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In particular, the number of examples where the C\u2010based ligand is not part of the chelating ligand remains scarce. These compounds are of interest because they could pave the way to designing catalytic cycles of bond forming reactions proceeding via organoiron(IV) intermediates. Herein, we report the synthesis and characterization, including single\u2010crystal X\u2010ray diffraction, of a family of alkynylferrates(III) and Fe(IV) alkynylide complexes. The alkynylferrates(III) are formed by transmetalation of the Fe(III) precursor [(N\n                    <jats:sub>3<\/jats:sub>\n                    N\u2019)Fe\n                    <jats:sup>III<\/jats:sup>\n                    ] (N\n                    <jats:sub>3<\/jats:sub>\n                    N\u2019\n                    <jats:sup>3\u2212<\/jats:sup>\n                    is tris(N\u2010\n                    <jats:italic>tert<\/jats:italic>\n                    \u2010butyldimethylsilyl\u20102\u2010amidoethyl)amine) with lithium alkynylides, and their further one\u2010electron oxidation enables the synthesis of the corresponding Fe(IV) alkynylides. The electronic structure of this family of organometallic Fe(III) and Fe(IV) complexes has been thoroughly investigated by spectroscopic methods (EPR, NMR,\n                    <jats:sup>57<\/jats:sup>\n                    Fe M\u00f6ssbauer, X\u2010Ray absorption (XAS) and emission (XES) spectroscopies) and theoretical calculations. While alkynylferrates(III) are sluggish to engage into C\u2212C bond forming processes, the Fe(IV) alkynylides react to afford 1,3\u2010diynes at room temperature. A bimolecular reductive elimination from a bimetallic Fe(IV) intermediate to form the 1,3\u2010diynes is proposed based on the mechanistic investigations performed.\n                  <\/jats:p>","DOI":"10.1002\/anie.202421222","type":"journal-article","created":{"date-parts":[[2024,11,17]],"date-time":"2024-11-17T22:34:37Z","timestamp":1731882877000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["Synthesis of Iron(IV) Alkynylide Complexes and Their Reactivity to Form 1,3\u2010Diynes"],"prefix":"10.1002","volume":"64","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 34-36 45470 M\u00fclheim an der Ruhr Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Felix J.","family":"Becker","sequence":"additional","affiliation":[{"name":"Fachbereich Chemie Philipps-Universit\u00e4t Marburg  Hans-Meerwein-Stra\u00dfe 4 35043 Marburg Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Derya","family":"Demirbas","sequence":"additional","affiliation":[{"name":"Max-Planck-Institut f\u00fcr Kohlenforschung (MPI KOFO)  Kaiser-Wilhelm-Platz\u20051 45470 M\u00fclheim an der Ruhr Germany"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Daniel","family":"Jenisch","sequence":"additional","affiliation":[{"name":"Fachbereich Chemie Philipps-Universit\u00e4t Marburg  Hans-Meerwein-Stra\u00dfe 4 35043 Marburg 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Philipps-Universit\u00e4t Marburg  Hans-Meerwein-Stra\u00dfe 4 35043 Marburg Germany"}],"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 34-36 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 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