Automated Single Crystal Structure Determination – A Tool for … · 2014-02-03 · and its...
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3 5 1 4 2 ? cis/trans L/S ... ... Diffraction signal found? ! Determine space group(s) Data acquisition, collect and integrate remaining reflections, store all data on CD-ROM User Input Project name Formula sum Crystal description (optional) Color, Shape, Size Expose sample to X-rays Determine mosaicity, resolution, exposure time, index and refine Index& refinement successful? Data acquisition collect and integrate 180 degree Spot shape, resolution, R(int) OK? Good spot shapes Low Rint, few rejections after scaling Space group(s) found? Iterate over space groups, solve and refine structure R1<10%? Validate structure Generate comprehensive report Data acquisition Structure determination Report generation User input Crystal quality check Automated Single Crystal Structure Determination – A Tool for Synthetic Chemists? Bernd Hinrichsen a , Martin Adam a , Michael Carr b , Dieter Schollmeyer c , a Bruker AXS GmbH, Karlsruhe, Germany b Bruker UK Ltd, Coventry, United Kingdom c Johannes Gutenberg University, Institute of Organic Chemistry, Mainz, Germany E-mail: [email protected] Order Number DOC-P86-EXS023 © 2010 Bruker AXS GmbH. Printed in Germany. SC-XRD During recent years large improvements in software functionality and its ease-of-use have made single crystal X-ray structure determination easier than ever. These days most structures can be measured, processed, solved and refined using well selected defaults with no or little crystallographic knowledge. Recently, microfocus sources and CCD detectors both air-cooled, have entered the marketplace. Combining these innovations with an automated sample loader and an intelligent graphical user interface allows for the design of a table top single crystal diffractometer, which only requires a standard single phase power connection and no cooling water at all. An instrument taking advantage from these software and hardware developments would enable synthetic chemists or pharmacists to perform a complete single crystal structure analysis almost next to the reaction flask. [1] The authors are grateful to Prof. Dr. Stefan Laufer, Eberhard- Karls-University, Tübingen, Germany, for providing the samples. Performance analysis results To compare the system performance a family of p38 MAP kinase inhibitors was crystallized and measured on the SMART X2S. Data were collected on a state of the art research instrument (SMART APEXII) and a previous generation rotating anode instrument (CAD4). The data collection time and the resulting quality can be gleaned from the tables below. All structures were solved and refined automatically by the SMART X2S diffractometer. It is clear that the SMART X2S has a superior performance over the previous generation system and shows very competitive performance in comparison to the state-of-the art research instrument.
Transcript of Automated Single Crystal Structure Determination – A Tool for … · 2014-02-03 · and its...
3
5
1
4
2
?cis/transL/S......
Diffraction signal found?
!Determine space
group(s)
Data acquisition, collect and integrate remaining reflections, store all data
on CD-ROM
User InputProject nameFormula sum
Crystal description (optional)Color, Shape, Size
Expose sample to X-rays
Determinemosaicity, resolution,
exposure time, index and refine
Index& refinement successful?
Data acquisition collect and integrate
180 degree
Spot shape, resolution,
R(int) OK?
Good spot shapes
Low Rint, few rejections after scaling
Space group(s) found?
Iterate over space groups, solve and
refine structure
R1<10%?Validate structure
Generate comprehensive
report
Data acquisition
Structure determination
Report generation
User input
Crystal quality check
Automated Single Crystal Structure Determination – A Tool for Synthetic Chemists? Bernd Hinrichsena, Martin Adama, Michael Carrb, Dieter Schollmeyerc, aBruker AXS GmbH, Karlsruhe, GermanybBruker UK Ltd, Coventry, United KingdomcJohannes Gutenberg University, Institute of Organic Chemistry, Mainz, GermanyE-mail: [email protected]
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-P86
-EX
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0 B
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. Prin
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in G
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any.
SC-XRD
During recent years large improvements in software functionality and its ease-of-use have made single crystal X-ray structure determination easier than ever. These days most structures can be measured, processed, solved and refined using well selected defaults with no or little crystallographic knowledge. Recently, microfocus sources and CCD detectors both air-cooled, have entered the marketplace. Combining these innovations with an automated sample loader and an intelligent graphical user interface allows for the design of a table top single crystal diffractometer, which only requires a standard single phase power connection and no cooling water at all. An instrument taking advantage from these software and hardware developments would enable synthetic chemists or pharmacists to perform a complete single crystal structure analysis almost next to the reaction flask.
[1] The authors are grateful to Prof. Dr. Stefan Laufer, Eberhard-Karls-University, Tübingen, Germany, for providing the samples.
Performance analysis resultsTo compare the system performance a family of p38 MAP kinase inhibitors was crystallized and measured on the SMART X2S. Data were collected on a state of the art research instrument (SMART APEXII) and a previous generation rotating anode instrument (CAD4). The data collection time and the resulting quality can be gleaned from the tables below. All structures were solved and refined automatically by the SMART X2S diffractometer. It is clear that the SMART X2S has a superior performance over the previous generation system and shows very competitive performance in comparison to the state-of-the art research instrument.
