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Of those, the bulkier 1,3,5\u2010tri\u2010<jats:italic>tert<\/jats:italic>\u2010butylbenzene (mes*) derivative [Fe(mes*)(CO)<jats:sub>2<\/jats:sub>]\u22c5<jats:sup>+<\/jats:sup> was fully characterized by XRD analysis, IR, NMR, cw\u2010EPR, M\u00f6ssbauer spectroscopy and cyclic voltammetry as the [Al(OR<jats:sup>F<\/jats:sup>)<jats:sub>4<\/jats:sub>]<jats:sup>\u2212<\/jats:sup> (R<jats:sup>F<\/jats:sup>=C(CF<jats:sub>3<\/jats:sub>)<jats:sub>3<\/jats:sub>) salt. Chemical electronation, i.\u2009e., the single electron reduction, with decamethylferrocene generates neutral [Fe(mes*)(CO)<jats:sub>2<\/jats:sub>], whereas further deelectronation under CO\u2010pressure leads to a dicationic three\u2010legged [Fe(mes*)(CO)<jats:sub>3<\/jats:sub>]<jats:sup>2+<\/jats:sup> salt with [Al(OR<jats:sup>F<\/jats:sup>)<jats:sub>4<\/jats:sub>]<jats:sup>\u2212<\/jats:sup> counterion. The full substitution of the carbonyl ligands in [Fe(CO)<jats:sub>5<\/jats:sub>]\u22c5<jats:sup>+<\/jats:sup>[Al(OR<jats:sup>F<\/jats:sup>)<jats:sub>4<\/jats:sub>]<jats:sup>\u2212<\/jats:sup> mainly resulted in disproportionation reactions, giving solid Fe(0) and the dicationic bis\u2010arene salts [Fe(\u03b7<jats:sup>6<\/jats:sup>\u2010arene)<jats:sub>2<\/jats:sub>]<jats:sup>2+<\/jats:sup>([Al(OR<jats:sup>F<\/jats:sup>)<jats:sub>4<\/jats:sub>]<jats:sup>\u2212<\/jats:sup>)<jats:sub>2<\/jats:sub> (arene=1,3,5\u2010trimethylbenzene, benzene and fluorobenzene). Only by employing the very large fluoride bridged anion [F\u2010{Al(OR<jats:sup>F<\/jats:sup>)<jats:sub>3<\/jats:sub>}<jats:sub>2<\/jats:sub>]<jats:sup>\u2212<\/jats:sup>, it was possible to isolate an open shell bis\u2010arene cation salt [Fe(C<jats:sub>6<\/jats:sub>H<jats:sub>6<\/jats:sub>)<jats:sub>2<\/jats:sub>]\u22c5<jats:sup>+<\/jats:sup>[F\u2010{Al(OR<jats:sup>F<\/jats:sup>)<jats:sub>3<\/jats:sub>}<jats:sub>2<\/jats:sub>]<jats:sup>\u2212<\/jats:sup>. The highly reactive cation was characterized by XRD analysis, cw\u2010EPR, M\u00f6ssbauer spectroscopy and cyclic voltammetry. The disproportionation of [Fe(C<jats:sub>6<\/jats:sub>H<jats:sub>6<\/jats:sub>)<jats:sub>2<\/jats:sub>]\u22c5<jats:sup>+<\/jats:sup> salts to give solid Fe(0) and [Fe(C<jats:sub>6<\/jats:sub>H<jats:sub>6<\/jats:sub>)<jats:sub>2<\/jats:sub>]<jats:sup>2+<\/jats:sup> salts was analyzed by a suitable cycle, revealing that the thermodynamic driving force for the disproportionation is a function of the size of the anion used and the polarity of the solvent.<\/jats:p>","DOI":"10.1002\/chem.202400105","type":"journal-article","created":{"date-parts":[[2024,2,1]],"date-time":"2024-02-01T08:49:21Z","timestamp":1706777361000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":6,"title":["From the Iron Pentacarbonyl Cation to Heteroleptic \u03b7<sup>6<\/sup>\u2010arene Carbonyls and bis\u2010\u03b7<sup>6<\/sup>\u2010arene 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