Routine ab initio structure determination of chlorothiazide by X-ray powder diffraction using optimised data collection and analysis strategies

Abstract

The likelihood of solving crystal structures from powder diffraction data is greatly enhanced if data collection and analysis strategies can be designed to effectively remove Bragg peak overlap. In this way, accurate normalised structure factors of essentially single-crystal quality are obtained. Such strategies are illustrated here with theab initio solution, from powder diffraction data using traditional direct methods, of the clinically used diuretic compound chlorothiazide. The structure solution is outstanding in that, despite the non-centrosymmetric, triclinic symmetry, all 17 non-hydrogen atom positions are clearly visible in the E-map generated from the top direct methods solution.

References

1. G. H. Stout and L. H. Jensen, X-ray Structure Determination, Wiley Interscience, New York, 1989.
2. W. I. F. David, J. Appl. Crystallogr., 1987, 20, 316.
3. G. Bricogne, Acta Crystallogr., Sect. A, 1991, 47, 803.
4. J. Jansen, R. Peschar and H. Schenk, J. Appl. Crystallogr., 1992, 25, 231.
5. M. A. Estermann and V. Gramlich, J. Appl. Crystallogr., 1993, 26, 396.
6. D. S. Sivia and W. I. F. David, Acta Crystallogr., Sect. A, 1994, 50, 703.
7. J. I. Langford and D. Louër, Rep. Prog. Phys., 1996, 59, 131.
8. P. Lightfoot, M. Tremayne, C. Glidewell and K. D. M. Harris, J. Chem. Soc., Perkin Trans. 2, 1993, 1625.
9. R. G. Delaplane, W. I. F. David, R. M. Ibberson and C. C. Wilson, Chem. Phys. Lett., 1993, 201, 75.
10. H. Fjellvag and P. Karen, Inorg. Chem., 1992, 31, 3260.
11. D. M. Poojary, R. B. Borade, F. L. Campbell and A. Clearfield, J. Solid State Chem., 1994, 112, 106.
12. R. E. Morris, W. T. A. Harrison, J. M. Nicol, A. P. Wilkinson and A. K. Cheetham, Nature (London), 1992, 359, 519.
13. R. E. Morris, J. J. Owen, J. K. Stalick and A. K. Cheetham, J. Solid State Chem., 1994, 111, 52.
14. D. M. Poojary, A. Cabeza, M. A. G. Aranda, S. Bruque and A. Clearfield, Inorg. Chem., 1996, 35, 1468.
15. W. I. F. David, Accuracy in Powder Diffraction, NIST Special Publication no. 846, 1992, 210.
16. I. C. Madsen and R. J. Hill, J. Appl. Crystallogr., 1994, 27, 385.
17. P. L. Dupont and O. Dideberg, Acta Crystallogr., Sect. B, 1970, 26, 1884.
18. A. Boultif and D. Louer, J. Appl. Crystallogr., 1991, 24, 987.
19. M. M. Eddy, A. K. Cheetham and W. I. F. David, Zeolites, 1986, 6, 449.
20. L. W. Finger, D. E. Cox and A. P. Jephcoat, J. Appl. Crystallogr., 1994, 27, 892.
21. W. I. F. David, R. M. Ibberson and J. C. Matthewman, Rutherford Appleton Laboratory Report RAL-92-032, 1992.
22. C. J. Gilmore and S. R. Brown, J. Appl. Crystallogr., 1988, 21, 571.
23. G. A. Jeffrey and W. Saenger, Hydrogen Bonding in Biological Structures, Springer-Verlag, Berlin, 1991.
24. M. Tremayne, B. M. Kariuki and K. D. M. Harris, J. Mater. Chem., 1996, 6, 1601.
25. Y. G. Andreev, P. Lightfoot and P. G. Bruce, Chem. Commun., 1996, 2169.