Cryo crystal structure determination and application to intermediates

Abstract

Ever since Wilhelm Conrad Röntgen discovered X-rays a century ago and von Laue, Friedrich, Knipping, Braggs and Braggs developed an analytical method almost nine decades ago, single crystal structure analysis has become the most powerful analytical tool used to elucidate unequivocally the three dimensional structure of solid matter. New X-ray detectors like image plates or CCD-detectors permit the collection of two datasets a day. However, this recent development should not only result in a higher ‘turn-over’ of crystal structure determinations, but should also be utilized in new research approaches. One can think of monitoring chemical reactions in terms of Echtzeit crystallography. The challenge is to synthesize, crystallize and analyze reaction intermediates by cryo crystal structure determination. Alkali organometallic compounds are omnipresent in any chemical laboratory where they are used as highly reactive starting materials in a vast number of reactions. It would be of great use to be able to freeze out intermediates along a reaction pathway in order to deduce new synthetic routes and concepts from the structural knowledge obtained by single crystal structure determinations.