Ether cleavage of [2.2.2]cryptand: synthesis and X-ray crystal structure of [NH(CH2CH2I)3][I5]

Treatment of 2.2.2]cryptand1 in toluene with HI(g) has resulted in the formation of a twophase liquid clathrate solution from which the complex NH(CH₂CH₂I)₃]I₅]2 has been isolated and crystallographically characterized. Crystal data for2: triclinic, space group $P\bar 1$ ,a=9.301(3) Å,b=10.419(3) Å,c=11.078(3) Å, α=90.20(2)^o, β=103.28(2)^o γ=96.50(2)^o,D _c =3.57g/cm³,Z=2,R _f =0.054,R _w =0.054. The salt is a product of an ether cleavage of the macrobicycle. The crystal structure of2 contains NH(CH₂CH₂I)₃]⁺ ions and zigzag chains of I₅]^? ions which self-assemble to form alternating layers, of cations and anions.