Single crystal X-ray diffraction

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Presentation transcript:

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

Power of crystallography Crystals <1mm long Complete 3D 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. CH2Cl2/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 X-ray notice board outside G.07 Contact number – lab phone no & HW email LABELLED Samples in the analytical services fridge/freezer in the 200mHz 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