Skip to main content

Thank you for visiting You are using a browser version with limited support for CSS. To obtain the best experience, we recommend you use a more up to date browser (or turn off compatibility mode in Internet Explorer). In the meantime, to ensure continued support, we are displaying the site without styles and JavaScript.

Determination of complex structures by combined neutron and synchrotron X-ray powder diffraction


THE feasibility of determining crystal structures from powder diffraction data has improved substantially during the past decade. Early work using laboratory X-ray data1,2 has been followed by studies that take advantage of the higher resolution provided by synchrotron X-ray3 and neutron4 diffraction instrumentation. Other advances have been made in the computational aspects of the problem5,6. Nevertheless, there has remained a disparity between the complexity of structures that can be solved, ab initio, from powder data, and those that can in principle be refined by the Rietveld profile method7. For example, refinements with up to 34 atoms8 and 132 positional parameters9 have been reported, but the most complex unknown structure to be solved from powder data contains only 17 atoms in the asymmetric unit cell10. Here we describe the solution and refinement of Ga2(HPO3)3.4H2O, a novel framework structure with 29 atoms in the asymmetric unit cell and 117 structural parameters, by the combined use of synchrotron X-ray and neutron powder diffraction. Exploiting the complementary nature of these techniques further extends the power of powder diffraction for structure determination.

This is a preview of subscription content, access via your institution

Access options

Rent or buy this article

Get just this article for as long as you need it


Prices may be subject to local taxes which are calculated during checkout


  1. Berg, J.-E. & Werner, P.-E. Zeits. krist. 145, 310–320 (1977).

    CAS  Google Scholar 

  2. Rudolf, P. & Clearfield, A. Acta cryst. B41, 418–425 (1985).

    Article  Google Scholar 

  3. Attfield, J. P., Sleight, A. W. & Cheetham, A. K. Nature 322, 630–632 (1986).

    Article  ADS  Google Scholar 

  4. Cheetham, A. K. et al. Nature 320, 46–48 (1986).

    Article  ADS  CAS  Google Scholar 

  5. David, W. I. F. Nature 346, 731–734 (1990).

    Article  ADS  CAS  Google Scholar 

  6. Bricogne, C. & Gilmore, C. J. Acta cryst. A46, 248–297 (1990).

    Article  Google Scholar 

  7. Rietveld, H. M. J. appl. Cryst. 2, 65 (1969).

    Article  CAS  Google Scholar 

  8. Battle, P. D., Cheetham, A. K., Harrison, W. T. A. & Pollard, N. J. J. Solid State Chem. 58, 221–225 (1985).

    Article  ADS  CAS  Google Scholar 

  9. Hathaway, B. J. & Hewat, A. M. J. Solid State Chem. 51, 364–375 (1984).

    Article  ADS  CAS  Google Scholar 

  10. McCusker, L. B. J. appl. Cryst. 21, 305–310 (1988).

    Article  CAS  Google Scholar 

  11. Wilson, S. T., Lok, B. M., Messina, C. A., Cannan, T. R. & Flanigen, E. M. J. Am. chem. Soc. 104, 1146–1156 (1982).

    Article  CAS  Google Scholar 

  12. Flanigen, E. M., Lok, B. M., Patten, E. R. & Wilson, S, T. Stud. Surf. Sci. Catal. 28, 103–112 (1986).

    Article  CAS  Google Scholar 

  13. Esterman, M., McCusker, L. B., Baerlocher, C., Merrouche, A. & Kessler, H. Nature 352, 320–322 (1991).

    Article  ADS  Google Scholar 

  14. Ortiz-Avilla, C. Y., Squattrino, P. J., Shieh, M. & Clearfield, A. Inorg. Chem. 28, 2608 (1989).

    Article  Google Scholar 

  15. Sgyar, M., Durand, J., Cot, L. & Rafiq, M. Acta cryst. C47, 2515–2517 (1991).

    Google Scholar 

  16. Morris, R. E., Attfield, M. P. & Cheetham, A. K. Acta cryst. C (submitted).

  17. Werner, P.-E., Eriksson, L. & Westdahl, M. J. J. appl. Cryst. 18, 3647 (1985).

    Article  Google Scholar 

  18. Le Bail, A., Duroy, H. & Fourquet, J. L. Mat. Res. Bull. 23, 447 (1988).

    Article  CAS  Google Scholar 

  19. Larson, A. C. & Von Dreele, R. B. Los Alamos Laboratory Rep. No. LA-UR-86-748 (1987).

  20. Watkin, D. J., Carruthers, J. R. & Betteridge, P. W. CRYSTALS User Guide (Chemical Crystallography Laboratory, Univ. of Oxford, 1989).

    Google Scholar 

  21. Sheldrick, G. M. SHELXS-86 User Guide (Univ. of Gottingen, 1986).

    Google Scholar 

  22. Morris, R. E., Harrison, W. T. A., Stucky, G. D. & Cheetham, A. K. J. Solid State Chem. 94, 227–235 (1991).

    Article  ADS  CAS  Google Scholar 

  23. Harrison, W. T. A., Stucky, G. D., Morris, R. E. & Cheetham, A. K. Acta cryst. C48, 1365–1367 (1992).

    Google Scholar 

Download references

Author information

Authors and Affiliations


Rights and permissions

Reprints and Permissions

About this article

Cite this article

Morris, R., Harrison, W., Nicol, J. et al. Determination of complex structures by combined neutron and synchrotron X-ray powder diffraction. Nature 359, 519–522 (1992).

Download citation

  • Received:

  • Accepted:

  • Issue Date:

  • DOI:

This article is cited by


By submitting a comment you agree to abide by our Terms and Community Guidelines. If you find something abusive or that does not comply with our terms or guidelines please flag it as inappropriate.


Quick links

Nature Briefing

Sign up for the Nature Briefing newsletter — what matters in science, free to your inbox daily.

Get the most important science stories of the day, free in your inbox. Sign up for Nature Briefing