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Here, we report the synthesis of a three\u2010member redox series of isostructural mononitrosylated [Fe<jats:sub>4<\/jats:sub>S<jats:sub>4<\/jats:sub>] clusters. Mononitrosylation was achieved by binding NO to a 3\u2009:\u20091 site\u2010differentiated [Fe<jats:sub>4<\/jats:sub>S<jats:sub>4<\/jats:sub>]<jats:sup>+<\/jats:sup> cluster; subsequent oxidation and reduction afforded the other members of the series. All three clusters feature a local high\u2010spin Fe<jats:sup>3+<\/jats:sup> center antiferromagnetically coupled to <jats:sup>3<\/jats:sup>[NO]<jats:sup>\u2212<\/jats:sup>. The observation of an anionic NO ligand suggests that NO binding is accompanied by formal electron transfer from the cluster to NO. Preliminary reactivity studies with the monocationic cluster demonstrate that exposure to excess NO degrades the cluster, supporting the intermediacy of mononitrosylated intermediates in NO sensing\/signaling.<\/jats:p>","DOI":"10.1002\/anie.202213032","type":"journal-article","created":{"date-parts":[[2022,10,4]],"date-time":"2022-10-04T15:35:18Z","timestamp":1664897718000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":28,"title":["The Elusive Mononitrosylated [Fe<sub>4<\/sub>S<sub>4<\/sub>] Cluster in Three Redox States"],"prefix":"10.1002","volume":"61","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-7378-2301","authenticated-orcid":false,"given":"Youngsuk","family":"Kim","sequence":"first","affiliation":[{"name":"Department of Chemistry Massachusetts Institute of Technology  77 Massachusetts Ave Cambridge MA 02139 USA"},{"name":"Department of Chemistry Pusan National University  Busan 46241 Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9249-8894","authenticated-orcid":false,"given":"Arun","family":"Sridharan","sequence":"additional","affiliation":[{"name":"Department of Chemistry Massachusetts Institute of Technology  77 Massachusetts Ave Cambridge MA 02139 USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0916-1973","authenticated-orcid":false,"given":"Daniel L. 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