Variable temperature experiments made easy with automated software

Variable temperature experiments made easy with automated software S. J. Coles*, M. B. Hursthouse, S. L. Huth & M. E. Light*. School of Chemistry, University of Southampton, SO 17 1 BJ. UK. ; Email: [email protected]. ac. uk The software Why automate? Cryogui is a graphical user interface that links the operation of a Kappa. CCD and an Oxford Cryosystems Cryostream. The code is written in PYTHON and utilises the ability of a Kappa CCD to interface with a cryostream, and the accessibility of the Bruker-Nonius COLLECT data collection modules, classes and functions. The user is able to select the start and end temperatures (going either up or down), the ramp step and rate and a wait time to allow the cryostream to stabilise. To enable the system to work it is necessary to connect the cryostream to the server PC serial port via an RS 232 cable and then set the cryostream type and port number in the Server Software. Variable temperature experiments have, in the past, involved a large amount of operator input and effort. As a result many interesting results may have been missed or found only as a result of serendipity. In Southampton this situation has been addressed by the development of inhouse software to perform such variable temperature experiments in a fully automated manner. This enables variable temperature experiments to be carried out without manually changing the temperature and setting up the experiment. Configure data collection parameters The types of experiment that can be carried out include thermal dehydration of compounds such as zeolites, parametric studies to look for effects like negative thermal expansion, phase transition location, and investigation of temperature dependant ion migration. Start data collection Visualise and manipulate data After a data set has been collected it is automatically integrated and scaled to produce an hkl file. Other output includes an html file containing all the unit cell dimensions (useful when just running unit cell determinations) and the same information in a tab delimited file readable by excel. Test case Sample 300 -166 -1 exhibited unusual, temperature dependent, physical properties when investigated by Differential Scanning Calorimetry. Pna 21 Cmc 21 Temp 1 Pna 21 Temp 2 Pna 21 Temp 3 Cmc 21 Temp 4 Temp 5