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Whereas carbon dioxide to CO conversion has precedent in homo\u2010 and heterogeneous catalysis, deoxygenative coupling of CO to products with C\u2212C bonds\u2014as in liquid fuels\u2014remains challenging. Here, we report coupling of two CO molecules by a diiron complex. Reduction of Fe<jats:sub>2<\/jats:sub>(CO)<jats:sub>2<\/jats:sub><jats:bold>L<\/jats:bold> (<jats:bold>2<\/jats:bold>), where <jats:bold>L<\/jats:bold><jats:sup>2\u2212<\/jats:sup> is a bis(\u03b2\u2010diketiminate) cyclophane, gives [K(THF)<jats:sub>5<\/jats:sub>][Fe<jats:sub>2<\/jats:sub>(CO)<jats:sub>2<\/jats:sub><jats:bold>L<\/jats:bold>] (<jats:bold>3<\/jats:bold>), which undergoes silylation to Fe<jats:sub>2<\/jats:sub>(CO)(COSiMe<jats:sub>3<\/jats:sub>)<jats:bold>L<\/jats:bold> (<jats:bold>4<\/jats:bold>). Subsequent C\u2010OSiMe<jats:sub>3<\/jats:sub> bond cleavage and C=C bond formation occurs upon reduction of <jats:bold>4<\/jats:bold>, yielding Fe<jats:sub>2<\/jats:sub>(\u03bc\u2010CCO)<jats:bold>L<\/jats:bold>. CO derived ligands in this series mediate weak exchange interactions with the ketenylidene affording the smallest <jats:italic>J<\/jats:italic> value, with changes to local metal ion spin states and coupling schemes (ferro\u2010 vs. antiferromagnetism) based on DFT calculations, M\u00f6ssbauer and EPR spectroscopy. Finally, reaction of <jats:bold>5<\/jats:bold> with KEt<jats:sub>3<\/jats:sub>BH or methanol releases the C<jats:sub>2<\/jats:sub>O<jats:sup>2\u2212<\/jats:sup> ligand with retention of the diiron core<\/jats:p>","DOI":"10.1002\/anie.202308813","type":"journal-article","created":{"date-parts":[[2023,8,18]],"date-time":"2023-08-18T23:58:20Z","timestamp":1692403100000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":10,"title":["Partial Deoxygenative CO Homocoupling by a Diiron Complex"],"prefix":"10.1002","volume":"62","author":[{"given":"Devender","family":"Singh","sequence":"first","affiliation":[{"name":"Center for Catalysis and Florida Center for Heterocyclic Compounds Department of Chemistry University of Florida  Gainesville FL USA"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Brian J.","family":"Knight","sequence":"additional","affiliation":[{"name":"Center for Catalysis and Florida Center for Heterocyclic Compounds Department of Chemistry University of Florida  Gainesville FL USA"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Vincent J.","family":"Catalano","sequence":"additional","affiliation":[{"name":"Department of Chemistry University of Nevada  Reno NV USA"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Ricardo","family":"Garc\u00eda\u2010Serres","sequence":"additional","affiliation":[{"name":"Universit\u00e9 Grenoble Alpes CNRS CEA IRIG Laboratoire de Chimie et Biologie des M\u00e9taux  17 rue des Martyrs 38000 Grenoble France"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Vincent","family":"Maurel","sequence":"additional","affiliation":[{"name":"Universit\u00e9 Grenoble Alpes CEA CNRS IRIG SyMMES  38000 Grenoble France"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Jean\u2010Marie","family":"Mouesca","sequence":"additional","affiliation":[{"name":"Universit\u00e9 Grenoble Alpes CEA CNRS IRIG 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