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

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Abstract

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.

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MacGillivray, L.R., Atwood, J.L. Ether cleavage of [2.2.2]cryptand: synthesis and X-ray crystal structure of [NH(CH2CH2I)3][I5]. J Chem Crystallogr 27, 209–213 (1997). https://doi.org/10.1007/BF02575956

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