A case study in direct-space structure determination from powder x-ray diffraction data: Finding the hydrate structure of an organic molecule with significant conformational flexibility

Crystal Growth and Design

Volumn 5, Issue 6, 2005, Pages 2084-2090

  Pan, Zhigang ^a   Cheung, Eugene Y ^a   Harris, Kenneth D M ^a   Constable, Edwin C ^b   Housecroft, Catherine E ^b  

^a CARDIFF UNIVERSITY   (United Kingdom)

^b UNIVERSITY OF BASEL   (Switzerland)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 27744529811     PISSN: 15287483     EISSN: None     Source Type: Journal    
DOI: 10.1021/cg050212d     Document Type: Article

References (33)

1. (a) Harris, K. D. M.; Tremayne, M. Chem. Mater. 1996, 8, 554.
2. (b) Harris, K. D. M.; Tremayne, M.; Kariuki, B. M. Angew. Chem., Int. Ed. 2001, 40, 1626.
3. (c) Chernyshev, V. V. Russ. Chem. Bull. 2001, 50, 2273.
4. (d) Harris, K. D. M.; Cheung, E. Y. Chem. Soc. Rev. 2004, 33, 526.
5. (e) Altomare, A.; Caliandro, R.; Camalli, M.; Cuocci, C.; Giacovazzo, C,; Moliterni, A. G. G.; Rizzi, R.; Spagna, R.; Gonzalez-Platas, J. Z. Kristallogr. 2004, 216, 833.
6. (f) Harris, K. D. M.; Habershon, S.; Cheung, E. Y.; Johnston, R. L. Z. Kristallogr. 2004, 216, 838.
7. (g) Favre-Nicolin, V.; Černý, R. Z. Kristallogr. 2004, 216, 847.
8. (h) Shankland, K.; Markvardsen, A. J.; David, W. I. F. Z. Kristallogr. 2004, 216, 857.
9. Harris, K. D. M.; Tremayne, M.; Lightfoot, P.; Bruce, P. G. J. Am. Chem. Soc. 1994, 116, 3543.
10. (a) McCusker, L. B.; Von Dreele, R. B.; Cox, D. E.; Louër, D.; Scardi, P. J. Appl. Crystallogr. 1999, 32, 36.
11. (b) Rietveld, H. M. J. Appl. Crystallogr. 1969, 2, 65.
12. (c) Young, R. A., Ed. The Rietveld Method; International Union of Crystallography: Oxford, U.K., 1993.
13. (a) Kariuki, B. M.; Serrano-González, H.; Johnston, R. L.; Harris, K. D. M. Chem. Phys. Lett. 1997, 280, 189.
14. (b) Harris, K. D. M.; Johnston, R. L.; Kariuki, B. M. Acta Crystallogr. 1998, A54, 632.
15. (c) Habershon, S.; Harris, K. D. M.; Johnston, R. L. J. Comput. Chem. 2003, 24, 1766.
16. (d) Cheung, E. Y.; Kitchin, S. J.; Harris, K. D. M.; Imai, Y.; Tajima, N.; Kuroda, R. J. Am. Chem. Soc. 2003, 125, 14658.
17. (e) Albesa-Jové, D.; Kariuki, B. M.; Kitchin, S. J.; Grice, L.; Cheung, E. Y.; Harris, K. D. M. ChemPhysChem 2004, 5, 414.
18. (f) Guo, F.; Harris, K. D. M. J. Am. Chem. Soc. 2005, 127, 7314.
19. 7 The aim of pattern decomposition/profile fitting is to fit the complete experimental powder X-ray diffraction profile by refinement of variables that describe peak positions, background intensity distribution, peak widths, peak shapes, and peak intensities. No structural model is used in this fitting process (except insofar as the unit cell parameters determined in the indexing stage are used to establish the initial peak positions), and the peak intensities are simply a set of intensity variables that are refined to give optimal fit to the experimental powder X-ray diffraction pattern without reference to any structural model. Clearly, the pattern decomposition/profile fitting procedure establishes a limit to the quality of fit that could be obtained in a Rietveld refinement calculation for the same experimental powder X-ray diffraction pattern (taken over the same 2θ range). In Rietveld refinement, the peak intensities are tied to a structural model and are therefore not independent refinable variables.
20. Pawley, G. S. J. Appl. Crystallogr. 1981, 14, 357.
21. Le Bail, A.; Duroy, H.; Fourquet, J. L. Mater. Res. Bull. 1988, 23, 452.
22. Habershon, S.; Turner, G. W.; Kariuki, B. M.; Cheung, E. Y.; Hanson, A. J.; Tedesco, E.; Albesa-Jové, D.; Chao, M.-H.; Lanning, O. J.; Johnston, R. L.; Harris, K. D. M. EAGER-A Computer Program for Direct-Space Structure Solution from Powder X-ray Diffraction Data; Cardiff University and University of Birmingham.
23. Larson, A. C.; Von Dreele, R. B. GSAS; Los Alamos Laboratory Report No. LA-UR-86-748, 1987.
24. Visser, J. W. J. Appl. Crystallogr. 1969, 2, 89.
25. -1, which may suggest that the OH group is involved in hydrogen bonding.
26. 2 bonds relative to the orientation of the C(4)-H bond of the central phenyl ring.
27. 3 bonds relative to the orientation of the C(4)-O bond of the peripheral phenyl rings.
28. (a) Saad, J. M.; Soepadamo, E.; Fang, X.-P.; McLaughlin, J. L.; Fanwick, P. E. J. Nat. Prod. 1991, 54, 1681.
29. (b) Wallet, J. C.; Molins, E.; Miravitlles, C. Acta Crystallogr. 1995, C51, 103.
30. (c) Lockhart, J. C.; McDonnell, M. B.; Clegg, W.; Hill, M. N. S. J. Chem. Soc., Perkin Trans. 2 1987, 639.
31. (d) Krygowski, T. M.; Pindelska, E.; Anulewicz-Ostrowska, T.; Grabowski, S. J.; Dubis, A. T. J. Phys. Org. Chem. 2001, 14, 349.
32. (a) Aliev, A. E.; MacLean, E. J.; Harris, K. D. M.; Kariuki, B. M.; Glidewell, C. J. Phys. Chem. B 1998, 102, 2165.
33. (b) Serrano-González, H.; Harris, K. D. M.; Wilson, C. C.; Aliev, A. E.; Kitchin, S. J.; Kariuki, B. M.; Bach-Vergés, M.; Glidewell, C.; MacLean, E. J.; Kagunya, W. W. J. Phys. Chem. B 1999, 103, 6215.