Single crystal Xray diffraction Dr Georgina Rosair Lab

Single crystal X-ray diffraction Dr Georgina Rosair Lab: G. 06/7 Ground floor below crush area

Power of crystallography • Crystals <1 mm long • Complete 3 D structure

Crystal growing tips – PURIFY your compound as much as is practically possible. – FILTER the solution you will grow the crystals from – TEST THE CRYSTALS are they the RIGHT compound – Remove a few crystals to see if they lose solvent and examine them by infrared, nmr etc. – Grow the crystals SLOWLY and with the MINIMUM of vibration - a fridge is a good place. – PERSEVERE - you may need to try several methods

Crystal growing methods • Solvent diffusion – Dissolve your compound in a solvent in which it is soluble and layer slowly on top a second solvent in which it is almost insoluble. – The two solvents must be miscible. CH 2 Cl 2/hexane is a common combination. – Nmr samples have been used successfully

When you have crystals, what do you do? • Completed forms into the pocket on the Xray notice board outside G. 07 • Contact number – lab phone no & HW email • LABELLED Samples in the analytical services fridge/freezer in the 200 m. Hz NMR room

X-ray crystallography and your research • • Structure solution and refinement Access to databases Pictures and tables for reports and papers X-seed software you can download and use on your laptop • Advice and training from me

Crystallographic results