ETHER CLEAVAGE OF [2.2.2]CRYPTAND - SYNTHESIS AND X-RAY CRYSTAL-STRUCTURE OF [NH(CH2CH2I)(3)][I-5]

Treatment of [2.2.2]cryptand 1 in toluene with HI(g) has resulted in t he formation of a two; phase liquid clathrate solution from which the complex [NH(CH2CH2I)(3)][I-5] 2 has been isolated and crystallographic ally characterized. Crystal data for 2: triclinic, space group P (1) o ver bar, a = 9.301(3) Angstrom, b = 10.419(3) Angstrom, c = 11.078(3) Angstrom, alpha = 90.20(2)degrees, beta = 103.28(2)degrees, gamma = 96 .50(2)degrees, D-c = 3.57 g/cm(3), Z = 2, R-f = 0.054, R-w = 0.054. Th e salt is a product of an ether cleavage of the macrobicycle. The crys tal structure of 2 contains [NH(CH2CH2I)(3)](+) ions and zigzag chains of [I-5](-) ions which self-assemble to form alternating layers of ca tions and anions.