Hostname: page-component-78c5997874-94fs2 Total loading time: 0 Render date: 2024-11-14T18:10:09.558Z Has data issue: false hasContentIssue false
  • English
  • Français

UACIEM: A new method to extract reliable intensities of nonequivalent systematical overlapping reflections from powder diffraction data

Published online by Cambridge University Press:  05 March 2012

H. W. Ma ,
J. K. Liang ,
G. Y. Liu  and
G. H. Rao
H. W. Ma*
Affiliation:
Institute of Physics & Center for Condensed Matter Physics, Chinese Academy of Sciences, Beijing 100080, China
J. K. Liang*
Affiliation:
Institute of Physics & Center for Condensed Matter Physics, Chinese Academy of Sciences, Beijing 100080, Chinaand International Center for Materials Physics, Academia Sinica, Shenyang 110015, China
G. Y. Liu
Affiliation:
Institute of Physics & Center for Condensed Matter Physics, Chinese Academy of Sciences, Beijing 100080, China
G. H. Rao
Affiliation:
Institute of Physics & Center for Condensed Matter Physics, Chinese Academy of Sciences, Beijing 100080, China
*
a)Electronic mail: hwma@aphy.iphy.ac.cn
b)Electronic mail: jkliang@aphy.iphy.ac.cn
Get access Rights & Permissions [Opens in a new window]

Abstract

A new method, namely UACIEM, to extract reliable intensities of nonequivalent systematical overlapping reflections has been proposed and tested by simulated powder diffraction data from known crystal structures. Using both crystallographic and structural chemistry information, the method reconstructs diffraction intensities and solves a crystal structure through an iterative procedure. Our study shows that UACIEM is successful for cases where more than 30% of the total scattering power is located with precision from equivalent systematical overlapping reflections. The UACIEM process is not needed when equivalent systematical overlapping reflections are sufficient to reveal a crystal structure. UACIEM may fail in cases when: (i) only a small portion of the total scattering power (e.g., less than 7%) can be located, and (ii) most of the total scattering power (e.g., 95%) is located, but the atomic coordinates are not accurately known. The UACIEM method is superior to the simple equipartition methods for nonequivalent systematical overlapping reflections.

Keywords

nonequivalent systematical overlapping reflectionUACIEMstructure determination
Type
Selected Papers from 2003 Chinese National Symposium on XRD
Information
Powder Diffraction , Volume 19 , Issue 4 , December 2004 , pp. 333 - 339
Copyright
Copyright © Cambridge University Press 2004

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Cheetham, A. K. and Wilkinson, A. P. (1991). “Structure Determination and Refinement with Synchrotron X-ray Powder Diffraction Data,” J. Phys. Chem. Solids JPCSAW 10, 1199–1208.CrossRefGoogle Scholar
Davaid, W. I. F. (1990). “Extending the Power of Powder Diffraction for Structure Dtermination,” Nature (London) NATUAS 346, 731–734.CrossRefGoogle Scholar
Davaid, W. I. F. (1987). “The Probabilistic Determination of Intensities of Overlapping Reflections in Powder Diffraction Patterns,” J. Appl. Crystallogr. JACGAR 20, 316–319.CrossRefGoogle Scholar
Estermann, M. A. and Gramlich, V. (1993). “Improved Treatment of Severely or Exactly Overlapping Bragg Reflections for the Application of Direct Methods to Powder Data,” J. Appl. Crystallogr. JACGAR 26, 396–404.CrossRefGoogle Scholar
Estermann, M. A., Mccusker, L. B., and Baerlocher, C. (1992). “Ab Initio Structure Determination from Severely Overlapping Powder Diffraction Data,” J. Appl. Crystallogr. JACGAR 25, 539–543.CrossRefGoogle Scholar
Giacovazzo, C. (1996). “Direct Methods and Powder Data: State of the Art and Perspectives,” Acta Crystallogr., Sect. A: Found. Crystallogr. ACACEQ A52, 331–339.CrossRefGoogle Scholar
Harder, S., Prosenc, M. H., and Rief, U. (1996). “Syntheses and X-ray Structures of Anionic Sodocence Sandwiches,” Organometallics ORGND7 15, 118–122.CrossRefGoogle Scholar
Harris, K. D. M., Tremayne, M., and Kariuki, B. M. (2001). “Contemporary Advances in the Use of Powder X-ray Diffraction for Structure Determination,” Angew. Chem., Int. Ed. ACIEF5 40, 1626–1651.3.0.CO;2-7>CrossRefGoogle ScholarPubMed
Harris, K. D. M. and Tremayne, M. (1996). “Crystal Structure Determination from Powder Diffraction Data,” Chem. Mater. CMATEX 8, 2254–2570.CrossRefGoogle Scholar
Jansen, J., Peschar, P., and Schenk, H. (1992). “On the Determination of Accurate Intensities from Powder Diffraction Data. II. Estimation of Intensities of Overlapping Reflections,” J. Appl. Crystallogr. JACGAR 25, 237–243.Google Scholar
Khalili, M. M., Bodak, O. I., Marusin, E. P., and Pecharskaya, A. O. (1990). “Crystal Structure of Er4Ni13C4 and U2W4C4,” Kristallografiya KRISAJ 35, 337–341.Google Scholar
Le Bail, A. (1994–2002). “Structure Determination from Powder Diffraction—Database,” http://www.cristal.org.Google Scholar
Le Bail, A., Duroy, H., and Fourquet, J. L. (1988). “Ab Initio Structure Determination of LiSbWO6 by X-ray Powder Diffraction,” Mater. Res. Bull. MRBUAC 23, 447–452.Google Scholar
Liang, J. K. (2003). Crystal Structure Determination from Powder Diffraction Data, 1st ed. (Science Press, Beijing).Google Scholar
Louër, D. (1998). “Advances in Powder Diffraction Analysis,” Acta Crystallogr., Sect. A: Found. Crystallogr. ACACEQ 54, 922–933.CrossRefGoogle Scholar
Newmann, M. A., Leusen, F. J. J., Engel, G. E., and Conesa-Moratilla, C. (2002). “Recent Advances in Structure Solution from Powder Diffraction Data,” Int. J. Mod. Phys. A IMPAEF 16, 407–414.Google Scholar
Pawley, G. A. (1981). “Unit Cell Refinement from Powder Diffraction Scans,” J. Appl. Crystallogr. JACGAR 14, 357–361.CrossRefGoogle Scholar
Poojary, D. M. and Clearfield, A. (1997). “Application of X-ray Powder Diffraction Techniques to the Solution of Unknown Crystal Structures,” Acc. Chem. Res. ACHRE4 30, 414–422.CrossRefGoogle Scholar
Popov, A. I., Val kovskii, M. D., Kiselev, Y. M., Chumaevskii, N. A., Sokolov, V. B., and Spirin, S. N. (1990). “Structure of Flouroaurates(V) Earth Alkaili Elenents,” Zh. Neorg. Khim. ZNOKAQ 35, 1770–1777.Google Scholar
Porob, D. G. and Row, T. N. G. (2001). “Ab Initio Structure Determination via Powder X-ray Diffraction,” Proc.-Indian Acad. Sci., Chem. Sci. PIAADM 113, 435–444.CrossRefGoogle Scholar
Sasaki, Y. (1969). “The Crystal Structure of Diamminecdmium(II) Tetracyanoniccolate(II) Benzen Clathrate, Cd(NH3)2Ni(CN)4∙2C6H6,” Bull. Chem. Soc. Jpn. BCSJA8 142, 2412–2415.CrossRefGoogle Scholar
Sheldrick, G. M. (1997). User manual of SHELX-97.Google Scholar
Vickery, G. C., Olmsted, M. M., Fung, E. Y., and Balch, A. L. (1997). “Solvent Stimulated Luminescence from the Superamolecular Aggregation of the Trinuclear Gold(I) Complex that Displays Extensive Intermolecular Au–Au Interactions,” Angew. Chem., Int. Ed. Engl. ACIEAY 36 1179–1180.CrossRefGoogle Scholar
Wessels, T., Baerlocher, C., and Mccusker, L. B. (1999). “Single-Crystal-Like Diffraction Data from Polycrystalline Materials,” Science SCIEAS 284, 475–478.Google Scholar
Yvon, K., Jeitschko, W., and Parthé, E. (1977). “LAZY PULVERIX, A Computer Program for Calculating X-ray and Neutron Diffraction Powder Patterns,” J. Appl. Crystallogr. JACGAR 10, 73–74.CrossRefGoogle Scholar
Zubkov, V. G., Perelyaev, B. A., Berger, I. F., Kontsevaya, I. A., Makarova, O. V., Turzhevskii, S. A., and Gubanov, V. A. (1990). “One Dimensional Clusters of Niobium Monooxide in Ba0.5Nb5O8,” Sverkhprovodimost: Fiz., Khim., Tekh. SFKTE6 3, 2121–2126.Google Scholar