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
Subscribe to this journal
Receive 51 print issues and online access
$199.00 per year
only $3.90 per issue
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
Berg, J.-E. & Werner, P.-E. Zeits. krist. 145, 310–320 (1977).
Rudolf, P. & Clearfield, A. Acta cryst. B41, 418–425 (1985).
Attfield, J. P., Sleight, A. W. & Cheetham, A. K. Nature 322, 630–632 (1986).
Cheetham, A. K. et al. Nature 320, 46–48 (1986).
David, W. I. F. Nature 346, 731–734 (1990).
Bricogne, C. & Gilmore, C. J. Acta cryst. A46, 248–297 (1990).
Rietveld, H. M. J. appl. Cryst. 2, 65 (1969).
Battle, P. D., Cheetham, A. K., Harrison, W. T. A. & Pollard, N. J. J. Solid State Chem. 58, 221–225 (1985).
Hathaway, B. J. & Hewat, A. M. J. Solid State Chem. 51, 364–375 (1984).
McCusker, L. B. J. appl. Cryst. 21, 305–310 (1988).
Wilson, S. T., Lok, B. M., Messina, C. A., Cannan, T. R. & Flanigen, E. M. J. Am. chem. Soc. 104, 1146–1156 (1982).
Flanigen, E. M., Lok, B. M., Patten, E. R. & Wilson, S, T. Stud. Surf. Sci. Catal. 28, 103–112 (1986).
Esterman, M., McCusker, L. B., Baerlocher, C., Merrouche, A. & Kessler, H. Nature 352, 320–322 (1991).
Ortiz-Avilla, C. Y., Squattrino, P. J., Shieh, M. & Clearfield, A. Inorg. Chem. 28, 2608 (1989).
Sgyar, M., Durand, J., Cot, L. & Rafiq, M. Acta cryst. C47, 2515–2517 (1991).
Morris, R. E., Attfield, M. P. & Cheetham, A. K. Acta cryst. C (submitted).
Werner, P.-E., Eriksson, L. & Westdahl, M. J. J. appl. Cryst. 18, 3647 (1985).
Le Bail, A., Duroy, H. & Fourquet, J. L. Mat. Res. Bull. 23, 447 (1988).
Larson, A. C. & Von Dreele, R. B. Los Alamos Laboratory Rep. No. LA-UR-86-748 (1987).
Watkin, D. J., Carruthers, J. R. & Betteridge, P. W. CRYSTALS User Guide (Chemical Crystallography Laboratory, Univ. of Oxford, 1989).
Sheldrick, G. M. SHELXS-86 User Guide (Univ. of Gottingen, 1986).
Morris, R. E., Harrison, W. T. A., Stucky, G. D. & Cheetham, A. K. J. Solid State Chem. 94, 227–235 (1991).
Harrison, W. T. A., Stucky, G. D., Morris, R. E. & Cheetham, A. K. Acta cryst. C48, 1365–1367 (1992).
Rights 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). https://doi.org/10.1038/359519a0
This article is cited by
Synthesis and crystal structures of aluminum and iron phosphites
Journal of Chemical Crystallography (1994)
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.