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The crystal structure of [4-C 2 H 5 -C 6 H 4 NH 3 ] 2 ZnBr 4  ( 1 ) has been determined at 150(2) K: triclinic,  P 1̅,  a =724.82(2),  b =1194.20(4),  c =1322.26(4) pm,  α =74.151(3),  β =80.887(3),  γ =80.434(3)°, and  Z =2. There are two crystallographically independent cations in the unit cell of  1 : one has its benzene ring perpendicular to the crystallographic  a  axis of the unit cell and the other one has its benzene ring perpendicular to the  c  axis. These cations are alternatingly located along the  c  axis and form organic layers, and the ZnBr 4  anions form inorganic layers in between. Zn–Br···H–N hydrogen bonds are formed between cations and anions. In accordance with the crystal structure, four nuclear quadrupole resonance (NQR) lines of  81 Br were observed. The temperature dependence of the  81 Br NQR frequencies between 77 and 320 K shows a peculiar feature which is not due to a structural phase transition. The measurement of  13 C nuclear magnetic resonance spectra at around  T =340 K indicates a redistribution of cations. The temperature dependence of  81 Br NQR frequencies and differential thermal analysis measurements show that [4-C 2 H 5 -C 6 H 4 NH 3 ] 2 CdBr 4  ( 2 ) undergoes a structural phase transition at around 190 K.

NQR, NMR, and X-ray crystal structure studies of [4-C 2 H 5 -C 6 H 4 NH 3 ] 2 MBr 4 (M=Zn, Cd)