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Ultrahigh resolution 1H-1H coupling measurement

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Organization
Abstract
Homonuclear scalar couplings are a double-edged sword. They deliver a wealth of structural information, but equally they are detrimental to spectral resolution, impeding their accurate measurement. One way to disentangle individual couplings from complex spectra is the SERF experiment, which delivers a 2D J-resolved spectrum containing only selected couplings [1]. A variant of this experiment, G-SERF, uses the Zangger-Sterk pulse sequence element to deliver simultaneously all the individual couplings to one selected resonance [2]. Other recent variants incorporate band-selective and Zangger-Sterk pure shift acquisition [3,4]. However, all these methods can break down in crowded spectra, either because of signal overlap or because chemical shift differences between coupled spins are too small. Here, we present the PSYCHEDELIC (Pure Shift Yielded by CHirp Excitation to DELiver Individual Couplings) experiment, derived from the PSYCHE pure shift method [5]. It delivers simultaneously all individual couplings to a selected proton, with minimal constraints on spectral overlap and chemical shift difference, with the usual high sensitivity and spectral purity of PSYCHE. [1] T. Facke, and S. Berger, J. Magn. Res. Ser. A, (1995), 113(1), 114-116. [2] N. Giraud, L. Beguin, J. Courtieu, and D. Merlet, Angew. Chem. Int. Ed., (2010), 49(20), 3481-3484. [3] J. E. H. Pucheta et al., Chem. Commun., (2015), 51(37), 7939-7942. [4] D. Pitoux, et al., Chem. Eur. J., (2015), 21(25), 9044-9047. [5] M. Foroozandeh, R. W. Adams, N. J. Meharry, D. Jeannerat, M. Nilsson, and G. A. Morris, Angew. Chem. Int. Ed., (2014), 53(27), 6990-6992.
Keywords
NMR spectroscopy

Citation

Please use this url to cite or link to this publication:

MLA
Sinnaeve, Davy, et al. “Ultrahigh Resolution 1H-1H Coupling Measurement.” FGMR 37th Annual Meeting, Abstracts, 2015.
APA
Sinnaeve, D., Foroozandeh, M., Nilsson, M., & Morris, G. A. (2015). Ultrahigh resolution 1H-1H coupling measurement. FGMR 37th Annual Meeting, Abstracts. Presented at the FGMR 37th Annual meeting: Joint discussion meeting of the German and British Magnetic Resonance Societies, Darmstadt, Germany.
Chicago author-date
Sinnaeve, Davy, Mohammadali Foroozandeh, Mathias Nilsson, and Gareth A Morris. 2015. “Ultrahigh Resolution 1H-1H Coupling Measurement.” In FGMR 37th Annual Meeting, Abstracts.
Chicago author-date (all authors)
Sinnaeve, Davy, Mohammadali Foroozandeh, Mathias Nilsson, and Gareth A Morris. 2015. “Ultrahigh Resolution 1H-1H Coupling Measurement.” In FGMR 37th Annual Meeting, Abstracts.
Vancouver
1.
Sinnaeve D, Foroozandeh M, Nilsson M, Morris GA. Ultrahigh resolution 1H-1H coupling measurement. In: FGMR 37th Annual meeting, Abstracts. 2015.
IEEE
[1]
D. Sinnaeve, M. Foroozandeh, M. Nilsson, and G. A. Morris, “Ultrahigh resolution 1H-1H coupling measurement,” in FGMR 37th Annual meeting, Abstracts, Darmstadt, Germany, 2015.
@inproceedings{6980417,
  abstract     = {{Homonuclear scalar couplings are a double-edged sword. They deliver a wealth of structural information, but equally they are detrimental to spectral resolution, impeding their accurate measurement. One way to disentangle individual couplings from complex spectra is the SERF experiment, which delivers a 2D J-resolved spectrum containing only selected couplings [1]. A variant of this experiment, G-SERF, uses the Zangger-Sterk pulse sequence element to deliver simultaneously all the individual couplings to one selected resonance [2]. Other recent variants incorporate band-selective and Zangger-Sterk pure shift acquisition [3,4]. However, all these methods can break down in crowded spectra, either because of signal overlap or because chemical shift differences between coupled spins are too small.
Here, we present the PSYCHEDELIC (Pure Shift Yielded by CHirp Excitation to DELiver Individual Couplings) experiment, derived from the PSYCHE pure shift method [5]. It delivers simultaneously all individual couplings to a selected proton, with minimal constraints on spectral overlap and chemical shift difference, with the usual high sensitivity and spectral purity of PSYCHE.
[1] T. Facke, and S. Berger, J. Magn. Res. Ser. A, (1995), 113(1), 114-116.
[2] N. Giraud, L. Beguin, J. Courtieu, and D. Merlet, Angew. Chem. Int. Ed., (2010), 49(20), 3481-3484.
[3] J. E. H. Pucheta et al., Chem. Commun., (2015), 51(37), 7939-7942.
[4] D. Pitoux, et al., Chem. Eur. J., (2015), 21(25), 9044-9047.
[5] M. Foroozandeh, R. W. Adams, N. J. Meharry, D. Jeannerat, M. Nilsson, and G. A. Morris, Angew. Chem. Int. Ed., (2014), 53(27), 6990-6992.}},
  author       = {{Sinnaeve, Davy and Foroozandeh, Mohammadali and Nilsson, Mathias and Morris, Gareth A}},
  booktitle    = {{FGMR 37th Annual meeting, Abstracts}},
  keywords     = {{NMR spectroscopy}},
  language     = {{eng}},
  location     = {{Darmstadt, Germany}},
  title        = {{Ultrahigh resolution 1H-1H coupling measurement}},
  year         = {{2015}},
}