Abstract
Two compounds, 7,13,16,21,24-hexaoxa-1,10-diazoniabicyclo[8.8.8]hexacosane bis(tribromide) and bis(bromodiiodide) — [H2(Crypt-222)]2+·2Br −3 (I) and [H2(Crypt-222)]2+·1.45(BrI2)−·0.4(Br2I)−·0.15 I −3 (II) — are prepared and characterized by single crystal XRD; the refinement of the second compound was more accurate. Isomorphous monoclinic structures (I, space group C2/c, Z = 4, a = 12.090, b = 15.833 Å, c = 15.732 Å, β = 95.83°; II, a = 12.548 Å, b = 16.417 Å, c = 15.748 Å, β = 94.53°) are solved by a direct method and refined in the anisotropic full-matrix approximation to R = 0.057 (I) and 0.044 (II) using all 2635 (I) and 2852 (II) measured independent reflections (automated CAD-4 diffractometer, λMoK α). In the structures of I and II one of the trihalide anions sits at the inversion center i(000), and the second trihalide anion and the dication [H2(Crypt-222)]2+ are situated at crystallographic axis 2. In the structure of II iodine is located in the center of trihalide anions, while the terminal atoms are disordered and are represented by a statistical combination of iodine and bromine atoms.
Similar content being viewed by others
References
M. Hiraoka, Crown Compounds: their Characteristics and Applications, Elsevier Science Publishers (1982).
A. N. Chekhlov, Zh. Strukt. Khim., 46, No. 3, 585–590 (2005).
A. C.T. North, D. C. Phillips, and F. S. Mathews, Acta rystallogr., A24, No. 3, 351–359 (1968).
G. M. Sheldrick, 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. II, No. 12, S1–S19 (1987).
J. van Eerden, S. Harkema, and D. Feil, Acta Crystallogr., B46, No. 2, 222–229 (1990).
R. Taylor and O. Kennard, J. Am. Chem. Soc., 104, No. 19, 5063–5070 (1982).
Author information
Authors and Affiliations
Additional information
Original Russian Text Copyright © 2007 by A. N. Chekhlov
__________
Translated from Zhurnal Strukturnoi Khimii, Vol. 48, No. 1, pp.137–142, January–February, 2007.
Rights and permissions
About this article
Cite this article
Chekhlov, A.N. Isomorphous crystal structures of 4,7,13,16,21,24-hexaoxo-1,10-diaziniabicyclo[8.8.8]·hexacosane bis(tribromide) and bis(bromoiodide). J Struct Chem 48, 137–143 (2007). https://doi.org/10.1007/s10947-007-0020-1
Received:
Issue Date:
DOI: https://doi.org/10.1007/s10947-007-0020-1