| Summary: | In total, three novel organic derivatives of lanthanide borohydrides, n-But<sub>4</sub>N<i>RE</i>(BH<sub>4</sub>)<sub>4</sub> (TBA<i>RE</i>B), <i>RE</i> = Ho, Tm, Yb, have been prepared utilizing mechanochemical synthesis and purified via solvent extraction. Studies by single crystal and powder X-ray diffraction (SC-XRD and PXRD) revealed that they crystalize in two polymorphic forms, α- and β-TBA<i>RE</i>B, adopting monoclinic (<i>P</i>2<sub>1</sub>/c) and orthorhombic (<i>P</i>nna) unit cells, previously found in TBAYB and TBAScB, respectively. Thermal decomposition of these compounds has been investigated using thermogravimetric analysis and differential scanning calorimetry (TGA/DSC) measurements, along with the analysis of the gaseous products with mass spectrometry (MS) and with analysis of the solid decomposition products with PXRD. TBAHoB and TBAYbB melt around 75 °C, which renders them new ionic liquids with relatively low melting points among borohydrides.
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