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New in Bruker User Library: Manchester Experiments

A new contribution to our online user library (The Resonance Exchange) has just been made available by Peter Kiraly, Ralph W. Adams, James Montgomery, Mathias Nilsson and Gareth A. Morris from the NMR Methodology Group of the University of Manchester. It features an extensive collection of pulse programs, au macros and parameter files for setting up experiments that include various pure shift (i.e. homodecoupled) and diffusion NMR methods. The new experiments are also made available in the Experiment Selector, facilitating their selection and setup (see Fig. 1).

Figure 1

Fig. 1. The Manchester Experiments in the Experiment Selector.

Many experiments are compatible with automatic update by WaveMaker (wvm). Any valid WaveMaker waveform definition can be used (e.g. userA1 = rsnob). The shaped pulse parameters can be easily changed and updated by using cnst50 for the effective bandwidth definition; in automation (xaua) the au_wvm macro provided automatically calls WaveMaker.

The pure shift HSQC experiments include a hardware protection feature. High F2 resolution HSQC experiments require a relatively long acquisition time (AQ); this is needed to take full advantage of pure shift acquisition, but can be dangerous due to the use of high power broadband decoupling. The pulse program files and setup au macros include a maximum limit for the power used, which should be adjusted to the safe limit for a given probe/spectrometer.  Using WaveMaker with appropriate parameter settings, adiabatic 13C decoupling can be optimised to minimise sample heating.

Fig. 2. Pure shift NMR spectra of 16β-estradiol in dmso-d6 acquired using the band-selective interferogram method (a) with and (b) without SAPPHIRE, and (d) broadband Zangger-Sterk method with (c/e) excerpts from conventional 1H spectrum.  The periodic sidebands, marked by red asterisks in (b), are completely suppressed in (a).

Compatibility

The pulse program codes were developed on an Avance Neo spectrometer running TopSpin 4. With the exception of the real-time HSQC and semi-real-time pure shift experiments it is expected to be compatible with legacy Avance systems and TopSpin 3.

The experiments in this package are described in detail in reference [1-13].

References

[1] K. Zangger and H. Sterk J Magn Reson, 1997, 124, 486-489.

[2] Juan A. Aguilar, Stephen Faulkner, Mathias Nilsson, and Gareth A. Morris Angew. Chem. Int. Ed.

2010, 49, 3901-3903.

[3] Foroozandeh M, Adams RW., Kiraly P, Nilsson M, Morris GA. Chem.Commun. 2015, 15410-15413.

[4] Foroozandeh M, Morris GA., Nilsson M Chem.Eur.J. 2018, 24, 13988-14000.

[5] Moutzouri, P.; Chen, Y.; Foroozandeh, M.; Kiraly, P.; Phillips, A. R.; Coombes, S. R.; Nilsson, M.;

Morris, G. A. Chem. Commun. 2017, 53, 10188-10191.

[6] Pelta, MD, Morris, GA, Stchedroff, MJ and Hammond, SJ. Magnetic Resonance in Chemistry

40(13):S147-S152.

[7] Kiraly, P.; Swan, I.; Nilsson, M.; Morris, G.A. J. Magn. Reson. 2016, 270, 24-30.

[8] Botana, A., Aguilar, J. A., Nilsson, M., Morris, G. A. J. Magn. Reson. 2011, 208, 270-278.

[9] P. Kiraly, Nilsson M , Morris GA. Magn.Reson.Chem. 2018, 56, 993-1005

[10] P. Kiraly et al, J.Biomol.NMR. 2015, Vol. 62, 43-52.

[11] L. Paudel et al, Angew.Chem.Int.Ed. 2013, Vol. 125, 11830-11833.

[12] Concilio, M. G.; Kiraly, P.; Morris, G. A. J. Magn. Reson., 2019, 301, 85-93.

[13] Kiraly, P.; Nilsson, M.; Morris, G. A. J. Magn. Reson., 2018, 293, 19-27.

The Bruker online User Library, the Resonance Exchange is an online platform that allows Bruker users to share their latest developments. The User Library can be accessed from the following site: (https://www.bruker.com/service/information-communication/nmr-pulse-program-lib/bruker-user-library.html). The readers are encouraged to share their own latest developments with the vast community of the Bruker users via the Resonance Exchange.