Bulletin of the Korean Chemical Society

Korean Chemical Society (대한화학회)
권호 표지
DOI QR코드

DOI QR Code

The Crystal Structure of a Sulfur Sorption Complex of the Dehydrated Partially $Co^{2+}$-Exchanged Zeolite A

  • Published : 1995.09.20
Download PDF
⟨ Previous Next ⟩

Abstract

The crystal structure of a sulfur sorption complex of the dehydrated partially Co2+ exchanged zeolite A (a=12.058(2) Å) has been determined by single-crystal X-ray techniques. The crystal structure was solved and refined in cubic space group Pm3m at 21(1) ℃. Ion Exchange with aqueous 0.05 M Co(NO3)2 was done by the static method. The crystal of Na4Co4-A was dehydrated at 380 ℃ and 2 × 10-6 Torr for 2 days, followed by exposure to about 100 Torr of sulfur at 330 ℃ for 72 h. Full matrix least-squares refinement converged to R1=0.084 and Rw=0.074 with 102 reflections for which I > 3σ(I). Crystallographic analysis shows that 2.8 Co2+ ions and 4 Na+ ions per unit cell occupy 6-ring sites on the threefold axes. 1.2 Co2+ ions occupy the 8-ring sites on fourfold axes. 2.8 Co2+ ions at Co(1) are recessed 0.66 Å into the large cavity and 4 Na+ ion at Na(1) are recessed 0.77 Å into the sodalite cavity from the (111) plane of O(3)'s. Approximately 16 sulfur atoms were sorbed per unit cell. Two S8 rings, each in a butterfly form, are found in the large cavity. The bond length between S and its adjacent S is 2.27(3) Å. The distance between 6-ring Co2+ ion and its adjacent sulfur is 2.53 (2) Å and that between 8-ring Co2+ ions and its adjacent sulfur is 2.72(9) Å. The angles of S-S'-S and S'-S-S'/ in octasulfur rings are 119.0(2)°and 113.0(2)°, respectively.

Keywords

References

  1. J. Phy. Chem. v.76 Seff, K.
  2. J. Chem. Soc. A Barrer, R. M.;Whiteman, J. L.
  3. Chem. Rev. v.64 Myer, B.
  4. Sulfur in Organic and Inorganic Chemistry v.2 no.A Johnson, D. A.;Sennig(ed.)
  5. Chem. Rev. v.76 Myer, B.
  6. J. Phys. Chem. v.76 Myer, B.;Spitzer, K.
  7. J. Phys. Chem. v.72 Ward, A. T
  8. J. Chem. Soc. A Ozin, G. A.
  9. Can. J. Chem. v.47 Anderson, A.;Loh, Y. T.
  10. Spectrochem., Acta. v.30 Gautier, G.;Debeau, M.
  11. J. Cryst. Growth v.8 Charnell, J. F.
  12. Inorg. Chem. v.13 Riley, P. E.;Seff, K.
  13. J. Phys. Chem. v.95 Kim, Y.;Lee, S. K.;Seff, K.
  14. J. Phys. Chem. v.88 Seff, K.;Mellum, M. D.
  15. Acc. Chem. Res. v.9 Structural Chemistry Inside Zeolite A Seff, K.
  16. Principal computer program and used in this study is MolEN supplied from the Enraf-Nonius
  17. J. Am. Chem. Soc. v.100 Kim, Y.;Seff, K.
  18. International Tables for X-ray Crystallography v.Ⅲ Kynoch Press
  19. Encyclopedia of Inorganic Chemistry v.7 Burce King, R.
  20. J. Am. Chem. Soc. v.66 Lu, C. S.;Donohue, J.
  21. Acta Crystallogr. v.8 Abrahams, S. C.
  22. Acta Crystallogr. v.14 Abrahams, S. C.
  23. Acta Crystallogr. v.14 Cooper, A. S.;Bond, W. L.;Abrahams, S. C.
  24. Acta Crystallogr. v.18 Abrahams, S. C.
  25. J. Acta Crystallogr. v.14 Caron, A.;Donohue, J.
  26. J. Acta Crystallogr. v.18 Caron, A.;Donohue, J.
  27. Bull. Korean Chem. Soc. v.10 Kim, Y.;Lee, S. H.;Seff, K.
  28. The Nature of the Chemical Bond(3rd Ed.) Pauling, L.
  29. Handbook of Chemistry and physics(67th Ed.) Chemical Rubber Co.
  30. Angew. Chem. Int. Ed. v.14 Steudel, R.
  31. Advance Inorganic Chemistry(4th Ed.) Cotton, F. A.;Wilkinson, G.