X-Ray Diffraction Laboratory

Anion-bound cryptate snow crystal
The X-ray diffraction laboratory is located in the Graham Oldham building and a computer cluster for structural analysis is on the second floor of the Chemistry building.
Our facilities and other useful links are described under the following headings:

Instrumentation
Crystallography Training
Single Crystal Sample Submission
Crystallography Databases and Useful Links
Chemistry Department Homepage

Instrumentation

The X-ray diffraction laboratory is equipped with:

A Bruker APEXII single crystal diffractometer, operating at low temperature (150K)
A Rigaku AFC7 four circle single crystal diffractometer
A Bruker D8 powder diffractometer with Anton Parr HTK 1200 furnace attachment
A Philips Xpert powder diffractometer

$ApexII diffractometer$

Bruker APEXII Single Crystal Diffractometer (left)

The crystal for which data are being collected is mounted on a glass fibre on the end of the brass pin at the centre of the picture. The crystal size is generally of the order of 0.10 - 0.25 mm. The X-ray beam comes in horizontally from the right and is scattered by the crystal. The diffracted beams are collected by the CCD detector on the left. The crystal is cooled to 150K by a stream of cold nitrogen gas delivered by the vertical tube.

In addition to work using our in-house diffractometers, we have made use of synchrotron radiation sources at the Daresbury (RIP) and the ALS (Advanced Light Source) at Berkely for single crystal studies on small molecules.

Descriptions of projects involving significant amounts of single crystal structure analysis can be found on the webpages of:

Dr Mark Elsegood or Prof Vickie McKee.

$d8 diffractometer$
Bruker D8 Powder Diffractometer (right)

Up to 9 microcrystalline powder samples can be loaded into the automatic sample changer (the horizontal rack) and analysed sequentially. The X-ray beam comes in from the top left and strikes the sample, which is rotated in its sample-holder. The diffracted X-rays are collected by the position-sensitive detector on the right.

Descriptions of projects involving significant amounts of powder diffraction analysis can be found on the webpages of:

Dr Sandie Dann or Dr Caroline Kirk

Crystallography Training

Training in diffraction techniques is available for interested postgraduate students (or staff); contact Sandie Dann or Caroline Kirk in connection with powder diffraction and Mark Elsegood or Vickie McKee in connection with single crystal studies. Regular tutorial/problem-solving sessions are held in the department.
Before you can be authorised to use the diffraction equipment yourself, you must also complete the University Radiation Training and Safety forms. These can be found at:

Single Crystal Sample Submission

Structural studies also contribute significantly to the work of a many of other groups in the chemistry department. In the period 2009-11 approximately 50% of the papers published in refereed journals by members of the department contained single crystal structure determinations. Dr Elsegood and Prof McKee work with other groups inthe department and outside on a collaborative basis. A form for submission of single crystal samples is available in here in word format. Please fill it in as completely as possible.

Crystallography Databases and Useful Links

Crystallographic Databases

Crystallographic data for small molecules are archived in the Cambridge Structural Database Centre (CCDC) and/or the Inorganic Crystal Structure Database (ICSD). Protein structures can be accessed from the World Wide Protein Data Bank (wwPDB).
Academics and research students in UK universities can access the CCDC and ICSD (and other databases) via the Chemical Database Service (CDS), where you will find also instructions on how to register and use these databases.