Structure and vibrational dynamics of isotopically labeled lithium borohydride using neutron diffraction and spectroscopy

The crystalline structure of a 7 Li and 11 B labeled lithium borohydride has been investigated using neutron powder diffraction at 3.5, 360, and 400 K. The B–H bond lengths and H–B–H angles for the [BH4] � tetrahedra indicated that the tetrahedra maintained a nearly ideal configuration throughout the temperature range investigated. The atomic displacement parameters at 360 K suggest that the [BH4] � tetrahedra become increasingly disordered as a result of large amplitude librational and reorientational motions as the orthorhombic to hexagonal phase transition (T ¼ 384 K) is approached. In the high-temperature hexagonal phase, the [BH4] � tetrahedra displayed extreme disorder about the trigonal axis along which they are aligned. Neutron vibrational spectroscopy data were collected at 5 K over an energy range of 10–170 meV, and were found to be in good agreement with prior Raman and low-resolution neutron spectroscopy studies.