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The temperature dependence of  127 I NQR and DSC as well as the crystal structure at room temperature of the title compound were determined. This compound shows a first-order phase transition of an order-disorder type at 245 K. Eight  127 I(v 1 :m = ±1/2 ↔ ±3/2) NQR lines of 79.57, 81.86, 82.56, 83.36, 84.68, 87.72, 88.34, and 88.86 MHz, and corresponding eight  127 I(v 2 : m = ±3/2 ↔±5/2) NQR lines were observed at liquid nitrogen temperature. Three  127 I(υ i ) NQR lines wfth an intensity ratio of 1:1:2 in the order of decreasing frequency were observed just above the transition point and two NQR lines except for the middle-frequency line disappeared around room temperature. This temperature behavior of NQR lines is very similar to that observed in [N(CH 3 ) 4 ] 2 Hgl 4 . Another first-order phase transition takes place at 527 K. The structure of the room-temperature phase was redetermined: orthorhombic, Pnma, Z = 4, a = 1342.8(3), b = 975.7(2), c = 1696.5(3) pm. The NQR result of three lines with an intensity ratio of 1:1:2 is in agreement with this structure. The thermal displacement parameters of atoms in both cations and anions are large.

127 I NQR and Crystal Structure Studies of [N(CH 3 ) 4 ] 2 CdI 4