The Laue technique is suitable to study effects that depend on wavelength such as absorption, anomalous dispersion or secondary extinction. The accuracy of the measured integrated intensities for X-ray structure determination is comparable with measurements of conventionally collected data. The present paper describes and discusses the results of a single-crystal data collection with a Laue diffractometer. The results obtained from the Laue data are in very good agreement with the results from conventionally collected data.
IntroductionThe availability of synchrotrons as white-radiation X-ray sources of high spectral brilliance is the reason for recent developments in Lane diffraction techniques for data collection, especially in the field of protein crystallography. Several two-dimensional detector systems are in use, such as films (e.g. Rabinovich & Lourie, 1987), image plates (e.g. Miyahara, Takahashi, Amemiya, Kamiya & Satow, 1986), multiwire proportional chambers (e.g. Baru et al., 1978), the FAST system (Bartunik & Borchert, 1989) and others (International Tables for Crystallography, 1992).Since it is the primary intention in this field to increase the speed of data collection, less attention is paid to the accuracy of a single measurement. Only one attempt (Sakamaki, Hosoya & Fukamachi, 1980) has been made to incorporate the Laue technique into an ordinary four-circle-diffractometer device. The present authors reported in a series of short communications on the hardware development of devices suitable for this purpose (Lange & Burzlaff, 1991a,b).It is the intention of this paper to report first results on the basis of a medium-sized inorganic structure, to compare the data with a data set collected in the classical way and to discuss the results and the technique in comparison with the work of Sakamaki et al.
Measurement of integrated intensitiesSingle-crystal X-ray diffraction with white radiation differs from the monochromatic technique in the following ways:1. Instead of one well defined Ewald sphere with radius R = l/A, a continuous distribution of Ewald spheres with Rmin ~ R < Rmax is present resulting in a simultaneous diffraction process for a large number of reciprocal-lattice vectors hi. Each vector hi selects its own Ewald sphere depending on its position in the reciprocal space.For the simultaneous registration of the reflections, a two-dimensional detector is necessary that allows the angular localization of the diffracted beams. In addition, the wavelength distribution within the diffracted beam has to be known. Approximately 17% (Cruickshank, Helliwell & Moffat, 1987) of all diffracted beams contain a series of nA related to the scattering vectors nh of the reflection (n = 1, 2, 3 .... ).2. In contrast to the conventional monochromatic technique, a property of the crystal is utilized in another way. With the model for a real crystal composed of small mosaic blocks, the end point of the scattering vector h must be replaced by a small fragment of a spherical surface. Its shape is d...