Synthesis and Characterization of a Rhodium(I) σ-Alkane Complex in the Solid State

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Science  28 Sep 2012:
Vol. 337, Issue 6102, pp. 1648-1651
DOI: 10.1126/science.1225028

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Transition metal–alkane complexes—termed σ-complexes because the alkane donates electron density to the metal from a σ-symmetry carbon–hydrogen (C–H) orbital—are key intermediates in catalytic C–H activation processes, yet these complexes remain tantalizingly elusive to characterization in the solid state by single-crystal x-ray diffraction techniques. Here, we report an approach to the synthesis and characterization of transition metal–alkane complexes in the solid state by a simple gas-solid reaction to produce an alkane σ-complex directly. This strategy enables the structural determination, by x-ray diffraction, of an alkane (norbornane) σ-bound to a d8–rhodium(I) metal center, in which the chelating alkane ligand is coordinated to the pseudosquare planar metal center through two σ-C–H bonds.

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