High-Pressure Crystallography pp 57-68 | Cite as
High-Pressure Single-Crystal Diffractometry with Laboratory X-Ray Sources
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 ReflectionPreview
Unable to display preview. Download preview PDF.
References
- 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.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.Arndt, U.W. and Willis, B.T.M. (1966) Single Crystal Diffractometry, University Press, Cambridge.CrossRefGoogle Scholar
- 4.Van Valkenburg, A. (1964) Diamond high–pressure windows, Diamond Research, 17–20.Google Scholar
- 5.Fourme, R. (1968) Appareillage pour etudes radiocrystallographiques sous pression et à temperature variable, J. Appl. Ciystallogr. 1, 23–30.CrossRefGoogle Scholar
- 6.Tkacz, M. (1995) Novel high–pressure technique for loading diamond anvil cell with hydrogen, Polish J. Chem. 69, 1205–1209.Google Scholar
- 7.Holzapfel, W.B. and Isaacs N.S. (Eds.) High–Pressure Techniques in Chemistry and Physics, Oxford University Press, Oxford 1997.Google Scholar
- 8.Hazen, R.T. and Finger, L.W. (1982) Comparative Crystal Chemistry, John Wiley & Sons, New York.Google Scholar
- 9.King, H.E.Jr. (1981). High-Pressure Crystallography with a CAD-4, Enraf-Nonius, Delft.Google Scholar
- 10.Ahsbahs, H. (1987) X-Ray diffraction on single crystals at high pressure, Prog. Crystal Growth and Charact. 14, 263–302.CrossRefGoogle Scholar
- 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.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.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.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.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.Katrusiak, A. (2002) Absorption correction for crystal-environment attachments from direction cosines, Z. Kristallogr. 216, 646–647.CrossRefGoogle Scholar
- 17.Katrusiak, A. (1999) A hinge goniometer head, J. Appl. Crystallogr. 32, 576–578.CrossRefGoogle Scholar
- 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.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.Dera, P. and Katrusiak, A. (1999) Diffractometric crystal centring, J. Appl. Crystallogr. 32, 510–515.CrossRefGoogle Scholar
- 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.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.Katrusiak, A. and Ryan, T.W. (1988). Homogeneity of graphite-monochromated X-ray beams, Acta Crystallogr. A44, 623–627.Google Scholar
- 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.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.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.Kumakhov, M.A. and Komarov, F.F. (1990) Multiple reflection from surface X-ray optics, Phys. Rep. 191, 289–350.ADSCrossRefGoogle Scholar
- 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.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.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.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.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.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.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.Katrusiak, A. (1995) High-pressure X-ray diffraction study of pentaerithritol, Acta Cryst. B51, 873–879.Google Scholar
- 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.Ibraimov, N.S., Kumakhov, M.A. and Lutsu, A.V. (2003) Personal communication.Google Scholar
- 38.Katrusiak, A. (1993) High-Pressure X-ray Diffraction studies on organic crystals, Cryst. Struct. Technology 26, 523–531.CrossRefGoogle Scholar
- 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.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.Katrusiak, A. (2004). Shadowing and absorption corrections for single-crystal high-pressure diffraction measurements - being published.Google Scholar
- 42.Seal, M. (1984) Diamond anvils, High Temperatures – High Pressures 16, 573–579.Google Scholar
- 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.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.Pasternak, M.P. (2001) — personal communication.Google Scholar
- 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