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TopSpin

TopSpin. TopSpin Training Course, 22 nd November 2006. Overview. Introduction to TopSpin Acquiring data through IconNMR Processing data Plotting/storing data Interpretation – a worked example Questions. What is the same?.

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TopSpin

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  1. TopSpin TopSpin Training Course, 22nd November 2006

  2. Overview • Introduction to TopSpin • Acquiring data through IconNMR • Processing data • Plotting/storing data • Interpretation – a worked example • Questions

  3. What is the same? • Before looking at the new features it is worth mentioning what has not changed in TopSpin: • Parameters and Data format: you can still process TopSpin data with XWINNMR (not from AVII hardware) • Most text commands are either the same or aliased to the equivalent TopSpin command (i.e. you still type efp, …) • IconNMR has a few new features, but broadly remains the same – automation users will not need re-training, and most will never notice any difference! • XWINPLOT is essentially the same, so if you are already using it in xwinnmr you are ready for TopSpin Plot Editor!

  4. What is New? • Integrated data browser • Command line history (and concatenation) • Configurable interface • Full support for handling multiple datasets • New interactive tools for Phasing, Integration, Peak Picking,… • Interactive guides (acquisition, processing, relaxation,…) • Acquisition status bar and tools • Extendable via AU programs, Python programs, etc. (including access to user interface) • …and much much more!

  5. Acquiring Data • Sample preparation is key • Selecting the right experiment: • What information do you need? • Which experiment(s) will give you this information?

  6. IconNMR

  7. Manipulating your experiment

  8. H H H H H H H H H H H H CH3 C C C OH H H H H OH H2C C C C OH OH OH H CH2 C C C H H H H H H H H H H H Main types of experiment H H

  9. O 2 5 4 1 6 O 3 M e M e 2 3 5 1 6 Example of a PROTON spectrum 3H t J = 7.1 Hz 1H dq J = 6.9, 15.5 Hz 3H dd J =1.7, 6.9 Hz 2H q J =7.1 Hz 1H dq J =1.7, 15.5 Hz

  10. 1/6 4 2/3 2/3 5 O 2 5 4 1 6 O 3 M e M e Example of CARBON spectra

  11. O 2 5 1 6 4 O 3 M e M e Example of a COSY spectrum 2 3 5 1 6

  12. M e M e O 2 5 1 6 4 O 3 Example of an HSQC spectrum 2 3 5 1 6

  13. O 2 5 4 1 6 O 3 M e M e Example of an HMBC experiment 2 3 5 1 6

  14. An introduction to processing • Most spectra run through IconNMR will be processed (and perhaps printed) already • You could simply open the processed spectrum and look at the data • You could reprocess - fundamentally: • multiplier, Fourier transform and phase (more on this later) • Then you can integrate, peak pick, calibrate etc.

  15. Hz or ppm datasets Y-scale Measure distance grid See later… All Retain scale Last expansion Data Display Buttons File handling, print,copy/paste, last 1D/2D/3D Horizontal position Vertical position Vertical scale Horizontal scale • Buttons seen will depend upon data-type (1D or 2D), and any customisation!

  16. Processing 1D data • Processing guide (automatic/manual) • Processing -> Data Processing Guide • Command line automatic: “xaup” – this will probably also print a spectrum • Command line manual: em, ft, apk/apks • Button: if you have one set up…. …of course you could set one up…

  17. Processing 2D data • Processing guide (automatic/manual) • Processing -> Data Processing Guide • Command line automatic: “xaup” – this will probably also print a spectrum • Command line manual: xfb, abs1, abs2 • Button: if you have one set up…. … of course you could set one up …

  18. Other Buttons – interactive menus calibration peak picking multiple display zoom overview integration baseline correction phase correction

  19. “screen dump” Output • Printer icon • File -> Print • Ctrl P

  20. Worked example 1H spectrum DMSO

  21. HSQC CH2 CH CH3

  22. HSQC expansion 1 CH CH3 CH2

  23. 6 7 3 5 4 2 COSY 1

  24. HMBC 3 1 C 6 5 4 7 2 CH CH3 CH2 C

  25. 2D NOESY 2 C 1 6 3 5 4 7

  26. 1 3 5 6 2 2D NOESY expansion B C A

  27. 1D selective NOESY C B 1 A 5 6 3 2 4 7

  28. Interpretation summary • Techniques • 13C NMR • DEPT variations • 1H NMR • COSY • HSQC/HMQC • HMBC • NOESY (1D and 2D) • Key Uses • Chemical environment, carbon count • Multiplicity determination • Chemical environment, quantification • Spin-spin coupled nuclei • Directly bonded 1H and 13C • 1H and 13C correlation across multiple bonds • Interactions through space

  29. Summary • Think about data you need … don’t waste instrument time by submitting every sample for all experiments • Remember sometimes you can obtain C13 chemical shifts from combination of 2D spectra when sample is limited • Use processing guides !! • Remember you can create a button for tasks you often repeat • “Save” is implicit in TopSpin – any processing changes you make will be remembered for next time • “Prnt” gives you quick and dirty screen dump • Plot Editor gives you pretty spectra for hard/electronic copy • ………….any questions??

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