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Phase and X-ray study of clathrate formation in the tetraisoamylammonium fluoride-water system

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Abstract

The phase diagram of the binary (i-C5H11)4NF-water system has been studied in the clathrate formation region. Three polyhydrates have been discovered, two of which (1∶38.9 and 1∶32.7) are the known orthorhombic and tetragonal phases:Pbmn,a=11.88,b=21.53,c=12.70 Å,ρ means=1.019 g cm-3 (0°C), m.p.=32.4°C andP42/m, a=23.729,c=12.466 Å,ρ means=1.062 g cm-3, (0°C), m.p.=31.2°C, respectively. A single crystal X-ray analysis of the novel clathrate hydrate (i-C5H11)4NF·27 H2O is reported. This new clathrate hydrate is tetragonal,I4I/a, witha=16.894(5),c=17.111(2) Å,Z=4, (−50°C), and m.p.=34.6°C. Each (i-C5H11)4N+ cation occupies a four-chamber cavity built of 15-hedra 71635942 (idealized description), with small vacant 5444 cavities filling the intervening space.

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References

  1. 1.

    H. Nakayama:Bull. Chem. Soc. Jpn. 54, 3117 (1981).

  2. 2.

    R.K. McMullan and G.A. Jeffrey:J. Chem. Phys. 31, 1231 (1959).

  3. 3.

    D. Feil and G.A. Jeffrey:J. Chem. Phys. 35, 1863 (1961).

  4. 4.

    H. Nakayama:Bull. Chem. Soc. Jpn. 55, 389 (1982).

  5. 5.

    Yu.A. Dyadin, F.V. Zhurko and Yu.M. Zelenin:Izv. Sib. Otd. Akad. Nauk SSSR, Ser. Khim. Nauk 1, 13 (1984).Chem. Abstr. 100:198457d.

  6. 6.

    Yu.A. Dyadin, F.V. Zhurko and Yu.M. Zelenin:Izv. Akad. Nauk SSSR, Ser. Khim. Nauk 2, 479 (1983).Chem. Abst. 98:156144k.

  7. 7.

    H. Nakayama:Bull. Chem. Soc. Jpn. 60, 2319 (1987).

  8. 8.

    Yu.A. Dyadin and L.S. Kiselyova:Izv. Sib. Otd. Akad. Nauk SSSR, Ser. Khim. Nauk 1, 124 (1980).Chem. Abstr. 92:186613e.

  9. 9.

    Yu.A. Dyadin and K.A. Udachin:Zh. Strukt. Khim. 28, 75 (1987).

  10. 10.

    T.V. Rodionova, Yu.A. Dyadin, K.A. Udachin, J. Lipkowski and K. Suwinska:Sib. Khim. Zh. 2, 54 (1992).Chem. Abstr. 117:119355u.

  11. 11.

    B.S. Smolyakov, Yu.A. Dyadin and L.S. Aladko:Izv. Sib. Otd. Akad. Nauk SSSR, Ser. Khim. Nauk 6, 66 (1980).Chem. Abstr. 94:113955z.

  12. 12.

    J. Mitchell and D.M. Smith:Aquametry, 2nd Ed., New York, John Wiley & Sons (1980).

  13. 13.

    G.M. Sheldrick:SHELXS86, in G.M. Sheldrick, C. Krueger and R. Goddard (Eds.)Crystallographic Computing 3, pp. 175–189. Oxford University Press (1985).

  14. 14.

    G.M. Sheldrick:SHELXS76, Program for Crystal Structure Determination, University of Cambridge, England (1976).

  15. 15.

    R.K. McMullan, G.A. Jeffrey and T.H. Jordan:J. Chem. Phys. 47, 1229 (1967).

  16. 16.

    J. Lipkowski, K. Suwinska, T.V. Rodionova, J.A. Udachin and Yu.A. Dyadin: Polish School on ‘Supramolecular Chemistry’, Abstracts, Gdansk, p. 14 (1990).

  17. 17.

    Yu.A. Dyadin, I.V. Bondaryuk and F.V. Zhurko:Clathrate Hydrates at High Pressures, inInclusion Compounds, Eds., J.L. Atwood, J.E.D. Davies and D.D. MacNicol, Oxford University Press, Vol. 5, p. 213 (1991).

  18. 18.

    G.A. Jeffrey and R.K. McMullan:Prog. Inorg. Chem. 8, 43 (1967).

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Supplementary Data relevant to this paper have been deposited with the Britsh Library as Supplementary Publication SUP 82162 (13 pages).

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Lipkowski, J., Suwinska, K., Rodionova, T.V. et al. Phase and X-ray study of clathrate formation in the tetraisoamylammonium fluoride-water system. J Incl Phenom Macrocycl Chem 17, 137–148 (1994). https://doi.org/10.1007/BF00711854

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Key words

  • Clathrate hydrate
  • phase diagram
  • crystal structure
  • tetraisoamylammonium fluoride