Abstract
[C16H27N2O2]+·C1O −4 ·1/2H2O,M r =387.86, is monoclinic:P21,a=8.934(1),b=14.625(1),c=14.449(1) Å, β=103.03(1)°,V c =1839.3(2) Å3,Z=4,D x =1.40(1) g cm−3, λ(CuKα)=1.54178 Å,μ(CuKα)=20.29 cm−1,F(000)=808 e,T=292K,R=0.057 for 3428 observed reflections. Two independent cations are connected into chains along [101] by short hydrogen bonds between their oxygen atoms O(C2) and O(N16); distances, 2.607(5) and 2.625(5) Å. The water molecule has short contacts with the two independent perchlorate anions, which indicates that the anions are linked by weak hydrogen bonds utilizing the water molecule. The conformations of the two independent cations are similar and can be described as distorted half-chair, chair, distorted boat, and chair for ringsA, B, C, andD, respectively. Except for the flexible ringA, few changes in conformation of the cations are observed in comparison to the cations of lupanineN(16)-oxide perchlorate or 17-β-meth-yllupanine perchlorate.
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References
Bratek-Wiewiórowska, D., Skolik, L., and Wiewiórowski, M. (1977)Bull. Acad. Pol. Sci. Ser. Sci. Chim. 25, 595.
Duax, W. L., and Norton, D. A. (1975)Atlas of Steroid Structure (Plenum, London).
Johnson, C. K. (1965)ORTEP Report ORNL-3794 (Oak Ridge National Laboratory, Oak Ridge, TN).
Kaluski, Z., Gusiev, A. I., Struchkov, J. T., Skolik, J., Baranowski, P., and Wiewiórowski, M. (1972)Bull. Acad. Polon. Sci. Ser. Sci. Chim. 20, 1.
Kaluski, Z., Skolik, J., and Wiewiórowski, M. (1978)Proceedings, Pre-Congress Symposium on Organic Crystal Chemistry, Dymaczewo, Poland, pp. 321–343.
Katrasiak, A., and Kaluski, Z. (1988)J. Crystallogr. Spectrosc. Res. 18, 365.
Katrusiak, A., Ratajczak-Sitarz, M., and Kałuski, Z. (1987).Acta Cryst. C43, 2386.
Kitaigorodsky, A. I. (1973)Molecular Crystals and Molecules (Academic Press, London).
Klyne, W., Scopes, P. N., Thomas, R. N., Skolik, J., Gawroriski, J., and Wiewiórowski, M. (1974)J. Chem. Soc. Perkin Trans. 1, 2565.
Lehmann, M. S., and Larsen, F. K. (1974)Acta Cryst. A30, 580.
Maluszyńska, H. (1977) Ph.D. thesis (Adam Mickiewicz University, Poznan, Poland).
Motherwell, W. D. S., and Clegg, W. (1978)Pluto 78, program for drawing molecular and crystal structures (University of Cambridge, Cambridge, England).
Sheldrick, G. M. (1976)Shelx 76, program for crystal structure determination (University of Cambridge, Cambridge, England).
Skrzypczak-Jankun, E., Maluszynska, H., Perkowska, H., and Kaluski, Z. (1980)J. Crystallogr. Spectrosc. Res. 10, 67.
Szymczak, A. (1983) Thesis (Adam Mickiewicz University, Poznan, Poland).
Taylor, R., and Kennard, O. (1982)J. Am. Chem. Soc. 104, 5063.
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Katrusiak, A., Kaluski, Z. Crystal and molecular structure of 17-β-methyllupanineN(16)-oxide perchlorate hemihydrate. Journal of Crystallographic and Spectroscopic Research 18, 375–385 (1988). https://doi.org/10.1007/BF01195690
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DOI: https://doi.org/10.1007/BF01195690