Abstract:Recording NMR signals of several nuclear species simultaneously by using parallel receivers provides more information from a single measurement and at the same time increases the measurement sensitivity per unit time. Here we present a comprehensive series of the most frequently used NMR experiments modified for simultaneous direct detection of two of the most sensitive NMR nuclei - (1) H and (19) F. We hope that the presented material will stimulate interest in and further development of this technique.
“…The unique chemical shift of the fluorinated 13 C resonances at ~150 ppm, separated from the aromatic 13 C H resonances (at ~120 ppm), will further aid the assignment of 19 F resonances. With the appropriate NMR probe design, experiments that encode both 1 H- 13 C and 19 F- 13 C correlations can be recorded using parallel receivers 40 .…”
Obtaining atomic level information about the structure and dynamics of biomolecules is critical to understand their function. Nuclear magnetic resonance (NMR) spectroscopy provides unique insights into the dynamic nature of biomolecules and their interactions, capturing transient conformers and their features. However, relaxation-induced line broadening and signal overlap make it challenging to apply NMR to large biological systems. Here, we take advantage of the high sensitivity and the broad chemical-shift range of
19
F nuclei, and leverage the remarkable relaxation properties of the aromatic
19
F-
13
C spin pair to disperse
19
F resonances in a 2-dimensional transverse relaxation optimized TROSY spectrum. We demonstrate the application of the
19
F-
13
C TROSY to investigate proteins and nucleic acids. This experiment expands the scope of
19
F NMR in the study of structure, dynamics and function of large and complex biological systems and provides a powerful background-free NMR probe.
“…The unique chemical shift of the fluorinated 13 C resonances at ~150 ppm, separated from the aromatic 13 C H resonances (at ~120 ppm), will further aid the assignment of 19 F resonances. With the appropriate NMR probe design, experiments that encode both 1 H- 13 C and 19 F- 13 C correlations can be recorded using parallel receivers 40 .…”
Obtaining atomic level information about the structure and dynamics of biomolecules is critical to understand their function. Nuclear magnetic resonance (NMR) spectroscopy provides unique insights into the dynamic nature of biomolecules and their interactions, capturing transient conformers and their features. However, relaxation-induced line broadening and signal overlap make it challenging to apply NMR to large biological systems. Here, we take advantage of the high sensitivity and the broad chemical-shift range of
19
F nuclei, and leverage the remarkable relaxation properties of the aromatic
19
F-
13
C spin pair to disperse
19
F resonances in a 2-dimensional transverse relaxation optimized TROSY spectrum. We demonstrate the application of the
19
F-
13
C TROSY to investigate proteins and nucleic acids. This experiment expands the scope of
19
F NMR in the study of structure, dynamics and function of large and complex biological systems and provides a powerful background-free NMR probe.
“…A system patterned with 19 F nuclei is in contrast particularly advantageous since 19 F NMR is readily performed. [78][79][80] It is in these directions that we are now working.…”
This report details how the design of specific nuclear-spin patterns on ligands modulates spin-relaxation times in a set of open-shell vanadium(iv) complexes.
“…The NOAH approach represents one category of techniques that employ multi‐FID acquisitions in a single concatenated experiment that are gaining recognition as time‐efficient data collection strategies . These are attractive as they can be executed using conventional spectrometer hardware without the need for multiple receivers, as used in parallel acquisition NMR spectroscopy, nor do they suffer the technical complexities associated with single‐scan ultrafast correlation methods …”
Section: Introductionmentioning
confidence: 99%
“…The NOAH approach represents one category of techniques that employ multi-FID acquisitions in a single concatenated experiment that are gaining recognition as time-efficient data collection strategies. [3][4][5][6] These are attractive as they can be executed using conventional spectrometer hardware without the need for multiple receivers, as used in parallel acquisition NMR spectroscopy, [7][8][9] nor do they suffer the technical complexities associated with single-scan ultrafast correlation methods. [10][11][12] Recently, we have demonstrated the NOAH BS-element as being the optimum ordering to sample HMBC (B) and HSQC (S) correlation data in a single experiment and exemplified its use in the BSC and BSCN combinations (where C signifies COSY and N NOESY).…”
A series of NMR supersequences are presented for the time‐efficient structure characterisation of small molecules in the solution state. These triplet sequences provide HMBC, HSQC, and one homonuclear correlation experiment of choice according to the NMR by Ordered Acquisition using 1H detection principle. The experiments are demonstrated to be compatible with non‐uniform sampling schemes and may be acquired and processed under full automation.
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