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Department of Chemistry

Crystallography

Enquiries should be addresses to the service manager, Dr. Dmitry Yufit

Email: d.s.yufit@durham.ac.uk
Phone: +44 (0) 191 334 2004

Crystal structure analysis is one of the most powerful techniques for elucidating molecular and solid state structures, as well as characterising materials. Molecular geometry is afforded with unprecedented accuracy and intermolecular interactions can be analysed.

The Department is a recognised centre of excellence in crystallography and attracts collaborations from all over the world, due to its unique range of instrumentation. We have collaborated successfully with multinational companies and smaller local businesses, although we serve primarily the needs of the chemistry department and advance the method through our extensive research activities. The crystallography service is closely associated with Professor J.A.K. Howard's research group, and Ph.D. applications are welcome.

The single crystal diffraction facilities include two Bruker SMART-CCD, a Nonius KappaCCD and a Rigaku Spider Image Plate diffractometers . Samples can be measured at temperatures as low as 10 K for solving structures with reduced thermal motion. In addition, samples can be subjected to high pressures, high temperatures and laser irradiation to study a variety of unusual phenomena.

The service provides crystal structure determinations at temperatures between 10K-800K. Air sensitive, extremely air sensitive, light sensitive, low melting crystalline compounds and in-situ crystallization of liquids can be handled. Several pieces of equipment, listed here, are available for this purpose:

1) SMART-1K, SMART-6K and Kappa-CCD area detector diffractometers.

These diffractometers allow fast screening of samples. A routine data collection will last between 8hrs and 24hrs and it will be carried out at 120K unless otherwise requested.

Working temperatures can easily be between 90K-500K and temperatures between 30K-90K and 500K-800K can also be achieved for special/interesting cases. Samples are visible and accessible at all times during the experiment allowing, for example, data collections with the sample under laser irradiation. These diffractometers have a Molybdenum target X-ray source producing X-rays with a wavelength of 0.71073 Angstroms.

2) Fddd four circle cryodiffractometer

This diffractometer is mainly used for special research projects but it can be used for service samples when there is a special interest in a structure determination at very low temperatures (<30K). Data collections are possible at T=10K-300K. Samples are 'hidden' inside 2 Be cans and under vacuum. Very sensitive samples are more difficult to handle but not impossible. A similar instrument but integrated to a Bruker-APEX II CCD area detector and a Bruker microfocus TXS rotating anode will be commisioned in summer 2008. This new instrument will also allow measurements down to 2K, while simultaneously allowing high pressure and/or light irradiation of the samples.

In addition, X-ray powder diffraction of polycrystalline samples at temperatures between 17K-1200K is also available. The powder diffraction facilities include four Bruker powder diffractometers equipped with sample changer, PSD detectors and low and high temperature stages. It is also possible to perform experiments under laser irradiation while at temperatures as low as 17K as well as carry out measurements in capillary, flat, transmission, reflection modes. Phase identification and quantitative analysis are possible using this equipment. Contact Dr. Goeta for more information on this service.

A new single crystal area detector diffractometer equipped with a Copper high intensity microfocused X-ray source for the measurement of proteins will be commissioned at the end of 2008.

Single crystals growing service for X-ray analysis

is provided for small molecular substances preferably pharmaceutical compounds including polymorphs, pseudo polymorphs (hydrates or solvates) and co-crystals. Single crystals are grown from small (0.2-0.5 g) samples of pure crystalline materials stable at ambient conditions. Single crystals and their structure are obtained within a week excluding complicated cases.

Confidentiality is guaranteed. For further details, please, contact sin.cryst@durham.ac.uk