A 1D H, C correlation with homonuclear cross‐polarization

Zangger, Klaus; Sterk, H.

doi:10.1002/mrc.1260330714

Cited by 64 publications

(131 citation statements)

References 21 publications

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“…Homodecoupling, as a means of suppressing scalar interactions for enhanced spectral resolution, has been recognized for several years . Subsequent seminal developments of broadband homodecoupling techniques to achieve complete collapse of multiplets to pure‐shift singlets include: Zangger–Sterk (ZS) decoupling scheme and its refined variants for multidimensional NMR that rely on spatially encoded excitation in the presence of slice‐selective z‐gradient pulse.…”

Section: Introductionmentioning

confidence: 99%

Real‐time homonuclear broadband and band‐selective decoupled pure‐shift ROESY

Kakita

Jagadeesh

2014

Magnetic Reson in Chemistry

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Unambiguous spectral assignments in (1)H solution-state NMR are central, for accurate structural elucidation of complex molecules, which is often hampered by signal overlap, primarily because of scalar coupling multiplets, even at typical high magnetic fields. The recent advances in homodecoupling methods have shown powerful means of achieving high resolution pure-shift (1)H spectra in 1D and also in 2D J-correlated experiments, by effectively collapsing the multiplet structures. The present work extends these decoupling strategies to through-space correlation experiments as well and describes two new pure-shift ROESY pulse schemes with homodecoupling during acquisition, viz., homodecoupled broadband (HOBB)-ROESY and homodecoupled band-selective (HOBS)-ROESY. Furthermore, the ROESY blocks suppress the undesired interferences of TOCSY cross peaks and other offsets. Despite the reduced signal sensitivity and prolonged experimental times, the HOBB-ROESY is particularly useful for molecules that exhibit an extensive scalar coupling network spread over the entire (1)H chemical shift range, such as natural/synthetic organic molecules. On the other hand, the HOBS-ROESY is useful for molecules that exhibit well-separated chemical shift regions such as peptides (NH, Hα and side-chain protons). The HOBS-ROESY sensitivities are comparable with the conventional ROESY, thereby saves the experimental time significantly. The power of these pure-shift ROESY sequences is demonstrated for two different organic molecules, wherein complex conventional ROE cross peaks are greatly simplified with high resolution and sensitivity. The enhanced resolution allows deriving possibly more numbers of ROEs with better accuracy, thereby facilitating superior means of structural characterization of medium-size molecules.

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Section: Introductionmentioning

confidence: 99%

Real‐time homonuclear broadband and band‐selective decoupled pure‐shift ROESY

Kakita

Jagadeesh

2014

Magnetic Reson in Chemistry

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“…19 Recently, a novel idea based on the use of selective pulses and weak gradients to achieve homonuclear broadband decoupling was described. 20 Here we propose a new alternative to obtain decoupled spectra in the weak scalar coupling approximation, termed analytical decoupling. Using a data processing method similar to that proposed for measuring longrange scalar coupling constants,21 the method requires conventional spin echo experiments : a set of echoes is recorded for di †erent values of the echo time, and a T E , treatment is performed employing a two-stage procedure, giving a new signal in the time domain.…”

Section: Introductionmentioning

confidence: 99%

Broadband analytical decoupling in high-resolution NMR spectra

1998

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“…Cross-peak integrals were measured after seven days of equilibration to ensure uniform deuteration of the sample. H-T-OH has been described as completely disordered in water [11]. Results and Discussion Figure 1 shows a ] H-NMR spectrum of Ac-T-NH2 in DMSO-d6 at 298 K. No signs of aggregation are visible in this spectrum and it does not change when the concentration of the sample is reduced by ca.…”

Section: Nmr Experimentsmentioning

confidence: 99%

An easy NMR method to study the formation of parallel β-sheets in peptide aggregates

1999

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There is currently great interest in the study of peptide aggregation by t-sheet formation because of its relevance in pathological states or in the design of self-assembling systems of technological interest. NMR studies of t-sheet aggregates are difficult because of their long correlation times and spectral degeneracy. In this communication we demonstrate the combination of a semiselective TOCSY-NOESY experiment with partial deuterium exchange of labile protons to assign inter-molecular NOE cross peaks and prove the presence of a soluble parallel t-sheet in fast exchange with monomeric Ac-ASTTTNYT-NH2 (Ac-T-NH2) in solution.

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A 1D H, C correlation with homonuclear cross‐polarization

Abstract: A 1D H,C correlation ROESY experiment is suggested and applications for signal assignments via thoughbond and tbrougb-space correlations are demonstrated using glutathione and l -o -m e t b y l -4 , a y~d~-~~ copyranoside.

Cited by 64 publications

References 21 publications

Real‐time homonuclear broadband and band‐selective decoupled pure‐shift ROESY

Real‐time homonuclear broadband and band‐selective decoupled pure‐shift ROESY

Broadband analytical decoupling in high-resolution NMR spectra

An easy NMR method to study the formation of parallel β-sheets in peptide aggregates

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