Single-Crystal X-Ray Diffractometry Using Synchrotron Radiation

Abstract

The properties of synchrotron radiation relevant to single-crystal X-ray diffractometry are: its high intensity over a wide spectral range, a small source size and a low divergence in the 0.1 mrad range, about 90% linear polarization in the horizontal plane, a pulsed time structure, and a time dependent intensity. The latter property requires monitoring of the primary beam intensity and its polarization state which slightly complicates data collection and needs particular attention in the data reduction stage. The other properties of synchrotron radiation, lowever, extend the range of X-ray diffractometry to experiments which are not feasable with sealed X-ray tubes. The high source intensity makes data collection possible on crystals down to and below 10 μm diameter. Measurement of weak and very weak ("forbidden") reflections profits from high intensity, low divergence, and a good peak-to-background ratio. Data collection at short wavelengths is useful to decrease both absorption and extinction effects and provides the resolution required for high precision structure analysis. Wavelength tunability is frequently used to exploit resonant X-ray scattering ("anomalous dispersion") for structure research. Examples are determination of absolute configuration, contrast variation, and phase determination from both singleand multiple-wavelength measurements ("MAD-phasing"). X-ray dichroism and double refraction are observed in the vicinity of absorption edges, causing an anisotropy and polarization dependence of anomalous scattering. This anisotropy may give rise to a violation of extinction rules for glide-planes and screw-axes, with orientation-and polarization-dependent intensities. More recently, these affects have been successfully used to derive (partial) phase information. Other applications are magnetic X-ray scattering and time-resolved X-ray diffraction, the latter exploiting the time structure of the synchrotron radiation source.

Instrumentation and Methods for Powder Diffraction with Synchrotron Radiation

“…Several single crystal diffraction methods (λ-method, Δ-synthesis, FRED, etc.) have been developed [12] which can be partially applied to powder diffraction. Recently a novel method has been introduced which allows the phase determination from powder data [13,14].…”

“…For the case of non-centrosymmetrical stuctures two different anomalous scatterers are needed and three measurements at different wavelengths must be performed. This general case is treated in [12].…”

Resonant Scattering of Light Atoms - Measuring Methods and Applications

“…The use of SR improves markedly the peak-tobackground ratio -owing to low vertical divergence and narrow wavelength bandpass Δλ/λ. It allows more precise measurements of high order reflections as well as weak high angle reflections [15].…”