fig5

Figure 5. (A) Proton-coupled ¹¹B NMR spectra of aliquots taken from a reaction mixture containing LiBH₄ and DMS·BH₃ in diglyme at 120 °C at different time intervals (t = 0 h was sampled before heating the mixture; intensities were normalized to the most intense signal); (B) Proposed sequence for the stepwise formation of B₁₂H₁₂^2- from BH₄^-; (C) Proton-decoupled (black) and -coupled (red) ¹¹B NMR spectra of the diethyl ether layer after liquid–liquid extraction of an aqueous solution of diglyme-solvated Li₂B₁₂H₁₂; (D) Proton-coupled ¹¹B NMR spectra of reaction mixtures containing LiB₁₁H₁₄ and either DMS·BH₃ or LiBH₄ in diglyme. ¹¹B NMR: ¹¹B nuclear magnetic resonance; LiBH₄: lithium borohydride; DMS·BH₃: borane dimethyl sulfide complex; Li₂B₁₂H₁₂: lithium dodecaborate.