Single crystal diffraction at the Rossendorf Beamline/ESRF

Christoph Hennig^a, Eleanor Lawrence Bight^a, Michael Bodensteiner^b_, Florian Meurer^b, Florian Kleemiss^c

^aRossendorf Beamline (BM20), European Synchrotron Radiation Facility, 71, Avenue des Martyrs, 38043 Grenoble, France, and Institute of Resource Ecology, Helmholtz-Zentrum Dresden-Rossendorf, Bautzner Landstrasse 400, 01314 Germany, ^bFaculty for Chemistry and Pharmacy, University of Regensburg, Universitätsstrasse 31, 93053 Regensburg, Germany, ^cInstitute for Inorganic Chemistry, RWTH Aachen, Landoltweg 1a, 52074 Aachen, Germany

e-mail: hennig@esrf.fr

Single crystal measurements at a synchrotron benefit from a slightly focussed beam, a very high intensity and a freely tunable wavelength [1]. Very small crystals can be measured, occasionally structures with strong disorder can be solved and resonant effects can be investigated [2]. On the other hand, some disadvantages should not remain unmentioned, such as the fact that radiation damage can easily occur and that the detector can easily become saturated due to high counting rates. Excellent data can be obtained if these problems are taken into consideration during the planning and conduction of the measurement.

We would like to present the current status of the diffractometer at the Rossendorf Beamline (ROBL, BM20) at ESRF and how we do single crystal diffraction. The diffractometer consists of a heavy optical bench with an exchangeable Huber kappa goniometer and a Pilatus3 X 2M detector. It is used for single crystal diffraction, in situ or operando powder measurements and Grazing Incidence diffraction. The diffractometer is controlled with the Pylatus software [3]. The single crystal data extraction is performed with Crysis [3] and CrysAlisPro [4]. A Si drift detector can be placed in different positions to combine diffraction with XRF and XAS measurements. Devices for non-ambient sample conditions are a LN2 cryostream (90-400K), a hot-air blower (RT-1100K), a heating chamber (RT-1470K) [1].

References

[1] Scheinost, A.; Claußner, J.; Exner, J.; Feig, M.; Findeisen, S.; Hennig, C.; Kvashnina, K.; Naudet, D.; Prieur, D.; Roßberg, A.; Schmidt, M.; Qiu, C.; Colomp, P.; Cohen, C.; Dettona, E.; Dyadkin, V.; Stumpf, T. Journal of Synchrotron Radiation 28 (2021) 333 – 349.

[2] Meurer, F., Dolomanov, O.V., Hennig, C., Peyerimhoff, N., Kleemiss, F., Puschmann, H., Bodensteiner, M. IUCrJ 9 (5) (2022) 604-609.

[3] Dyadkin V., Pattison P., Dmitriev V., Chernyshov D. A new multipurpose diffractometer PILATUS @ SNBL. J. Synchrotron Rad. 23 (2016) 825-829.

[4] CrysAlisPro Software System, Rigaku Diffraction (http://www.rigaku.com).