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The second order phase transition at 253 K of pyridinium tetrabromoantimonate(III), C 5 H 5 NHSbBr 4  , has been characterized by means of X-ray diffraction and  2 H NMR. As was suggested from the  81 Br NQR spectra, the Rietveld refinements of the X-ray diffraction patterns at 297 K and 116 K confirm the structural change of the anion from SbBr -  4  to SbBr 3  • Br - . The line shape analysis of the  2 H NMR using the deuterated analog revealed that the librational amplitude of the pyridinium ring about the axis normal to the plane increased with temperature and its rms amplitude reaching ca. 25° at T c  . The librational motion may induce the phase transition breaking the hydrogen bonds of the type N-H … Br. However, nearest-neighbor 2π/6 jump or reorientation such as seen in benzene were not observed even at 350 K.

Phase Transition of C 5 H 5 NHSbBr 4 Having a Hypervalent Bond: A 2 H NMR and X-Ray Diffraction Study [Phase Transition of C 5 H 5 NHSbBr 4 ]