Solvothermal synthesis and formation mechanism of lithium dodecaborate
(2026) Chemical Synthesis — Vol. 6, p. 56 (2026)
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- Metal dodecaborates, particularly lithium dodecaborate (Li2B12H12), are promising ionic conductors, but their broader application is hindered by complex synthesis. Here, we report a facile solvothermal synthesis of Li2B12H12 via the reaction of lithium borohydride (LiBH4) with borane dimethyl sulfide complex (DMS·BH3) in glyme solvents. This synthesis can be conveniently performed either in a Schlenk flask (with or without reflux) or in an autoclave, demonstrating high yields (up to 96%) and excellent purity. The enclosed system provided by the autoclave was shown to be more favorable for the synthesis of the B12H122- anion. A detailed mechanistic investigation utilizing 11B nuclear magnetic resonance (11B NMR) spectroscopy revealed the stepwise formation of B2H7-, B3H8-, B9H14-, B11H14-, and B11H132- intermediates. This synthetic strategy was successfully extended to other alkali metal dodecaborates (Na, K), and their glyme-coordinated complexes were characterized by single-crystal X-ray diffraction. Furthermore, we introduce a solvent-exchange approach using weakly coordinating solvents such as dimethyl sulfoxide (DMSO) or water, enabling simple and efficient desolvation, thereby offering a practical new approach to obtain anhydrous metal dodecaborates.
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Wang, J., Steenhaut, T., Robeyns, K., Li, H.-W., & Filinchuk, Y. (2026). Solvothermal synthesis and formation mechanism of lithium dodecaborate. Chemical Synthesis, 6, 56. https://doi.org/10.20517/cs.2026.01 (Original work published 2026)