Automated chemical crystallography

The first fully automated small-molecule robotic X-ray diffractometer is described. After demonstrating the utility of the instrument using multiple samples of ammonium bitartrate, we investigated the conformational chirality of diphenyl dichalcogenide (E2Ph2, where E = S, Se, or Te). Structural and computational studies suggest that the two enantiomers are energetically indistinguishable. Therefore, it was unsurprising that we found (in 35 suitable data collections) the proportion 0.51:0.49 of M-S2Ph2 to P-S2Ph2 in the bulk sample. Interestingly, after 65 data collections of Te2Ph2, (46 provided suitable data sets), we found the proportion 0.72 +/- 0.13 of M-Te2Ph2, suggesting there could be a statistically significant preference for the M-enantiomer in the sample examined here. We found that Se2Ph2 underwent homochiral crystallization, with all 24 crystals being M. Our experiments may represent a salutary lesson in statistical analysis.

Citation

Fuller , A , Scott-Hayward , L A S , Li , Y , Buehl , M , Slawin , A M Z & Woollins , J D 2010 , ' Automated chemical crystallography ' , Journal of the American Chemical Society , vol. 132 , no. 16 , pp. 5799-5802 . https://doi.org/10.1021/ja100247y

Publication

Journal of the American Chemical Society

Status

Peer reviewed

DOI

https://doi.org/10.1021/ja100247y

ISSN

0002-7863

Type

Journal article

Rights

This document is the Accepted Manuscript version of a Published Work that appeared in final form in Journal of The American Chemical Society, copyright © American Chemical Society after peer review and technical editing by the publisher. To access the final edited and published work see DOI: 10.1021/ja100247y

Collections

University of St Andrews Research

URI

http://hdl.handle.net/10023/1769