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The inherent thermal instability of high\u2010valent Fe<jats:sup>IV<\/jats:sup> compounds without \u03c0\u2010donor ligands (such as oxido (O<jats:sup>2\u2212<\/jats:sup>), imido (RN<jats:sup>2\u2212<\/jats:sup>) or nitrido (N<jats:sup>3\u2212<\/jats:sup>)) makes their isolation and structural characterization a very challenging task. We report the synthesis of an Fe<jats:sup>IV<\/jats:sup> cyanide complex [(N<jats:sub>3<\/jats:sub>N\u2032)FeCN] (<jats:bold>4<\/jats:bold>) by two consecutive single electron transfer (SET) processes from Fe<jats:sup>II<\/jats:sup> precursor [(N<jats:sub>3<\/jats:sub>N\u2032)FeLi(THF)] (<jats:bold>1<\/jats:bold>) with cyanobenziodoxolone (CBX). The Fe<jats:sup>IV<\/jats:sup> complex can also be prepared by reaction of [(N<jats:sub>3<\/jats:sub>N\u2032)Fe<jats:sup>III<\/jats:sup>] (<jats:bold>3<\/jats:bold>) with CBX. In contrast, the oxidation of Fe<jats:sup>II<\/jats:sup> with 1\u2010cyano\u20103,3\u2010dimethyl\u20103\u2010(1H)\u20101,2\u2010benziodoxole (CDBX) enables the preparation of Fe<jats:sup>III<\/jats:sup> cyanide complex [(N<jats:sub>3<\/jats:sub>N\u2032)Fe<jats:sup>III<\/jats:sup>(CN)(Li)(THF)<jats:sub>3<\/jats:sub>] (<jats:bold>2\u2010Li<jats:sup>THF<\/jats:sup><\/jats:bold>). Complexes <jats:bold>4<\/jats:bold> and <jats:bold>2\u2010Li<jats:sup>THF<\/jats:sup><\/jats:bold> have been structurally characterized by single crystal X\u2010ray diffraction and their electronic structure has been examined by M\u00f6ssbauer, EPR spectroscopy, and computational analyses.<\/jats:p>","DOI":"10.1002\/anie.202201699","type":"journal-article","created":{"date-parts":[[2022,3,14]],"date-time":"2022-03-14T03:05:08Z","timestamp":1647227108000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":16,"title":["Synthesis of Fe<sup>III<\/sup> and Fe<sup>IV<\/sup> Cyanide Complexes Using Hypervalent Iodine Reagents as Cyano\u2010Transfer One\u2010Electron Oxidants"],"prefix":"10.1002","volume":"61","author":[{"given":"Charafa","family":"Souilah","sequence":"first","affiliation":[{"name":"Fachbereich Chemie Philipps-Universit\u00e4t Marburg  Hans-Meerwein-Stra\u00dfe 4 35043 Marburg Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7406-6633","authenticated-orcid":false,"given":"Sergio A. V.","family":"Jannuzzi","sequence":"additional","affiliation":[{"name":"Max Planck Institute for Chemical Energy Conversion (MPI CEC)  Stiftstra\u00dfe 34\u201336 45470 M\u00fclheim an der Ruhr Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Derya","family":"Demirbas","sequence":"additional","affiliation":[{"name":"Max Planck Institute for Chemical Energy Conversion (MPI CEC)  Stiftstra\u00dfe 34\u201336 45470 M\u00fclheim an der Ruhr Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Sergei","family":"Ivlev","sequence":"additional","affiliation":[{"name":"Fachbereich Chemie Philipps-Universit\u00e4t Marburg  Hans-Meerwein-Stra\u00dfe 4 35043 Marburg Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8174-8488","authenticated-orcid":false,"given":"Marcel","family":"Swart","sequence":"additional","affiliation":[{"name":"ICREA  Pg. Llu\u00eds Companys 23 08010 Barcelona Spain"},{"name":"Institut de Qu\u00edmica Computacional i Cat\u00e0lisi, Facultat de Ci\u00e8ncies Universitat de Girona  c\/ M.A. Capmany 69 17003 Girona Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-5196-3400","authenticated-orcid":false,"given":"Serena","family":"DeBeer","sequence":"additional","affiliation":[{"name":"Max Planck Institute for Chemical Energy Conversion (MPI CEC)  Stiftstra\u00dfe 34\u201336 45470 M\u00fclheim an der Ruhr Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-6989-1751","authenticated-orcid":false,"given":"Alicia","family":"Casitas","sequence":"additional","affiliation":[{"name":"Fachbereich Chemie Philipps-Universit\u00e4t Marburg  Hans-Meerwein-Stra\u00dfe 4 35043 Marburg Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2022,3,29]]},"reference":[{"key":"e_1_2_7_1_1","unstructured":"\u00a0"},{"key":"e_1_2_7_2_2","doi-asserted-by":"publisher","DOI":"10.1021\/acs.chemrev.5b00547"},{"key":"e_1_2_7_3_2","doi-asserted-by":"publisher","DOI":"10.1021\/acs.accounts.7b00148"},{"key":"e_1_2_7_4_2","doi-asserted-by":"publisher","DOI":"10.1021\/acs.accounts.8b00468"},{"key":"e_1_2_7_5_1","unstructured":"\u00a0"},{"key":"e_1_2_7_6_2","doi-asserted-by":"publisher","DOI":"10.1002\/anie.201108267"},{"key":"e_1_2_7_6_3","doi-asserted-by":"publisher","DOI":"10.1002\/ange.201108267"},{"key":"e_1_2_7_7_2","doi-asserted-by":"publisher","DOI":"10.1021\/ja402082p"},{"key":"e_1_2_7_8_2","doi-asserted-by":"publisher","DOI":"10.1002\/anie.201309791"},{"key":"e_1_2_7_8_3","doi-asserted-by":"publisher","DOI":"10.1002\/ange.201309791"},{"key":"e_1_2_7_9_2","doi-asserted-by":"publisher","DOI":"10.1038\/nature14127"},{"key":"e_1_2_7_10_2","doi-asserted-by":"publisher","DOI":"10.1002\/chem.201406333"},{"key":"e_1_2_7_11_2","doi-asserted-by":"publisher","DOI":"10.1021\/acscentsci.6b00214"},{"key":"e_1_2_7_12_2","doi-asserted-by":"publisher","DOI":"10.1021\/jacs.6b00869"},{"key":"e_1_2_7_13_2","doi-asserted-by":"publisher","DOI":"10.1002\/anie.201507550"},{"key":"e_1_2_7_13_3","doi-asserted-by":"publisher","DOI":"10.1002\/ange.201507550"},{"key":"e_1_2_7_14_2","doi-asserted-by":"publisher","DOI":"10.1002\/chem.201704499"},{"key":"e_1_2_7_15_2","doi-asserted-by":"publisher","DOI":"10.1021\/jacs.1c05881"},{"key":"e_1_2_7_16_1","unstructured":"\u00a0"},{"key":"e_1_2_7_17_2","doi-asserted-by":"publisher","DOI":"10.1021\/ic000502d"},{"key":"e_1_2_7_18_2","doi-asserted-by":"publisher","DOI":"10.1126\/science.299.5609.1037"},{"key":"e_1_2_7_19_2","doi-asserted-by":"publisher","DOI":"10.1002\/anie.200390036"},{"key":"e_1_2_7_19_3","doi-asserted-by":"publisher","DOI":"10.1002\/ange.200390004"},{"key":"e_1_2_7_20_2","doi-asserted-by":"publisher","DOI":"10.1002\/anie.200602799"},{"key":"e_1_2_7_20_3","doi-asserted-by":"publisher","DOI":"10.1002\/ange.200602799"},{"key":"e_1_2_7_21_2","doi-asserted-by":"publisher","DOI":"10.1002\/anie.200900863"},{"key":"e_1_2_7_21_3","doi-asserted-by":"publisher","DOI":"10.1002\/ange.200900863"},{"key":"e_1_2_7_22_2","doi-asserted-by":"publisher","DOI":"10.1021\/jacs.7b04695"},{"key":"e_1_2_7_23_2","doi-asserted-by":"publisher","DOI":"10.1039\/C9SC02526J"},{"key":"e_1_2_7_24_2","doi-asserted-by":"publisher","DOI":"10.1021\/jacs.0c03085"},{"key":"e_1_2_7_25_1","unstructured":"\u00a0"},{"key":"e_1_2_7_26_2","volume-title":"Encyclopedia of Inorganic and Bioinorganic Chemistry","author":"Klein J. 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