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Saintdenis, Tyler G.
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article
Dimetalloylene (M‐E‐M) Complexes of Heavier Main Group Elements Ge, Sn, Pb, Bi via Cleavage of E‐X Bonds (X=N(SiMe<sub>3</sub>)<sub>2</sub>, O<i>t</i>Bu) with an Iridium Hydride
Abstract
<jats:title>Abstract</jats:title><jats:p>Reactions of the Ir<jats:sup>V</jats:sup> hydride [<jats:sup>Me</jats:sup>BDI<jats:sup>Dipp</jats:sup>]IrH<jats:sub>4</jats:sub> {BDI=(Dipp)NC(Me)CH(Me)CN(Dipp); Dipp=2,6‐<jats:italic>i</jats:italic>Pr<jats:sub>2</jats:sub>C<jats:sub>6</jats:sub>H<jats:sub>3</jats:sub>} with E[N(SiMe<jats:sub>3</jats:sub>)<jats:sub>2</jats:sub>]<jats:sub>2</jats:sub> (E=Sn, Pb) afforded the unusual dimeric dimetallotetrylenes ([<jats:sup>Me</jats:sup>BDI<jats:sup>Dipp</jats:sup>]IrH)<jats:sub>2</jats:sub>(<jats:italic>μ</jats:italic><jats:sub>2</jats:sub>‐E)<jats:sub>2</jats:sub> in good yields. Moreover, ([<jats:sup>Me</jats:sup>BDI<jats:sup>Dipp</jats:sup>]IrH)<jats:sub>2</jats:sub>(<jats:italic>μ</jats:italic><jats:sub>2</jats:sub>‐Ge)<jats:sub>2</jats:sub> was formed in situ from thermal decomposition of [<jats:sup>Me</jats:sup>BDI<jats:sup>Dipp</jats:sup>]Ir(H)<jats:sub>2</jats:sub>Ge[N(SiMe<jats:sub>3</jats:sub>)<jats:sub>2</jats:sub>]<jats:sub>2</jats:sub>. These reactions are accompanied by liberation of HN(SiMe<jats:sub>3</jats:sub>)<jats:sub>2</jats:sub> and H<jats:sub>2</jats:sub> through the apparent cleavage of an E−N(SiMe<jats:sub>3</jats:sub>)<jats:sub>2</jats:sub> bond by Ir−H. In a reversal of this process, ([<jats:sup>Me</jats:sup>BDI<jats:sup>Dipp</jats:sup>]IrH)<jats:sub>2</jats:sub>(<jats:italic>μ</jats:italic><jats:sub>2</jats:sub>‐E)<jats:sub>2</jats:sub> reacted with excess H<jats:sub>2</jats:sub> to regenerate [<jats:sup>Me</jats:sup>BDI<jats:sup>Dipp</jats:sup>]IrH<jats:sub>4</jats:sub>. Varying the concentrations of reactants led to formation of the trimeric ([<jats:sup>Me</jats:sup>BDI<jats:sup>Dipp</jats:sup>]IrH<jats:sub>2</jats:sub>)<jats:sub>3</jats:sub>(<jats:italic>μ</jats:italic><jats:sub>2</jats:sub>‐E)<jats:sub>3</jats:sub>. The further scope of this synthetic route was investigated with group 15 amides, and ([<jats:sup>Me</jats:sup>BDI<jats:sup>Dipp</jats:sup>]IrH)<jats:sub>2</jats:sub>(<jats:italic>μ</jats:italic><jats:sub>2</jats:sub>‐Bi)<jats:sub>2</jats:sub> was prepared by the reaction of [<jats:sup>Me</jats:sup>BDI<jats:sup>Dipp</jats:sup>]IrH<jats:sub>4</jats:sub> with Bi(NMe<jats:sub>2</jats:sub>)<jats:sub>3</jats:sub> or Bi(O<jats:italic>t</jats:italic>Bu)<jats:sub>3</jats:sub> to afford the first example of a “naked” two‐coordinate Bi atom bound exclusively to transition metals. A viable mechanism that accounts for the formation of these products is proposed. Computational investigations of the Ir<jats:sub>2</jats:sub>E<jats:sub>2</jats:sub> (E=Sn, Pb) compounds characterized them as open‐shell singlets with confined nonbonding lone pairs at the E centers. In contrast, Ir<jats:sub>2</jats:sub>Bi<jats:sub>2</jats:sub> is characterized as having a closed‐shell singlet ground state.</jats:p>