it poses fewer energy barriers during the rate\u2010limiting *O intermediate formation step. Iron\u2010substituted NiFe(DMBD)\u2010MOF achieves a current density of 100 mA cm<jats:sup>\u22122<\/jats:sup> at a small overpotential of 280\u00a0mV, indicating a new MOF platform for efficient OER catalysis.<\/jats:p>","DOI":"10.1002\/adma.202300945","type":"journal-article","created":{"date-parts":[[2023,3,13]],"date-time":"2023-03-13T06:19:11Z","timestamp":1678688351000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":110,"title":["Molecular Engineering of Metal\u2013Organic Frameworks as Efficient Electrochemical Catalysts for Water Oxidation"],"prefix":"10.1002","volume":"35","author":[{"given":"Yizhe","family":"Liu","sequence":"first","affiliation":[{"name":"Department of Chemistry City University of Hong Kong  Kowloon 999077 Hong Kong"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xintong","family":"Li","sequence":"additional","affiliation":[{"name":"Department of Chemistry City University of Hong Kong  Kowloon 999077 Hong Kong"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Shoufeng","family":"Zhang","sequence":"additional","affiliation":[{"name":"Department of Chemistry City University of Hong Kong  Kowloon 999077 Hong Kong"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zilong","family":"Wang","sequence":"additional","affiliation":[{"name":"Siyuan Laboratory Guangdong Provincial Engineering Technology Research Center of Vacuum Coating Technologies and New Energy Materials Department of Physics Jinan University  Guangzhou Guangdong 510632 P. 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