Synthesis, Polymorphism And Thermal Decomposition Process Of (N-C4h9)(4)Nre(Bh4)(4) For Re = Ho, Tm And Yb

In total, three novel organic derivatives of lanthanide borohydrides, n-But(4)NRE(BH4)(4) (TBAREB), RE = 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, alpha- and beta-TBAREB, adopting monoclinic (P2(1)/c) and orthorhombic (Pnna) 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 degrees C, which renders them new ionic liquids with relatively low melting points among borohydrides.