Abstract
The 127 I-NQR of(HOCH 2 ) 3 CNH 3 + I - was determined in the range 77 ≤ T/K ≤ 310. At T = 310 K the NQR signal fades out (T m = 463 K). The 127 I spectrum ( T =77 K.): v 1 =29.195 MHz, v 2 = 14.597 MHz, η( 121 l)=0, e QΦ zz h -1 ( 127 I) = 97.315 MHz, is in agreement with the crystal structure. The 127 I NQR spectrum of 1,3-diammonium-2,2-dimethylpropane diiodide, (H 3 NCH 2 C(CH 3 ) 2 CH 2 NH 3 ) 2+ ·2I - , is a quartet within the whole temperature range investigated, and the lines correspond to two crystallographically independent iodines: Space group P2 1 /c, Z = 4, a = 731.2(3) pm, b = 689.0(3) pm, c = 2255.1(8) pm, β = 104.90(1)°. At 7 = 7 7 K the 127 I NQR quartet is (MHz): v 1 = 34.145, v 2 = 32.805, v 3 = 22.113, v 4 = 16.787; at 295 K (same order, MHz): 30.559, 29.729, 19.810, 15.651. There are two combinations of the NQR frequencies. Considering the coordination of I - , the hydrogen bonds N -H ··· I, eQΦ zz Q h -1 and η, we choose for I (1) v 1 and v 3 , for I (2) v 2 and v 4 . At 77 K eQΦ zz Q h -1 (I (1) )= 118.86 MHz,η ( 127 I (1) ) = 0.498, eQΦ zz Q h -1 (I (2) ) = 109.75 MHz, η( 127 I (2) ) = 0.135 follow for the two iodine atoms. Both, eQΦ zz Q h -1 (I (1) ) and e eΦ zz Q h -1 (I (2) ) decrease smoothly with increasing T: η I (2) ) increases with increasing T whereas η( 127 I (1) ) is almost constant within 77 ≤ T /K ≤ 4 0 6 . The 79,81 Br NQR spectrum of l,3-diamino-2,2-dimethylpropane dihydrobromide is also a quartet, showing two crystallographic inequivalent Br atoms in the unit cell. The frequencies are (T =273 K, MHz): v 1 ( 79 Br)= 14.303, v 2 ( 79 Br)= 12.884, ( 81 Br)= 11.951, v 2 ( 81 Br) = 10.781; space group C2/c, Z = 8 , a = 2136.4(6) pm, b = 854.6(3) pm, c = 1125.8(3) pm, β = 93.23(1)°. Crystal structures and NQR results are discussed.