Automated chemical crystallography

Amy Fuller; Lindesay Alexandra Sarah Scott-Hayward; Yang Li; Michael Buehl; Alexandra Martha Zoya Slawin; J Derek Woollins

doi:10.1021/ja100247y

Automated chemical crystallography

Amy Fuller, Lindesay Alexandra Sarah Scott-Hayward, Yang Li, Michael Buehl, Alexandra Martha Zoya Slawin, J Derek Woollins

Research output: Contribution to journal › Article › peer-review

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.

Original language	English
Pages (from-to)	5799-5802
Number of pages	4
Journal	Journal of the American Chemical Society
Volume	132
Issue number	16
Early online date	2 Apr 2010
DOIs	https://doi.org/10.1021/ja100247y
Publication status	Published - 28 Apr 2010

Keywords

Absolute-configuration
Crystal-structure
Crystallization
Dichalcogenides

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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
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@article{b4c835eeb9dc429c905f58b35c2f25c8,

title = "Automated chemical crystallography",

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.",

keywords = "Absolute-configuration, Crystal-structure, Crystallization, Dichalcogenides",

author = "Amy Fuller and Scott-Hayward, \{Lindesay Alexandra Sarah\} and Yang Li and Michael Buehl and Slawin, \{Alexandra Martha Zoya\} and Woollins, \{J Derek\}",

year = "2010",

month = apr,

day = "28",

doi = "10.1021/ja100247y",

language = "English",

volume = "132",

pages = "5799--5802",

journal = "Journal of the American Chemical Society",

issn = "0002-7863",

publisher = "American Chemical Society (ACS)",

number = "16",

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TY - JOUR

T1 - Automated chemical crystallography

AU - Fuller, Amy

AU - Scott-Hayward, Lindesay Alexandra Sarah

AU - Li, Yang

AU - Buehl, Michael

AU - Slawin, Alexandra Martha Zoya

AU - Woollins, J Derek

PY - 2010/4/28

Y1 - 2010/4/28

N2 - 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.

AB - 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.

KW - Absolute-configuration

KW - Crystal-structure

KW - Crystallization

KW - Dichalcogenides

UR - https://www.scopus.com/pages/publications/77952577172

U2 - 10.1021/ja100247y

DO - 10.1021/ja100247y

M3 - Article

SN - 0002-7863

VL - 132

SP - 5799

EP - 5802

JO - Journal of the American Chemical Society

JF - Journal of the American Chemical Society

IS - 16

ER -

Automated chemical crystallography

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Structural Mechanostereochemistry: International Collaboration in Chemistry: Structral Mechanostereochemistry of Mechanically interlocked Polymers and Networks

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Automated chemical crystallography

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Structural Mechanostereochemistry: International Collaboration in Chemistry: Structral Mechanostereochemistry of Mechanically interlocked Polymers and Networks

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