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Using X-ray Powder Diffraction to Determine the Structure of VPI-5 - A Molecular Sieve with the Largest Known Pores

Published online by Cambridge University Press:  06 March 2019

Cyrus E. Crowder
Affiliation:
Analytical Sciences, 1897 Bldg. Dow Chemical Co., Midland, MI
Juan M. Garces
Affiliation:
Central Research, 1776 Bldg. Dow Chemical Co., Midland, MI
Mark E. Davis
Affiliation:
Virginia Polytechnic Institute Blacksburg, VA
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Extract

The synthesis of a new family of aluminophosphate-based molecular sieves containing pores defined by 18 tetrahedrally linked atoms has been described by Davis et al at Virginia Polytechnic Institute (VPI). This development reprsents the first reposted synthesis of a moleoular sieve with pores larger than those defined by 12 tetrahedrally linked atoms. This material has been shown to readily absorb triisopropyl benzene and exhibits a pore size distribution, determined from, its argon adsorption isotherm, which suggests the existence of molecular sieve pores larger than those found in known molecular sieves. Confirmation of a pore defined by 18 tetrahedrally linked aluminum and phosphorus atoms was accomplished by crystallographic structure determination using X-ray powder diffraction data. Single crystal methods were impossible due to an inability to synthesize crystals of suitable size. Details of the structure determination are reported in this work.

Type
VIII. Applications of Digitized XRD Patterns
Copyright
Copyright © International Centre for Diffraction Data 1988

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References

1. Davis, M.E., Saldarriaga, C., Montes, C., Garces, J., and Crowder, C., “A Molecular Sieve with Eighteen-membered Rings”, Nature 331:698 (1988).Google Scholar
2. Davis, M.E., Saldarriaga, C., Montes, C., Garces, J., and Crowder, C., “VPI-5: The First Molecular Sieve With Pores Larger Than Ten Angstroms”, Zeolites 8:36 (1988).Google Scholar
3. Breck, D.W., “Structure of Zeolites”, in: Zeolite Molecular Sieves Wiley, New York, (1974).Google Scholar
4. Flanigen, E.M., Lok, B.M., Patton, R.L., and Wilson, S.T., “Alumino-phosphate Molecular Sieves and the Periodic Table”, Pure & Appl. Chem. 58:1351 (1986).Google Scholar
5. Brown, A. and Edmonds, J.W., “Th Fitting of Powder Diffraction Profiles to an Analytical Expression and the Influence of Line Broadening Factors”, in: Advances in X-ray Analysis. 23:361, Rhodes, J.R. ed. , Plenum Press, New York, (1980).Google Scholar
6. Louër, D., and Vargas, R., “Indexation Automatique des Diagrammes de Poudre par Dichotomies Successives”, J. Appl. Cryst. 15:542 (1982).Google Scholar
7. Appleman, D.E. and Evans, H.T., “Indexing and Lesst-Squares Refinement of Powder Diffraction Data”, USGS-GD-73-003, (1973).Google Scholar
8. Henry, N.F.M. and Lonsdale, K., eds. “International Tables for X-ray Crystallography- Vol. I”, Kynoch Press, Birmingham, England (1969).Google Scholar
9. Davis, H.E., Montes, C., Hathaway, P.E., Arhancet, J.P., Hasha, D., and Garces, J., “Physicochemical Properties of VPI-5”, submitted to J. Amer. Chem. Soc.Google Scholar
10. Smith, J.V. and Dytrych, W. J., “Nets with Channels of Unlimited Diamater”, Nature 309-607 (1984).Google Scholar
11. Ch. Baerlocher, Hepp, A., and Meier, W.M., “DLS-76 - A Program for the Simulation of Crystal Structures by Geometric Refinement”, Institut für Kristallographie & Petrographie, ETH, Zurich, (1977).Google Scholar
12. Bennett, J.M., Cohen, J.P., Flanigen, E.M., Pluth, J.J., and Smith, J.V., “Crystcal Structure of Tetrapropylammonium Hydrostide-Aluminum Phosphate Number 5”, in: Intrazeolite Chemistry, ACS Symposium Series No. 218:109 (1983).Google Scholar
13. Bennett, J.M., Dytrych, W.J., Pluth, J.J., Richardson, J.W. Jr. and Smith, J.V., “Structural Features of Aluminophosphate Materials with Al/P = 1”, Zeolites 6:349 (1986).Google Scholar
14. Baerlocher, Ch., “Zeolite Structure Refinements Using Powder Data”, Zeolites 6:325 (1986).Google Scholar
15. Rietveld, H.M., “A Profile Refinement Method for Nuclear and Magnetic Structures”, J. Appl. Cryst. 2:65 (1969).Google Scholar