Frequency-swept pulse sequences for 19F heteronuclear spin decoupling in solid-state NMR

Chandran, C. Vinod; Madhu, P.K.; Wormald, Philip; Bräuniger, Thomas

doi:10.1016/j.jmr.2010.07.018

Cited by 18 publications

(14 citation statements)

References 81 publications

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“…[16]). The following parameters were used [12,17,18]: d aniso F was varied between 0 and 120 kHz simultaneously for both fluorines (corresponding to 0-180 ppm at…”

Section: Experimentalsmentioning

confidence: 99%

“…Most efforts in this development have addressed 1 H dipolar decoupling to cover a broad array of applications for solid-state NMR in chemistry and molecular biology. In most cases this development also lead to reasonably well-functioning decoupling sequences for 19 F decoupling applications although only few studies addressed this aspect in greater detail [12].…”

Section: Introductionmentioning

confidence: 99%

“…Addressing decoupling of dipolar couplings to 19 F spins one may encounter challenges associated with significantly larger isotropic chemical shift dispersion (shift range in the order of 300 ppm [12][13][14][15][16][17][18], being much larger than the 10-15 ppm seen for 1 H) and chemical shift anisotropies (anisotropies up to 150 ppm and in extreme cases even 300 ppm [12,[14][15][16][17][18], significantly exceeding the typical 3-10 ppm for 1 H [16]) putting different demands to the decoupling methods relative to 1 H decoupling. Chandran and coworkers [12] recently addressed these issues and presented a direct comparison of various state-of-the-art decoupling sequences in relation to 19 F decoupling in rigid organic compounds.…”

Section: Introductionmentioning

confidence: 99%

“…Chandran and coworkers [12] recently addressed these issues and presented a direct comparison of various state-of-the-art decoupling sequences in relation to 19 F decoupling in rigid organic compounds. This study revealed that standard CW decoupling is clearly insufficient in most cases, but also that commonly used high-performance methods such as TPPM [1] are far from optimally performing for such applications while SPINAL [2] and swept versions of TPPM and SPINAL, referred to as SW f -TPPM [8] and SW f -SPINAL [9], perform noticeably better.…”

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

Robust and efficient 19F heteronuclear dipolar decoupling using refocused continuous-wave rf irradiation

Vinther¹,

Khaneja²,

Nielsen³

2013

Journal of Magnetic Resonance

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“…[16]). The following parameters were used [12,17,18]: d aniso F was varied between 0 and 120 kHz simultaneously for both fluorines (corresponding to 0-180 ppm at…”

Section: Experimentalsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Robust and efficient 19F heteronuclear dipolar decoupling using refocused continuous-wave rf irradiation

Vinther¹,

Khaneja²,

Nielsen³

2013

Journal of Magnetic Resonance

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“…These parameters were optimised on a fluorinated model compound. More details on the application of SW f -TPPM for 19 F decoupling will be published elsewhere [24]. …”

Section: Introductionmentioning

confidence: 99%

Covalent Bonds in α‐SnF₂ Monitored by J‐Couplings in Solid‐State NMR Spectra

Bräuniger

Ghedia

Jansen

2010

Zeitschrift anorg allge chemie

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The stable ambient‐temperature phase of tin(II) fluoride, α‐SnF2, was studied by 19F and 119Sn magic‐angle spinning (MAS) NMR spectroscopy. A large chemical shift anisotropy (CSA) is observed in the spectra of both nuclides, which is indicative of the presence of stereochemically active lone electron pair on tin. Symmetric satellite lines with low intensity have been detected in the 119Sn MAS spectra acquired under 19F decoupling, and are assigned to indirect J‐couplings between the magnetically active tin isotopes. The detection of J‐couplings is evidence for the existence of genuine covalent bonds in α‐SnF2, a fact which was deduced before from X‐ray crystallography, which revealed the presence of Sn–F distances smaller than the sum of the respective ionic radii.

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Solid‐State NMR Spectroscopy: Introduction for Solid‐State Chemists

Zehe

Siegel

Senker

2017

Handbook of Solid State Chemistry

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Solid‐state nuclear magnetic resonance spectroscopy ( ssNMR ) is a powerful and flexible tool for deriving structural and dynamical information for a broad variety of material classes ranging from metals, intermetallics, and ceramics over organic, inorganic, and metal–organic frameworks to molecular crystals and polymers. The combination of relaxation experiments, lineshape analyses, and 2 D exchange techniques spans a dynamical window of about 14 decades with correlation times ranging from 10 −12 s for fast ion conduction and up to 100 s for the relaxation close to the glass transition. ssNMR is element selective and thus able to identify chemical building units and simultaneously probes their homo‐ and heteronuclear through‐bond and through‐space connectivities, orientation correlations, as well as distances up to a few nanometers. Thus, ssNMR is ideally suited and often used to complement diffraction studies and quantum chemical calculations. It does not suffer from a loss of long‐range order and may equally be applied to crystalline, disordered, and amorphous materials to make progress on the structure elucidation of complex compounds. This chapter provides an overview of fundamental aspects of ssNMR , including the most important nuclear spin interactions and their typical spectral lineshapes for both wideline and high‐resolution experiments. Based on this, we describe the development and application of various 1 D and 2 D NMR techniques, for both structural and dynamical aspects, on selected examples taken from the recent literature. In particular, we focus on strengths, weaknesses, and the expressiveness of the individual methods.

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Frequency-swept pulse sequences for 19F heteronuclear spin decoupling in solid-state NMR

Cited by 18 publications

References 81 publications

Robust and efficient 19F heteronuclear dipolar decoupling using refocused continuous-wave rf irradiation

Robust and efficient 19F heteronuclear dipolar decoupling using refocused continuous-wave rf irradiation

Covalent Bonds in α‐SnF₂ Monitored by J‐Couplings in Solid‐State NMR Spectra

Solid‐State NMR Spectroscopy: Introduction for Solid‐State Chemists

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Frequency-swept pulse sequences for 19F heteronuclear spin decoupling in solid-state NMR

Cited by 18 publications

References 81 publications

Robust and efficient 19F heteronuclear dipolar decoupling using refocused continuous-wave rf irradiation

Robust and efficient 19F heteronuclear dipolar decoupling using refocused continuous-wave rf irradiation

Covalent Bonds in α‐SnF2 Monitored by J‐Couplings in Solid‐State NMR Spectra

Solid‐State NMR Spectroscopy: Introduction for Solid‐State Chemists

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Product

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Covalent Bonds in α‐SnF₂ Monitored by J‐Couplings in Solid‐State NMR Spectra