Crystal Structure Based Design of Signal Enhancement Schemes for Solid-State NMR of Insensitive Half-Integer Quadrupolar Nuclei

O’Dell, Luke A.; Ratcliffe, Christopher I.

doi:10.1021/jp111531e

Cited by 23 publications

(19 citation statements)

References 55 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…The largest principal component of the EFG tensor (V 33 ) and the least shielded component of the CS tensor (δ 11 ) are predicted to be aligned approximately parallel to the N–C bond. These orientations are consistent with previous DFT studies of amino groups. , The correct CS tensor orientation for the 33 S nucleus, which was mislabeled in a previous publication, is also shown in Figure b for completeness. The least shielded component of the 33 S CS tensor (δ 11 ) lies approximately parallel to the S–C bond.…”

Section: Resultssupporting

confidence: 86%

“…An accurate isotropic chemical shift for the nitrogen site (−6.0 ppm) was obtained from the 15 N CPMAS spectrum (Figure a). Along with the quadrupolar coupling constant (C Q ) and asymmetry parameter (η Q ) that were recently determined using ultrawideline 14 N techniques, this provides constraints for the fitting of the 14 N overtone powder pattern obtained at 21.1 T (Figure b). 14 N overtone NMR spectra, in which the nuclei are irradiated at approximately twice the Larmor frequency in order to directly excite and observe the Δ m = 2 “overtone” transition, are insensitive to the first-order quadrupolar interaction, which for 14 N is typically on the order of several MHz .…”

Section: Resultsmentioning

confidence: 92%

“…These orientations are consistent with previous DFT studies of amino groups. 27,28 The correct CS tensor orientation for the 33 S nucleus, which was mislabeled in a previous publication, 11 is also shown in Figure 4b for completeness. The least shielded component of 3.3.…”

Section: Resultsmentioning

confidence: 99%

“…Parameters for the three nonequivalent oxygen sites are also obtained from an isotopically enriched sample and assigned to the correct crystallographic sites with the aid of DFT calculations. Solid-state 1 H and 13 C NMR spectra are also presented, which, in combination with a previous 33 S study, constitutes a near-complete set of NMR results for this model system.…”

Section: Introductionmentioning

confidence: 83%

See 3 more Smart Citations

Multinuclear Solid-State Nuclear Magnetic Resonance and Density Functional Theory Characterization of Interaction Tensors in Taurine

et al. 2012

Self Cite

View full text Add to dashboard Cite

A variety of experimental solid-state nuclear magnetic resonance (NMR) techniques has been used to characterize each of the elements in 2-aminoethane sulfonic acid (taurine). A combination of (15)N cross-polarization magic angle spinning (CPMAS), (14)N ultrawideline, and (14)N overtone experiments enabled a determination of the relative orientation of the nitrogen electric field gradient and chemical shift tensors. (17)O spectra recorded from an isotopically enriched taurine sample at multiple magnetic fields allowed the three nonequivalent oxygen sites to be distinguished, and NMR parameters calculated from a neutron diffraction structure using density functional theory allowed the assignment of the (17)O parameters to the correct crystallographic sites. This is the first time that a complete set of (17)O NMR tensors are reported for a sulfonate group. In combination with (1)H and (13)C MAS spectra, as well as a previously reported (33)S NMR study, this provides a very broad set of NMR data for this relatively simple organic molecule, making it a potentially useful structure on which to test DFT calculation methods (particularly for the quadrupolar nuclei (14)N, (17)O, and (33)S) or NMR crystallography approaches.

show abstract

Section: Resultssupporting

confidence: 86%

Section: Resultsmentioning

confidence: 92%

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 83%

See 2 more Smart Citations

Multinuclear Solid-State Nuclear Magnetic Resonance and Density Functional Theory Characterization of Interaction Tensors in Taurine

et al. 2012

Self Cite

View full text Add to dashboard Cite

show abstract

“…One of the most used techniques for dynamic characterization in the solid state is NMR. − It offers the possibility to study several nuclei ( 13 C, 2 H, 15 N, 1 H, etc.) at different temperatures, and more importantly, along with relaxometry measurements, it can cover a wide range of motional time scales.…”

Section: Impact Of Molecular Motion In Emissive Compoundsmentioning

confidence: 99%

Dual-State Emission (DSE) in Organic Fluorophores: Design and Applications

et al. 2021

View full text Add to dashboard Cite

Organic luminescent materials have attracted significant attention in the past few years due to their fascinating photophysical properties. Implementing these emissive organic compounds is now being actively pursued in many applications in solution (i.e., sensors, bioimaging) or their solid forms (i.e., optoelectronic devices or data encryption). Despite significant advances in the development of emissive compounds, there has been an increasing quest in the past decade for materials where the emission is preserved in both states, dual-state emission (DSE). These compounds are expected to detonate a myriad of applications in the future. On this nascent topic, this work addresses several factors that increase the probability of obtaining the dual-state emission property based on the precedent reports showing this phenomenon. Therefore, this review identifies and organizes the different structural characteristics useful to obtain these compounds. In addition, it has been devised to motivate the discussion in the materials science community and hopefully incentivize the efforts of many research groups around the world toward the synthesis of new dual-state emitters.

show abstract