Abstract
The crystal structures of normethisterone, gestonoronacetat, and griseofulvin were directly determined from the X-ray powder diffraction (XRPD) using the direct space approach by means of material studio (MS), the Rietveld refinement (RR), based on MS and generalized structural analysis system (GSAS) programs, was examined to practice and expand the Rietveld (whole-profile) technique in the pharmaceutical field. The RR converges to R wp=8.85%, 10.56%, and 5.92% for normethisterone (6.88%), gestonoronacetat (9.58%), and griseofulvin (5.24%), respectively. The crystallographic data obtained from the powder diffraction data were compared with the single-crystal X-ray diffraction (SXRD) data. The results showed that the maximum relative errors of lengths a, b, and c and volume were respectively 0.18%, 0.18%, 0.22%, and 0.39% between SXRD and XRPD. Thus, MS and GSAS programs were useful to powder diffractionists in determining the crystal structure of organic polycyclic molecules.
Article PDF
Similar content being viewed by others
References
Harris K D M. Powder diffraction crystallography of molecular solids. Top Curr Chem, 2012, 315: 133–177
Smith D K, Gorter S J. Powder diffraction program information. 1990 program list. 1990 program list. J Appl Crystallogr, 1991, 24: 369–402
Hu E P, Cheng Q, Guo L H, et al. Crystal structure determining of 7-ADCA based on X-ray powder diffraction. Chin Sci Bull, 2006, 51: 2421–2424
Lei X R, Yang J H, Lin X, et al. Crystal structure determination of Jatrorrhizine chloride. Chin Sci Bull, 2009, 54: 3244–3248
Guo P, Su Y H, Cheng Q, et al. Crystal structure determination of the β-cyclodextrin-p-aminobenzoic acid inclusion complex from powder X-ray diffraction data. Carbohydr Res, 2011, 346: 986–990
Young R A. The Rietveld Method. Oxford: International Union of Crystallography and Oxford University Press, 1993
Larson A C, Von Dreele R B. GSAS, Generalized structural analysis system, Document LAUR 86-748. Los Alamos National Laboratory, Los Alamos, NM, 1993
Rodriguez-Carvajal J. Fullprof: A program for Rietveld refinement and pattern matching analysis. In: Galy J, Louer D, eds. Satellite Meeting on Powder Diffraction of the 15th Congress of the IUCr. Toulouse: [sn], 1990. 127–128
TOPAS V3: General profile and structure analysis software for powder diffraction data. Bruker AXS, Karlsruhe, Germany, 2005
Rácz C P, Borodi G, Pop M M, et al. Structure of the inclusion complex of β-cyclodextrin with lipoic acid from laboratory powder diffraction data. Acta Crystallogr Sect B-Struct Sci, 2012, 68: 164–170
Pan Q Q, Guo P, Duan J, et al. Comparative crystal structure determination of griseofulvin: Powder X-ray diffraction versus single-crystal X-ray diffraction. Chin Sci Bull, 2012, 57: 3867–3871
Dolomanov O V, Bourhis L J, Gildea R J, et al. OLEX2: A complete structure solution, refinement and analysis program. J Appl Crystallogr, 2009, 42: 339–341
Neumann M A. X-cell: A novel indexing algorithm for routine tasks and difficult cases. J Appl Crystallogr, 2003, 36: 356–365
Boultif A, Louër D. Indexing of powder diffraction patterns for low-symmetry lattices by the successive dichotomy method. J Appl Crystallogr, 1991, 24: 987–993
Visser J W. A fully automatic program for finding the unit cell from powder data. J Appl Crystallogr, 1969, 2: 89–95
Werner P E, Eriksson L, Westdahl M. TREOR, a semi-exhaustive trial-and-error powder indexing program for all symmetries. J Appl Crystallogr, 1985, 18: 367–370
David W I F, Shankland K, McCusker L B, et al. Structure Determination from Powder Diffraction Data. Oxford: Oxford University Press, 2006
Shankland K, David W I F, Csoka T, et al. Structure solution of Ibuprofen from powder diffraction data by the application of a genetic algorithm combined with prior conformational analysis. Int J Pharm, 1998, 165: 117–126
Pawley G S. Unit-cell refinement from powder diffraction scans. J Appl Crystallogr, 1981, 14: 357–361
David V, Steven G L. A Monte Carlo simulated annealing approach to optimization over continuous variables. J Comput Phys, 1984, 56: 259–271
Brückner S. Estimation of the background in powder diffraction patterns through a robust smoothing procedure. J Appl Crystallogr, 2000, 33: 977–979
David W I F. Powder diffraction peak shapes. Parameterization of the pseudo-Voigt as a Voigt function. J Appl Crystallogr, 1986, 19: 63–64
Dollase W A. Correction of intensities for preferred orientation in powder diffractometry: Application of the March model. J Appl Crystallogr, 1986, 19: 267–272
Le Bail A, Duroy H, Fourquet J L. Ab-initio structure determination of LiSbWO6 by X-ray powder diffraction. Mater Res Bull, 1988, 23: 447–452
Sitepu H, O’Connor B H, Li D. Comparative evaluation of the March and generalized spherical harmonic preferred orientation models using X-ray diffraction data for molybdite and calcite powders. J Appl Crystallogr, 2005, 38: 158–167
Sheldrick M G. SHELXL-97: Program for Crystal Structure Refinement. Gottingen, Germany: University of Gottingen, 1997
Wondratschek H, Müller U. The International Union of Crystallography Volume A1: Symmetry Relations between Space Groups. Netherlands: Springer, 2004
Author information
Authors and Affiliations
Corresponding author
Additional information
This article is published with open access at Springerlink.com
Rights and permissions
This article is published under an open access license. Please check the 'Copyright Information' section either on this page or in the PDF for details of this license and what re-use is permitted. If your intended use exceeds what is permitted by the license or if you are unable to locate the licence and re-use information, please contact the Rights and Permissions team.
About this article
Cite this article
Wu, X., Tang, P., Pan, Q. et al. Crystal structure determination of three polycyclic compounds and comparative Rietveld refinement between MS and GSAS programs. Chin. Sci. Bull. 58, 2430–2434 (2013). https://doi.org/10.1007/s11434-013-5837-8
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s11434-013-5837-8