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Guanidinium hexabromoantimonate(V) [C(NH 2 ) 3 ]SbBr 6  was prepared. It was black in color at room temperature and showed a tendency to turn yellow by loosing bromine in open air. Six  81 Br NQRlines were observed at 77K.On heating, four of the six lines faded out around 200 K,while the remaining two lines could be observed up to room temperature. This temperature behavior suggests a preferential libration or reorientation around a pseudo C 4  axis of the octahedral [SbBr 6 ] -  anion. DTA measurement revealed a small heat anomaly at T c1  = 273 K (on heating), showing a thermal hysteresis, and a sharp and large anomaly at T c2  = 314 K. The temperature dependence curve of  1 H NMR T 1  is characterized by a single minimum of 26 ms (32 MHz) near 280 K, which is assigned to the C3 reorientation of the planar [C(NH2)3]+ cations. Its activation energy ( a) is 43.3 kJ/mol

81 Br NQR and 1 H NMR of Guanidinium Hexabromoantimonate(V) [C(NH 2 ) 3 ]SbBr 6 : Phase Transition and Molecular Motion