A straightforward and effective procedure to test for preferred orientation in polycrystalline samples prior to structure determination from powder diffraction data

Crystal Growth and Design

Volumn 3, Issue 5, 2003, Pages 705-710

  Cheung, Eugene Y ^a   Harris, Kenneth D M ^a   Foxman, Bruce M ^a,b  

^a UNIVERSITY OF BIRMINGHAM   (United Kingdom)

^b BRANDEIS UNIVERSITY   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

CRYSTALLIN;

ARTICLE; CHEMICAL STRUCTURE; CRYSTAL STRUCTURE; MATHEMATICAL COMPUTING; PHOTOGRAPHY; POWDER; X RAY DIFFRACTION;

EID: 0141851360     PISSN: 15287483     EISSN: None     Source Type: Journal    
DOI: 10.1021/cg0340796     Document Type: Article

References (18)

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2. Harris, K. D. M.; Tremayne, M. Chem. Mater. 1996, 8, 2554.
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5. Meden, A. Croat. Chem. Acta 1998, 71, 615.
6. Harris, K. D. M.; Tremayne, M.; Kariuki, B. M. Angew. Chem., Int. Ed. 2001, 40, 1626.
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9. Tremayne, M.; Kariuki, B. M.; Harris, K. D. M., manuscript in preparation.
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11. Altomare, A.; Cascarano, G.; Giacovazzo, C.; Guagliardi, A. J. Appl. Crystallogr. 1994, 27, 1045.
12. Peschar, R.; Schenk, H.; Capková, P. J. Appl. Crystallogr. 1995, 28, 127.
13. Wessels, T.; Baerlocher, C.; McCusker, L. B. Science 1999, 284, 477.
14. STOE Reciprocal Lattice Explorer: fiat film cassette placed in the position normally occupied for precession photography and positioned perpendicular to the incident X-ray beam (with μ = 0°); Ni-filtered CuKα radiation; generator settings, 40 kV, 20 mA; sample-to-film distance, 37 mm; typical exposure time, 45 min. Note that this instrument is normally used to record single-crystal X-ray diffraction photographs of either precession or de Jong-Bouman type.
15. 1 radiation; linear position-sensitive detector covering 8° in 2θ; step size Δ2θ = 0.0194°.
16. The comparison of experimental and calculated powder diffraction patterns in Figures 1b,c, 2b,c, 3b,c was made within the GSAS program [17] by fixing the fractional coordinates and atomic displacement parameters at those in the published structure of galvinoxyl [18] (determined from single-crystal X-ray diffraction at ambient temperature) and carrying out refinement of unit cell parameters, zero-point error, profile parameters (peak shape, peak width, and asymmetry) and overall scale factor.
17. Larson, A. C.; Von Dreele, R. B. Los Alamos Laboratory Rep. No. LA-UR-86-748, 1987.
18. Williams, D. E. Mol. Phys. 1969, 16, 141.