Alkylation of the [nido-5,6-R12C2B8H9]- anions (where R1 = H and Me) with alkyl halides (RX, where R = primary and secondary alkyls) in boiling tetrahydrofuran (THF) proceeds via unusual H2 elimination, followed by cage closure to give a series of the neutral closo-1,2-R12C2B8H7-3-R derivatives in ∼70-80% yields. In contrast, treatment of the unsubstituted [nido-5,6-C2B8H11]- anion with tert-butyl bromide (t-BuBr) led to the formation of the parent closo-1,2-C2B8H10 in >85% yield. The constitution of all compounds isolated has been confirmed unambiguously by multinuclear (11B, 1H, and 13C) nuclear magnetic resonance measurements and α-shift correlation assessments.

Institute of Inorganic Chemistry Academy of Sciences of the Czech Republic 250 68 Řež Czech Republic

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