International
Tables for
Crystallography
Volume F
Crystallography of biological macromolecules
Edited by E. Arnold, D. M. Himmel and M. G. Rossmann

International Tables for Crystallography (2012). Vol. F, ch. 8.1, pp. 194-195   | 1 | 2 |

Section 8.1.6. SR instrumentation

J. R. Helliwella*

aDepartment of Chemistry, University of Manchester, M13 9PL, England
Correspondence e-mail: john.helliwell@manchester.ac.uk

8.1.6. SR instrumentation

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The divergent continuum of X-rays from the source must be intercepted by the sample cross-sectional area. The crystal sample acceptance, as seen above, is a good way to illustrate to the machine designer the sort of machine emittances required. Likewise, the beamline optics, mirrors and monochromators should not degrade the X-ray beam quality. Mirror surface and shape finish have improved a great deal in the last few decades; slope errors of mirrors, even for difficult shapes like polished cylinders, which on bending give a toroidal reflecting surface, are now around 1 arc second (5.5 µrad) for a length of 1 m. Thus, over focusing distances of 10–20 m, say, the focal-spot smearing contribution from this is 55–110 µm, important for focusing onto small crystals. Further optics developments (e.g. Fresnel optics) have yielded micron focus beams and smaller, and are being applied to studying ever-smaller crystals in macromolecular crystallography and obviously have a variety of other diffraction and spectroscopy applications [for a review, see Riekel (2000)[link]]. The choice of materials has evolved, too, from the relatively easy-to-work-with and -finish fused quartz to silicon; silicon having the advantageous property that at liquid-nitrogen temperature the expansion coefficient is zero (Bilderback, 1986)[link]. This has been of particular advantage in the cooling of silicon monochromators at the ESRF, where the heat loading on optics is very high. An alternative approach with the rather small X-ray beams from undulators is the use of transparent monochromator crystals made of diamond, which is a robust material with the additional advantage of transparency, thus allowing multiplexing of stations, one downstream from the other, fed by one straight section of one or more undulator designs. For a review of the ESRF beamline optics, see Freund (1996)[link]; for reviews of the macromolecular crystallography programmes at the ESRF, see Miller (1994)[link], Branden (1994[link]) and Lindley (1999)[link], as well as the ESRF Foundation Phase Report (1987)[link]. See also Helliwell (1992)[link], Chapter 5.

Detectors have improved enormously. The early days of SR use saw considerable reliance on photographic film, as well as single-counter four-circle diffractometers. Evolution of area detectors, in particular, has been considerable and impressive, and in a variety of technologies. Gas detectors, i.e., the multiwire proportional chamber (MWPC), were invented and developed through various generations and types [Charpak (1970)[link]; for reviews of their use at SR sources, see e.g. Lewis (1994)[link] and Fourme (1997)[link]]. MWPCs have the best detector quantum efficiency (DQE) of the area detectors, but there are limitations on count rate (local and global) and their use at wavelengths less than ~1 Å is restricted due to geometric image parallax effects. The most popular devices at present are charge coupled devices (CCDs) [see Tate et al. (1995[link]), Allinson (1994)[link], Gruner & Ealick (1995[link]) and Westbrook & Naday (1997[link]) for details of their development]. Image plates (IPs) were popular during the late 1980s and early to mid-1990s, mainly, but not exclusively, with online scanners, notably the MAR Research devices. IPs are also used in a Weissenberg geometry [see Sakabe (1983[link], 1991[link]) and Sakabe et al. (1995[link]), and for a recent review see Amemiya (1997[link])]. IPs and CCDs are complementary in performance, especially with respect to size and duty cycle; IPs are larger, i.e., with many resolution elements possible, but are slower to read out than CCDs. Both are capable of imaging well at wavelengths shorter than 1 Å and with high count rates. Both have overcome the tedium of chemical development of film. Other detectors needed for crystallography include those for monitoring the beam intensity; these must not interfere with the beam collimation, and yet must monitor the beam downstream of the collimator (Bartunik et al., 1981[link]); also needed are fluorescence detectors for setting the wavelength for optimized anomalous-scattering applications (see Cianci et al., 2005[link]).

Most recently, an area-detector development has been the so-called pixel detector. This is made of silicon cells, each `bump bonded' onto associated individual electronic readout chains. Thus, extremely high count rates are possible. These devices can then combine the attributes of large image plate sensitive areas with the fast readout of CCDs, along with high count-rate capability and so on. Devices and prototypes have been developed at Princeton/Cornell (Eikenberry et al., 1998[link]), Berkeley/San Diego (Beuville et al. 1997[link]) and Imperial College, London (Hall, 1995[link]), and are now in use at the SLS (Broennimann et al., 2006[link]).

Provision of robotics for sample mounting on the synchrotron beamlines has been increasingly deployed in the last decade, improving efficiency and ease of use, often coupled with remote access (e.g. see Gonzalez et al., 2005[link]) and telepresence (e.g. see Warren et al., 2008[link]).

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