High-Pressure Single-Crystal Diffractometry with Laboratory X-Ray Sources

High-pressure structural determinations at home laboratories
  • A. Katrusiak
Conference paper
Part of the NATO Science Series book series (NAII, volume 140)

Abstract

The invention of the diamond-anvil high-pressure cell (DAC) [ 1,2] coincided with the development of 4-circle diffractometers [3]. When the application of gaskets paved the way for the first single-crystal high-pressure studies in hydrostatic environment [4], diffractometers were still not considered indispensable for determining the crystal structures at high pressures. For example, the high-pressure crystal structure of chloroform was studied using a modified precession camera [5]. Nevertheless, soon after it was the use of 4-circle diffractometers that came to dominate the scarce high-pressure determinations. The diffractometers then were usually equipped with sealed or rotating-anode X-ray tubes and ‘single-point’ scintillator-photomultiplier detectors. Throughout the 1980’s, the first synchrotron-sources were applied for high-pressure studies, and at the synchrotrons, 2dimensional image-plate detectors started to be used for high-pressure determinations. Nowadays we are witnessing rapid development in the designs of high-pressure DAC’s and diffractometers, which are now routinely equipped with 2-dimensional CCD detectors. Thus, in this way, history has come full circle, in that researchers trained in photographic techniques have applied their experience to 2-dimensional detectors. The component parts of diffractometric equipment, which itself is constantly under development, include sophisticated detectors, X-ray sources, goniometers and their controlling software. At present it may appear that the main thrust of high-pressure research has moved to synchrotrons.

Keywords

Primary Beam Beam Divergence Mosaic Spread Goniometer Head Ofthe Reflection 
These keywords were added by machine and not by the authors. This process is experimental and the keywords may be updated as the learning algorithm improves.

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References

  1. 1.
    Jamieson, J.C., Lawson, A.W. and Nachtrieb, N.D. (1959) New device for obtaining X–ray diffraction patterns from substances exposed to high pressure, Rev. Sci. Instrum. 30, 1016–1019ADSCrossRefGoogle Scholar
  2. 2.
    Weir, C.E., Lippincott, E.R., Van Valkenburg, A. and Bunting, E.N. (1959) Infrared studies in the 1– to 15micron region to 30,000 atmospheres, J Res. Nat. Bur. Standards, Sec. A63, 55–62.CrossRefGoogle Scholar
  3. 3.
    Arndt, U.W. and Willis, B.T.M. (1966) Single Crystal Diffractometry, University Press, Cambridge.CrossRefGoogle Scholar
  4. 4.
    Van Valkenburg, A. (1964) Diamond high–pressure windows, Diamond Research, 17–20.Google Scholar
  5. 5.
    Fourme, R. (1968) Appareillage pour etudes radiocrystallographiques sous pression et à temperature variable, J. Appl. Ciystallogr. 1, 23–30.CrossRefGoogle Scholar
  6. 6.
    Tkacz, M. (1995) Novel high–pressure technique for loading diamond anvil cell with hydrogen, Polish J. Chem. 69, 1205–1209.Google Scholar
  7. 7.
    Holzapfel, W.B. and Isaacs N.S. (Eds.) High–Pressure Techniques in Chemistry and Physics, Oxford University Press, Oxford 1997.Google Scholar
  8. 8.
    Hazen, R.T. and Finger, L.W. (1982) Comparative Crystal Chemistry, John Wiley & Sons, New York.Google Scholar
  9. 9.
    King, H.E.Jr. (1981). High-Pressure Crystallography with a CAD-4, Enraf-Nonius, Delft.Google Scholar
  10. 10.
    Ahsbahs, H. (1987) X-Ray diffraction on single crystals at high pressure, Prog. Crystal Growth and Charact. 14, 263–302.CrossRefGoogle Scholar
  11. 11.
    Miletich, R., Allan, D.R. and Kuhs, W.F. (2000) High-pressure single-crystal techniques, Reviews in Mineralogy and Geochemistry 41, 445–519.CrossRefGoogle Scholar
  12. 12.
    Angel, R.J., Downs, R.T. and Finger, L.W. (2000) High–temperature—high-pressure diffractometry, Reviews in Mineralogy and Geochemistry 41, 559–596.CrossRefGoogle Scholar
  13. 13.
    Kuhs, W.F., Bauer, F.C., Hausmann, R., Ahsbahs, H., Dorwarth, R. and Hölzer, K. (1996) Single crystal diffraction with X-rays and neutrons: high quality at high pressure? High Pressure Res. 14, 341–352.ADSCrossRefGoogle Scholar
  14. 14.
    Malinowski, M. (1987) A diamond-anvil high-pressure cell for X-ray diffraction on a single crystal, J. Appl. Crystallogr. 20, 379–382.CrossRefGoogle Scholar
  15. 15.
    Merrill, L. and Bassett, W.A. (1974) Miniature diamond anvil pressure cell for single crystal X-ray diffraction studies, Rev. Sci. Instrum. 45, 290–294.ADSCrossRefGoogle Scholar
  16. 16.
    Katrusiak, A. (2002) Absorption correction for crystal-environment attachments from direction cosines, Z. Kristallogr. 216, 646–647.CrossRefGoogle Scholar
  17. 17.
    Katrusiak, A. (1999) A hinge goniometer head, J. Appl. Crystallogr. 32, 576–578.CrossRefGoogle Scholar
  18. 18.
    Hamilton, W.C. (1974) Angle settings for four–circle diffractometers, in International Tables for X–ray Crystallography, Vol. IV, Birmingham: Kynoch Press (Present distributor: Kluwer Academic Publishers, Dordrecht). pp 273–284.Google Scholar
  19. 19.
    King, H.E.Jr. and Finger, L.W. (1979) Diffracted beam crystal centering and its application to high–pressure crystallography, J. Appl. Crystallogr. 12, 374–378.CrossRefGoogle Scholar
  20. 20.
    Dera, P. and Katrusiak, A. (1999) Diffractometric crystal centring, J. Appl. Crystallogr. 32, 510–515.CrossRefGoogle Scholar
  21. 21.
    Paciorek, W.A., Meyer, M. and Chapuis, G. (1999) On the geometry of a modern imaging diffractometer, Acta Cryst. A55, 543–557.Google Scholar
  22. 22.
    Budzianowski, A. and Katrusiak, A. (2003). High-pressure crystallographic experiments with a CCD detector. in High-Pressure Crystallography (Eds.: A. Katrusiak and P.F. McMillan), Kluwer, Dordrecht, pp. 101–112.Google Scholar
  23. 23.
    Katrusiak, A. and Ryan, T.W. (1988). Homogeneity of graphite-monochromated X-ray beams, Acta Crystallogr. A44, 623–627.Google Scholar
  24. 24.
    Stern, E. A. Kalman, Z. Lewis,. and Lieberman, K. (1988) Simple method for focusing X-rays using tapered capillaries, Appl. Opt. 27, 5135–5139.ADSCrossRefGoogle Scholar
  25. 25.
    Balaic, D.X., Nugent, G.A., Barnea, Z., Garrett, R. and Wilkins, S.W. (1995) Focusing of X-ray by total external reflection from a paraboloidally tapered glass capillary, J. Synchrotron Rad. 2, 295–299.CrossRefGoogle Scholar
  26. 26.
    Balaic, D.X., Barnea, Z., Nugent, G.A., Garrett, R., Varghese, J.N. and Wilkins, S.W. (1995) Protein crystal diffraction patterns using a capillary-focused synchrotron X-ray beam, J. Synchrotron Rad. 3, 289–295.CrossRefGoogle Scholar
  27. 27.
    Kumakhov, M.A. and Komarov, F.F. (1990) Multiple reflection from surface X-ray optics, Phys. Rep. 191, 289–350.ADSCrossRefGoogle Scholar
  28. 28.
    Li, P.-W. and Bi, R.-C. (1998) Applications of polycapillary X-ray optics in protein crystallography, J. Appl. Crystallogr. 31, 806–811.CrossRefGoogle Scholar
  29. 29.
    Gubarev, M., Ciszak, E., Ponomarev, I., Gibson, W. and Joy, M. (2000) A compact X–ray system for macromolecular crystallography, Rev. Sci. Instrum. 71, 3900–3904.ADSCrossRefGoogle Scholar
  30. 30.
    Coppens, P., Ross, F.K., Blessing, R.H., Cooper, W.F., Larsen, F.K., Leipoldt, J.G. and Rees, B. (1974) A cryostat for collection of three-dimensional diffractometer data at liquid helium temperatures, Acta. Cryst. 7, 315–319.Google Scholar
  31. 31.
    Konno, M., Okamoto, T., Shirotani, I. (1989) Structure changes and proton transfer between 0...0 in bis(dimethylglyoximato)platimum(II) at low temperature (150K) and at high pressures (2.39 and 3.14 GPa) Acta Cryst. B45, 142–147.Google Scholar
  32. 32.
    Yamanaka, T., Fukuda, T., Hattori, T. and Sumiya, H, (2001) New diamond anvil cell for single-crystal analysis, Rev. Sci. Instrum. 72, 1458–1462.ADSCrossRefGoogle Scholar
  33. 33.
    Loveday, J.S., McMahon, M.I. and Nelmes, R.J. (1990) The effect of diffraction of a diamond-anvil cell on single-crystal sample intensities, J. Appl. Crystallogr. 23, 392–396.CrossRefGoogle Scholar
  34. 34.
    Zhang, Li and Ahsbahs, H. (1998) New pressure domain in single crystal X-ray diffraction using a sealed source, Rev. High Pressure Sci. Technol. 7, 145–147.MATHCrossRefGoogle Scholar
  35. 35.
    Katrusiak, A. (1995) High-pressure X-ray diffraction study of pentaerithritol, Acta Cryst. B51, 873–879.Google Scholar
  36. 36.
    Yaoita, K., Katayama, Y., Tsuji, K., Kikegawa, T., and Shimomura, O. (1997) Angle-dispersive diffraction measurement system for high-pressure experiments using a multichannel collimator, Rev. Sci. Instrum. 68, 2106–2110.ADSCrossRefGoogle Scholar
  37. 37.
    Ibraimov, N.S., Kumakhov, M.A. and Lutsu, A.V. (2003) Personal communication.Google Scholar
  38. 38.
    Katrusiak, A. (1993) High-Pressure X-ray Diffraction studies on organic crystals, Cryst. Struct. Technology 26, 523–531.CrossRefGoogle Scholar
  39. 39.
    Katrusiak, A. and Nelmes, R.J. (1986) A test of the accuracy of high-pressure measurements using a MerrillBassett diamond–anvil cell, J. Appl. Cryst. 19, 73–76.CrossRefGoogle Scholar
  40. 40.
    Von Dreele, R.B. and Hanson, R.C. (1984) Structure of NH3–III at 1.28 GPa and room temperature, Acta Cryst. A40, 1635–1638.Google Scholar
  41. 41.
    Katrusiak, A. (2004). Shadowing and absorption corrections for single-crystal high-pressure diffraction measurements - being published.Google Scholar
  42. 42.
    Seal, M. (1984) Diamond anvils, High Temperatures – High Pressures 16, 573–579.Google Scholar
  43. 43.
    Silvera, I.F. (1999) The double-diamond anvil cell, the poor-man’s megabar pressure cell, Rev. Sci. Instrum. 70, 4609–4611.ADSCrossRefGoogle Scholar
  44. 44.
    Dadashev, A., Pasternak, M.P., Rozenberg, G.Kh. and Taylor, R.D. (2001) Applications of perforated diamond anvils for very high–pressure research, Rev. Sci. Instrum. 72, 2633–2637.ADSCrossRefGoogle Scholar
  45. 45.
    Pasternak, M.P. (2001) — personal communication.Google Scholar
  46. 46.
    Duisenberg, A.J.M., Hooft, R.W.W. Schreurs, A.M.M. and Kroon, J. (2000) Accurate cells from area-detector images, J. Appl. Crystallogr. 33, 893–898.CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media New York 2004

Authors and Affiliations

  • A. Katrusiak
    • 1
  1. 1.Faculty of ChemistryAdam Mickiewicz UniversityPoznańPoland

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