Abstract
New anionic ruthenium(II) aluminohydrides were synthesized from [Cp*RuCl](4), LiAlH4, and lithium alkyls. The reaction of [Cp*RuCl](4) with 8 equiv of LiAlH4 afforded the lithium salt [Li(DME)(3)][CP*Ru-2(2)(mu-H)(mu-AlH4)(2)] (1) in 65% isolated yield. Reactions of [Cp*RuCl](4), LiAlH4, and RLi (R = Me, Et, iPr, nBu) in THF yielded the new compounds [Li-5(THF)(2)Cp*6Ru6Al4Me4H19] (2) and ...
Abstract
New anionic ruthenium(II) aluminohydrides were synthesized from [Cp*RuCl](4), LiAlH4, and lithium alkyls. The reaction of [Cp*RuCl](4) with 8 equiv of LiAlH4 afforded the lithium salt [Li(DME)(3)][CP*Ru-2(2)(mu-H)(mu-AlH4)(2)] (1) in 65% isolated yield. Reactions of [Cp*RuCl](4), LiAlH4, and RLi (R = Me, Et, iPr, nBu) in THF yielded the new compounds [Li-5(THF)(2)Cp*6Ru6Al4Me4H19] (2) and [Li-2(THF)(2)Cp*RuAl2R2H7)](2) (3-5, R = Et, iPr, tBu). The compounds were characterized by single-crystal X-ray crystallography, multinuclear liquid and solid-state NMR spectroscopy, IR spectroscopy, and microanalysis. The molecular structures of 1-5 display novel anionic ruthenium(II) aluminate frameworks. In the case of 2-5, these anions associate into unusual cage structures via Li-H interactions in the solid state. Variable-temperature H-1 and Li-7 NMR studies on the fluxional complex 5 in deuterated toluene show that the cage structure of this compound is retained at low temperature in solution.
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