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Four new ionic rotator-crystals of [NEt   x   Me (3− x ) R][BEt 4 ] (R = Pr, Bu;  x  = 1, 2) were observed. Rotator crystals (two-dimensional plastic crystals) are mesophases between solid and isotropic liquid phases. Solid-state  1 H and  13 C nuclear magnetic resonance (NMR) measurements revealed that the ellipsoidal cations of [NEt   x   Me (3− x ) R] +  undergo uniaxial rotation about their N–R axis and libration motion of the axis, and the anions perform isotropic reorientations in the highest-temperature solid-phase (rotator phase). Differential scanning calorimetry (DSC) measurements showed small entropy changes of 8–11 J K −1  mol −1  at the melting point of the compounds. These results suggest that the cations and anions have large degrees of freedom of motion in the rotator phase. The diffraction patterns of X-ray diffraction (XRD) could be indexed to the trigonal structure (space group of  P 31 c ). Compared with the reported data for [NEt   x   Me (3− x ) Pr][BEt 3 Me] ( x  = 1, 2) compounds, which also have rotator-crystal phases and transform to a plastic crystalline phase, a model that explains why the cations of [BEt 4 ] salts hardly perform isotropic reorientation in the solid phases was proposed.

Solid-state 1 H and 13 C NMR studies of novel ionic rotator-crystals of [NEt x Me (3− x ) R][BEt 4 ] (R = Pr, Bu. x = 1, 2)