Heteronuclear polarization transfer by symmetry-based recoupling sequences in solid-state NMR

Zhao, Xin; Hoffbauer, Wilfried; Günne, Jörn Schmedt auf der; Levitt, Malcolm H.

doi:10.1016/j.ssnmr.2003.11.001

Cited by 110 publications

(159 citation statements)

References 26 publications

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“…The R18 7 1 recoupling sequence used a 1 H nutation frequency of 45 kHz for the R-elements, which consisted of simple p-pulses as described in the original PRESTO publication. 53 The 2D 43 Coherence transfer pathway selection was achieved with a 4-step phase cycle. The advantage of PRESTO over cross-polarization based HETCOR experiments is that the pulses on the 27 Al channel only require information about a selective central-transition pulse, while the Hartmann-Hahn condition of the CP experiment is more difficult to set up.…”

Section: Solid-state Nmrmentioning

confidence: 99%

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Structural investigation of aluminium doped ZnO nanoparticles by solid-state NMR spectroscopy

Avadhut

Weber

Hammarberg

et al. 2012

Phys. Chem. Chem. Phys.

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The electrical conductivity of aluminium doped zinc oxide (AZO, ZnO:Al) materials depends on doping induced defects and grain structure. This study aims at relating macroscopic electrical conductivity of AZO nanoparticles with their atomic structure, which is non-trivial because the derived materials are heavily disordered and heterogeneous in nature. For this purpose we synthesized AZO nanoparticles with different doping levels and narrow size distribution by a microwave assisted polyol method followed by drying and a reductive treatment with forming gas. From these particles electrically conductive, optically transparent films were obtained by spin-coating. Characterization involved energy-dispersive X-ray analysis, wet chemical analysis, X-ray diffraction, electron microscopy and dynamic light scattering, which provided a basis for a detailed structural solid-state NMR study. A multinuclear ( 27 Al, 13 C, 1 H) spectroscopic investigation required a number of 1D MAS NMR and 2D MAS NMR techniques (T 1 -measurements, 27 Al-MQMAS, 27 Al-1 H 2D-PRESTO-III heteronuclear correlation spectroscopy), which were corroborated by quantum chemical calculations with an embedded cluster method (EEIM) at the DFT level. From the combined data we conclude that only a small part of the provided Al is incorporated into the ZnO structure by substitution of Zn. The related 27 Al NMR signal undergoes a Knight shift when the material is subjected to a reductive treatment with forming gas. At higher (formal) doping levels Al forms insulating (Al, H and C containing) side-phases, which cover the surface of the ZnO:Al particles and increase the sheet resistivity of spin-coated material. Moreover, calculated 27 Al quadrupole coupling constants serve as a spectroscopic fingerprint by which previously suggested point-defects can be identified and in their great majority be ruled out.

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Section: Solid-state Nmrmentioning

confidence: 99%

“…48 Finally, the calculation of EFG and NMR , which is an R-symmetry pulse sequence where the R-element is a simple p-pulse, the recoupling sequence is used as described in detail in ref. 53.…”

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confidence: 99%

Structural investigation of aluminium doped ZnO nanoparticles by solid-state NMR spectroscopy

Avadhut

Weber

Hammarberg

et al. 2012

Phys. Chem. Chem. Phys.

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“…A wide range of recoupling methodology under MAS has been proposed in the last two decades to selectively restore the information of the heteronuclear dipolar couplings. 13,15,18,[24][25][26][27][28] In this study we use an R-type proton detected local field method (R-PDLF).…”

Section: Introductionmentioning

confidence: 99%

Segmental order parameters in a nonionic surfactant lamellar phase studied with 1H–13C solid-state NMR

Ferreira

Medronho

Martin

et al. 2008

Phys. Chem. Chem. Phys.

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A lyotropic nonionic lamellar system composed of pentaethyleneglycol mono n-dodecyl ether and D 2 O was studied using natural abundance 13 C NMR under magic-angle spinning. Applying a two-dimensional recoupling method proposed by Dvinskikh (R-PDLF), 1 H- 13C dipolar couplings were estimated over a range of temperatures (300-335 K), thus enabling analysis of structural changes in the liquid crystalline system. The results obtained are used to correlate the conformation and mobility of local sites in the surfactant molecule with overall changes in the lamellar structure.

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“…This sequence requires an order of magnitude less power than the PISEMA-MAS sequence, while the spectral resolution and line shape are similar in both the cases. This sequence would be highly valuable for systems where spin-locking of the transverse magnetization for heteronuclear coherence transfer is difficult [7,27]. The experimental results suggest that the performance of the sequence is independent of the spinning speed and rf power whereas it depends on the offset frequency of protons.…”

Section: Discussionmentioning

confidence: 97%

“…Several techniques have been used to recover the heteronucelar dipolar interaction between abundant (typically 1 H) and rare (typically 13 C or 15 N) spins that are usually averaged out by the magic angle spinning (MAS) [1][2][3][4][5][6][7]. Polarization inversion spin exchange at the magic angle (PISEMA) [1,[8][9][10] is one of the most frequently used methods to measure the dipolar coupling between a 1 H nucleus and a low γ nucleus such as 13 C or 15 N. Excellent features of the PISEMA pulse sequence have also led to applications under MAS [1,9,11,12].…”

Section: Introductionmentioning

confidence: 99%

PITANSEMA-MAS, a solid-state NMR method to measure heteronuclear dipolar couplings under MAS

Yamamoto

Ermakov

Lee

et al. 2005

Chemical Physics Letters

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A 2D NMR method is presented for the measurement of the dipole-dipole interaction between a proton and a low-frequency nuclear spin species in the solid state under the magic angle spinning. It employs the time averaged nutation concept to dramatically reduce the required radio frequency (rf) power on the low γ nuclear channel and spin exchange at the magic angle is used to suppress 1 H-1 H dipolar interactions and chemical shifts. The flexibility in choosing the spinning speed, rf power and the scaling factor of the pulse sequence are of considerable importance for the structural studies of biological solids. The performance of the pulse sequence has been numerically and experimentally demonstrated on several solids.

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Heteronuclear polarization transfer by symmetry-based recoupling sequences in solid-state NMR

Cited by 110 publications

References 26 publications

Structural investigation of aluminium doped ZnO nanoparticles by solid-state NMR spectroscopy

Structural investigation of aluminium doped ZnO nanoparticles by solid-state NMR spectroscopy

Segmental order parameters in a nonionic surfactant lamellar phase studied with 1H–13C solid-state NMR

PITANSEMA-MAS, a solid-state NMR method to measure heteronuclear dipolar couplings under MAS

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