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Examination of Single Crystals: Optical and X-Ray Diffraction Practice

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Book cover Structure Determination by X-ray Crystallography

Abstract

The preliminary optical examination of crystalline specimens is interesting and useful in its own right and is a major tool still employed by mineralogists and geologists. However, in structure determinations with modern equipment, it is not uncommon nowadays to by-pass this step and proceed immediately with X-ray studies. This is because in most cases, the X-ray technique is straightforward and test data can be quickly scanned with a single-crystal X-ray diffractometer, Sects. 5.5 and 5.6, or with area detector (see Sect. 5.7), and the suitability and quality of the crystal assessed. There are other situations, however, where complications may arise, for example, because of an unusual crystal habit, Sect. 5.3.5, pseudosymmetry, Sects. 7.2.2, 7.5.4, and Sect. 8.5.3, or twinning, Sect. 5.10. In such cases, it might be possible to extract useful information from an optical examination of a crystal before the more detailed, costly and time-consuming X-ray methods are tried.

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Notes

  1. 1.

    Similar to Geiger counters.

  2. 2.

    Hamamatsu Photonics KK C10158DK.

  3. 3.

    http://www.bruker-axs.com/x8_proteum.html

  4. 4.

    http://www.bruker-axs.com/chemical_crystallography.html.

  5. 5.

    http://www.rigaku.com/smc/scxmini.html.

References

  1. Bibliography, Gay (1967); Hartshorne and Stuart (1970)

    Google Scholar 

  2. See Bibliography, Buerger MJ (2009)

    Google Scholar 

  3. Ladd M, Palmer R (2003) Structure determination by X-ray crystallography, 4th edn. Kluwer Academic, New York

    Book  Google Scholar 

  4. http://www.bruker-axs.com/spacegroupdetermination.html

  5. See Bibliography, Jeffrey

    Google Scholar 

  6. Arndt UW, Wonacott AJ (eds) (1977) The rotation method in crystallography. North-Holland, Amsterdam

    Google Scholar 

  7. Mar Research (MAR IP) Norderstedt, Germany

    Google Scholar 

  8. Miyahara J et al (1986) Nucl Instrum Methods A246:572

    CAS  Google Scholar 

  9. Boyle W, Smith G (1970) Charge coupled semiconductor devices. Bell Syst Tech J 49:587

    Google Scholar 

  10. Einstein A (1905) Ann Phys 17:132

    Article  CAS  Google Scholar 

  11. Gruner SM (1994) Curr Opin Struct Biol 4:765

    Article  CAS  Google Scholar 

  12. Westbrook EM, Naday I (1987) Methods Enzymol 276:244

    Article  Google Scholar 

  13. Jones C (2001) Chem Commun 2293

    Google Scholar 

  14. Deacon A et al (1997) J Chem Soc Farad Trans 93:4305

    Article  CAS  Google Scholar 

  15. Walter RL et al (1995) Structure 3:835

    Article  CAS  Google Scholar 

  16. http://www.nonius.com

  17. http://www.bruker-axs.com

  18. Oxford Cryosystems,http://www.oxcryo.com

  19. Prince SM, Bryant PK (private communication) Manchester University

    Google Scholar 

  20. Brönnimann Ch et al (2004) Synchrotron Radiat News 17:23

    Article  Google Scholar 

  21. Brönnimann Ch et al (2006) J Synchrotron Radiat 13:120–130

    Article  Google Scholar 

  22. http://www.dectris.ch/sites/products.html

  23. http://www.dexela.com

  24. Plugrath JW (1999) Acta Crystallogr D55:1718

    Google Scholar 

  25. Otwinowski Z, Minor W (2001) ‘Denzo’ and ‘Scalepack 211’. in Arnold, E et al. (2012) (eds) International Tables for Crystallography, vol. F, I.U.Cr.

    Google Scholar 

  26. Leslie A (1993) Data collection and processing. In: Sawyer L, Isaacs N, Bailey S (eds) Proceedings of the CCP4 study weekend. Daresbury Laboratories, Warrington, UK, pp 44–51

    Google Scholar 

  27. Rossmann MG, van Beek CG (1999) Acta Crystallogr D55:1631

    CAS  Google Scholar 

  28. Sanderson MR (2007) Macromolecular crystallography conventional and high-throughput methods, Chapter 5. Oxford University Press, Oxford

    Google Scholar 

  29. Yarris Lynn, lcyarris@lbl.gov

    Google Scholar 

  30. http://www.xtl.ox.ac.uk/equip.html

  31. http://people.mbi.ucla.edu/sawaya/m230d/Data/data.html

  32. Freund AK (1996) Structure 4:155

    Article  Google Scholar 

  33. Franks A (1955) Proc Phys Soc London B68:1054

    Google Scholar 

  34. Bloomer AC, Arndt UW (1999) Acta Crystallogr D55:1672

    CAS  Google Scholar 

  35. http://www.lcm3b.uhp-nancy.fr/mathcryst/twins.htm

  36. http://xrayweb.chem.ou.edu/notes/twin.html

  37. http://www.bruker-axs.com/d8_advance.html

  38. http://www.rigaku.com/downloads/journal/Vol12.2.1995/raxisiv.pdf

Bibliography: Crystal Optics

  • Gay P (1967) An introduction to crystal optics. Longmans, London

    Google Scholar 

  • Hartshorne NH, Stuart A (1970) Crystals and the polarising microscope. Arnold, London

    Google Scholar 

X-Ray Scattering and Reciprocal Lattice

  • Arndt UW, Wonacott AJ (eds) (1977) The rotation method in crystallography: data collection from macromolecular crystals. North-Holland, Amsterdam

    Google Scholar 

  • Buerger MJ (2009) X-ray crystallography, 11th edn. Wiley, New York

    Google Scholar 

  • Jeffrey JW (1971) Methods in X-ray crystallography. Academic, London

    Google Scholar 

  • Woolfson MM (1997) An introduction to X-ray crystallography, 2nd edn. Cambridge University Press, Cambridge

    Book  Google Scholar 

Interpretation of X-Ray Diffraction Photographs

  • Henry NFM, Lipson H, Wooster WA (1960) The interpretation of X-ray diffraction photographs. Macmillan, London

    Google Scholar 

  • Jeffery JW (1971) Methods in X-ray crystallography. Academic, London

    Google Scholar 

Precession Method

  • Buerger MJ (1964) The precession method. Wiley, New York

    Google Scholar 

  • Ladd MFC, Palmer RA (2003) Structure determination by X-ray crystallography, 4th edn. Kluwer Academic, New York

    Book  Google Scholar 

Diffractometry

  • Arndt UW, Willis BTM (1966) Single crystal diffractometry. Cambridge University Press, Cambridge

    Book  Google Scholar 

Cryo-Crystallography

Macromolecular Crystallography

  • Carter CW Jr, Sweet RM (eds) (1997) Macromolecular crystallography. Academic, New York

    Google Scholar 

  • Arnold, E et al. (2012) (eds) International Tables for Crystallography, vol. F, I.U.Cr.

    Google Scholar 

Data Collection

Data Collection Services

  • The EPSC National Data Collection Service (University of Southampton) will collect, process, and optionally solve crystal structures (but there’s not much fun in that) for clients who supply suitable crystals. In a recent use of this service the following facilities were used

    Google Scholar 

  • Diffractometer: Nonius Kappa CCD Area Detector (φ scans and ω scans to fill the asymmetric unit sphere)

    Google Scholar 

  • Cell determination: DirAx (Duisenberg AJM (1992) J Appl Crystallogr 25:92)

    Google Scholar 

  • Data collection: Collect (Data collection software, Hooft R, Nonius BV (1998))

    Google Scholar 

  • Data reduction and cell refinement: Denzo (Otwinowski Z, Minor W (1997) Methods Enzymol 276); Macromol Crystallogr, loc. cit.

    Google Scholar 

  • Absorption correction: SORTAV (Blessing RH (1995) Acta Crystallogr A51:33); idem., J Appl Crystallogr 30:421 (1997)

    Google Scholar 

  • Structure solution: SHELXS-97 (Sheldrick GM (1990) Acta Crystallogr A46:467)

    Google Scholar 

  • Structure refinement: SHELXL-97 (Sheldrick GM (1997) University of Göttingen)

    Google Scholar 

  • Graphics: ORTEP3 for windows (Farrugia LJ (1997) J Appl Crystallogr 30:365)

    Google Scholar 

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Ladd, M., Palmer, R. (2013). Examination of Single Crystals: Optical and X-Ray Diffraction Practice. In: Structure Determination by X-ray Crystallography. Springer, Boston, MA. https://doi.org/10.1007/978-1-4614-3954-7_5

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