Solid-State NMR Spectroscopy

Dybowski, Cecil; Bai, Shi

doi:10.1021/ac800573y

Cited by 21 publications

(15 citation statements)

References 145 publications

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“…Solid-state nuclear magnetic resonance (NMR) spectroscopy is an extremely powerful probe of structure and dynamics for both crystalline and partially ordered/amorphous solid materials. [1][2][3][4][5][6][7] Many of the elements of the periodic table possess NMR active nuclei that can potentially be studied by solid-state NMR spectroscopy. The solid-state NMR spectra of heavier spin-1/2 nuclei (e.g., 77 Se, 113 Cd, 109 Ag, 183 W, 195 Pt, 207 Pb, etc.)…”

Section: Introductionmentioning

confidence: 99%

Rapid acquisition of wideline MAS solid-state NMR spectra with fast MAS, proton detection, and dipolar HMQC pulse sequences

Rossini

Hanrahan

Thuo

2016

Phys. Chem. Chem. Phys.

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The solid-state NMR spectra of many NMR active elements are often extremely broad due to the presence of chemical shift anisotropy (CSA) and/or the quadrupolar interaction (for nuclei with spin I > 1/2). These NMR interactions often give rise to wideline solid-state NMR spectra which can span hundreds of kHz or several MHz. Here we demonstrate that by using fast MAS, proton detection and dipolar hetero-nuclear multiple-quantum (D-HMQC) pulse sequences, it is possible to rapidly acquire 2D spectra which correlate H chemical shifts to the indirectly detected wideline MAS powder patterns of dipolar coupled hetero-nuclei. The D-HMQC pulse sequence enables broadband excitation of the wideline hetero-nuclear NMR spectrum and provides higher sensitivity by detecting the narrower and more sensitiveH NMR signal. This approach is demonstrated for the rapid acquisition of 2D H detectedPt solid-state NMR spectra of cisplatin and transplatin and the Ga solid-state NMR spectrum of a self-assembled Ga coordination polymer of unconfirmed structure. This approach should be broadly applicable for the rapid acquisition of wideline MAS solid-state NMR spectra of moderately abundant NMR nuclei.

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Section: Introductionmentioning

confidence: 99%

Rapid acquisition of wideline MAS solid-state NMR spectra with fast MAS, proton detection, and dipolar HMQC pulse sequences

Rossini

Hanrahan

Thuo

2016

Phys. Chem. Chem. Phys.

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“…Solid-state NMR spectroscopy [37] is a powerful technique for the characterization of solid catalysts, especially in their functioning state. [38] We have long been interested in mechanistic investigations of heterogeneously catalyzed reactions by the use of solid-state NMR spectroscopy techniques.…”

Section: Introductionmentioning

confidence: 99%

Reactivity of C₁ Surface Species Formed in Methane Activation on Zn‐Modified H‐ZSM‐5 Zeolite

Wang

et al. 2010

Chemistry A European J

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Solid‐state 13C magic angle spinning (MAS) NMR spectroscopy investigations identified zinc methyl species, formate species, and methoxy species as C1 surface species formed in methane activation on the zeolite Zn/H‐ZSM‐5 catalyst at T≤573 K. These C1 surface species, which are possible intermediates in further transformations of methane, were prepared separately by adsorption of 13C‐enriched methane, carbon monoxide, and methanol onto zinc‐containing catalysts, respectively. Successful isolation of each surface species allowed convenient investigations into their chemical nature on the working catalyst by solid‐state 13C MAS NMR spectroscopy. The reactivity of zinc methyl species with diverse probe molecules (i.e., water, methanol, hydrochloride, oxygen, or carbon dioxide) is correlated with that of organozinc compounds in organometallic chemistry. Moreover, surface formate and surface methoxy species possess distinct reactivity towards water, hydrochloride, ammonia, or hydrogen as probe molecules. To explain these and other observations, we propose that the C1 surface species interconvert on zeolite Zn/H‐ZSM‐5. As implied by the reactivity information, potential applications of methane co‐conversion on zinc‐containing zeolites might, therefore, be possible by further transformation of these C1 surface species with rationally designed co‐reactants (i.e., probe molecules) under optimized reaction conditions.

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“…Solid-state nuclear magnetic resonance (SSNMR) spectroscopy is a versatile tool for the structural characterization of inorganic and organic materials and biomolecules. [1][2][3][4] Sensitivity and resolution enhancement techniques such as fast magic angle spinning (MAS), [5][6][7] proton detection [8][9][10][11][12][13] and dynamic nuclear polarization (DNP) [14][15][16] have enabled the routine implementation of advanced multidimensional SSNMR experiments. Probing heteronuclear proximities using multidimensional heteronuclear correlation (HETCOR) experiments or dipolar coupling (D) measurements between nuclei is arguably one of the key strengths of SSNMR.…”

Section: Introductionmentioning

confidence: 99%

“…47 However, the g-encoded sequences are sensitive to rf inhomogeneity and suffer from dipolar truncation. As such, they typically offer lower efficiency than SR4 2 1 and adiabatic zero-quantum recoupling methods. 48,49 Alternatively, in the TRAPDOR-HMQC (T-HMQC) experiment presented by Carravetta and co-workers, 50 long duration, high power pulses are used for both heteronuclear dipolar recoupling and excitation of the indirectly detected nucleus.…”

Section: Introductionmentioning

confidence: 99%

t₁-Noise eliminated dipolar heteronuclear multiple-quantum coherence solid-state NMR spectroscopy

Venkatesh

Luan

Perras

et al. 2020

Phys. Chem. Chem. Phys.

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Solid-State NMR Spectroscopy

Cited by 21 publications

References 145 publications

Rapid acquisition of wideline MAS solid-state NMR spectra with fast MAS, proton detection, and dipolar HMQC pulse sequences

Rapid acquisition of wideline MAS solid-state NMR spectra with fast MAS, proton detection, and dipolar HMQC pulse sequences

Reactivity of C₁ Surface Species Formed in Methane Activation on Zn‐Modified H‐ZSM‐5 Zeolite

t₁-Noise eliminated dipolar heteronuclear multiple-quantum coherence solid-state NMR spectroscopy

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Solid-State NMR Spectroscopy

Cited by 21 publications

References 145 publications

Rapid acquisition of wideline MAS solid-state NMR spectra with fast MAS, proton detection, and dipolar HMQC pulse sequences

Rapid acquisition of wideline MAS solid-state NMR spectra with fast MAS, proton detection, and dipolar HMQC pulse sequences

Reactivity of C1 Surface Species Formed in Methane Activation on Zn‐Modified H‐ZSM‐5 Zeolite

t1-Noise eliminated dipolar heteronuclear multiple-quantum coherence solid-state NMR spectroscopy

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Reactivity of C₁ Surface Species Formed in Methane Activation on Zn‐Modified H‐ZSM‐5 Zeolite

t₁-Noise eliminated dipolar heteronuclear multiple-quantum coherence solid-state NMR spectroscopy