Abstract
In this work X-ray single crystal structural analysis was carried out on the clathrate hydrate of tetraisoamylammonium propionate with the composition (i-C5H11)4NC2H5CO2·36H2O. The hydrate was found to have an orthorhombic structure in space group Cmc2 1 with unit cell parameters: a = 21.281(2) Å, b= 12.010(7) Å, c = 24.768(3) Å (150 K). X-ray powder diffraction studies were performed of the hydrate phase, crystallized in the water–(i-C5H11)4NC2H5CO2 system in the concentration range of the salt (10–25 wt%) that is the crystallization region of the studied polyhydrate, according to the phase equilibria data. It was found, that in the given concentration region the same hydrate of orthorhombic structure is formed, unit cell parameters, obtained at 20 °C: a = 21.454(13) Å, b = 12.156(4) Å, c = 25.030(14) Å, are in a good agreement with the data of single crystal structural analysis.
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References
Jeffrey G.A., (1996), Hydrate inclusion compounds In Atwood J.L., Davies J.E.D., MacNicol D.D., Vögtle F., (eds), Comprehensive Supramolecular Chemistry 6, Pergamon Press Oxford pp. 757–788
Yu.A. Dyadin and K.A. Udachin: J. Struct. Chem. 28, 394 (1987) (translated from Russian Zh. Strukt. Khim. 28, 75 (1987))
Bonamico M., Jeffrey G.A., McMullan R.K., J. Chem. Phys. 37: 2219 (1962)
Beurskens G., Jeffrey G.A., McMullan R.K., J. Chem. Phys. 39, 3311 (1963)
Dyadin Yu.A., Gaponenko L.A., Aladko L.S., Bogatyryova S.V., J. Inclusion Phenom. 2: 259 (1984)
Lipkowski J.S., Komarov Yu.V., Rodionova T.V., Aladko L.S., Zh. Strukt. Khim. 46: S52 (2005)
Terekhova I.S., Bogatyryov V.L., Dyadin Yu.A., Zh. Strukt. Khim. 35, 67 (1994) (in Russian)
Otwinowski Z., Minor W., (1997) Processing of X-ray diffraction data collected in oscillation mode In Carter Jr. C.W., Sweet R.M., (eds), Methods in Enzymology, v.276: Macromolecular Crystallography, Part A Academic Press New York pp.307–326
Sheldrick G.M., (1998). SHELX-97 Release 97-2 Göttingen University Germany
Feil D., Jeffrey G.A., J. Chem. Phys. 35: 1863 (1961)
Acknowledgements
The authors wish to acknowledge the financial support of KBN Grant 4 T09A 143 23.
A.Yu. Manakov thanks “Russian Science Support Foundation” for the financial support.
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Suwinska, K., Lipkowski, J.S., Dyadin, Y.A. et al. Clathrate Formation in the Water–Tetraisoamylammonium Propionate System: X-ray Structural Analysis of the Clathrate Hydrate (i-C5H11)4NC2H5CO2·36H2O. J Incl Phenom Macrocycl Chem 56, 331–335 (2006). https://doi.org/10.1007/s10847-006-9102-5
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DOI: https://doi.org/10.1007/s10847-006-9102-5