Abstract
X-ray spectral analysis has been applied to study the crystal structure of 4,7,13,16,21,24-hexaoxa-1-aza-10-azoniabicyclo[8.8.8]hexacosane isocyanurate of an unusual composition: [H1.2(Crypt-222)]1,2+ · [H0.8(Crypt-222)]0.8+·2(C3H2N3O3)− (I). The structure of I (space group C2/c, a = 37.840 Å, b = 13.760 Å, c = 19.456 Å, β = 91.21°, Z = 8) was solved by a direct method and refined by the full-matrix least-squares technique in the anysotropic approximation up to R = 0.119 over 6500 independent reflections measured (autodiffractometer CAD-4, λ-MoK α). The structure of I has two independent cations of 2.2.2-cryptand linked by the proximate pseudo-center of inversion and they have a rare conformation of exo-exo type, in which H atom or lone pair at both their node atoms N are directed outward their cavity. In the structure of I, all H atoms at N atoms of cations and half of H atoms of isocyanurate anions are disordered and have the populations of positions 0.7, 0.5, and 0.3. There is a developed system of interionic hydrogen bonds in the crystal structure of I.
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References
J.-M Lehn, Angew. Chem. Int. Ed. 27, No. 1, 89–112 (1988).
G. M. Sheldrick, The SHELX-97 Manual, Univ. Göttingen, Germany (1997).
International Tables for Crystallography. Vol. C, Kluwer Academic Publishers, Dordrecht (1992).
F. H. Allen, O. Kennard, D. G. Watson, et al., J. Chem. Soc. Perkin Trans. 2, 12, S1–S19 (1987).
J. Van Eerden, S. Harkema, and D. Feil, Acta Crystallogr., B46, No. 2, 222–229 (1990).
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Translated from Zhurnal Strukturnoi Khimii, Vol. 47, No. 1, pp. 77–83, January–February, 2006.
Original Russian Text Copyright © 2006 by A. N. Chekhlov
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Chekhlov, A.N. Disordered crystal structure of 4,7,13,16,21,24-hexaoxa-1-aza-10-azoniabicyclo[8.8.8]hexacosane isocyanurate. J Struct Chem 47, 71–77 (2006). https://doi.org/10.1007/s10947-006-0267-y
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DOI: https://doi.org/10.1007/s10947-006-0267-y