| Summary: | The salt metathesis reaction between one equivalent of SmI<sub>2</sub>(THF)<sub>2</sub> and two equivalents of K(C<sub>5</sub>Me<sub>4</sub>H) in THF afforded single crystals of the unusual, toluene-soluble, and asymmetric bimetallic Sm(II)/Sm(II) complex, (C<sub>5</sub>Me<sub>4</sub>H)<sub>2</sub>Sm<sup>II</sup>(<i>μ-η<sup>3</sup>:η<sup>5</sup></i>-C<sub>5</sub>Me<sub>4</sub>H)Sm<sup>II</sup>(C<sub>5</sub>Me<sub>4</sub>H)(THF)<sub>2</sub>, instead of the expected product, (C<sub>5</sub>Me<sub>4</sub>H)<sub>2</sub>Sm<sup>II</sup>(THF)<sub>2</sub>. The toluene-insoluble products of this reaction can be worked up in 1,2-dimethoxyethane (DME) to provide X-ray quality crystals of the monomeric Sm(II) metallocene, (C<sub>5</sub>Me<sub>4</sub>H)<sub>2</sub>Sm<sup>II</sup>(DME). (C<sub>5</sub>Me<sub>4</sub>H)<sub>2</sub>Sm<sup>II</sup>(DME) can also be synthesized directly by the reaction between one equivalent of SmI<sub>2</sub>(THF)<sub>2</sub> and two equivalents of K(C<sub>5</sub>Me<sub>4</sub>H) in neat DME. The isolation and characterization of the bimetallic Sm(II)/Sm(II) complex provides supporting evidence for the possible oligomerization that may occur during the synthesis of Sm(II) complexes with cyclopentadienyl ligands that are less sterically bulky and less solubilizing than (C<sub>5</sub>Me<sub>5</sub>)<sup>1−</sup>.
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