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Automated chemical crystallography

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Abstract

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.

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Original languageEnglish
Pages (from-to)5799-5802
Number of pages4
JournalJournal of the American Chemical Society
Volume132
Issue number16
Early online date2 Apr 2010
DOIs
Publication statusPublished - 28 Apr 2010

    Research areas

  • Absolute-configuration, Crystal-structure, Crystallization, Dichalcogenides

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