Publication: A natural abundance 33S solid-state NMR study of layered transition metal disulfides at ultrahigh magnetic field
All || By Area || By Year| Title | A natural abundance 33S solid-state NMR study of layered transition metal disulfides at ultrahigh magnetic field | Authors/Editors* | A. Sutrisno, V. V. Terskikh, Y.Huang |
|---|---|
| Where published* | Chemical Communications |
| How published* | Journal |
| Year* | 2009 |
| Volume | |
| Number | |
| Pages | 186-188 |
| Publisher | RSC |
| Keywords | S-33 solid-state NMR, transition metal disulfides, low gamma quadrupolar nuclei |
| Link | |
| Abstract |
Many sulfur-containing materials are of industrial, technological and biological importance. Characterization of S environments by 33S solid-state NMR (SSNMR) has been difficult due to the unfavorable NMR characteristics of sulfur-33. In this work, we show that the high quality static 33S natural abundance SSNMR spectra of S in a less symmetric environment can be readily obtained at ultrahigh magnetic field of 21.1 T. Both 33S chemical shielding (CS) and electric field gradient (EFG) tensors can be directly extracted via spectral analysis. In particular, 33S SSNMR spectra of several practically important layered transition metal disulfides including MoS2, WS2, ZrS2, TiS2 and TaS2 were obtained for the first time and they were found to be highly sensitive to their local geometry and electronic properties. These closely related metal disulfides display a surprisingly wide range of quadrupole coupling constant, CQ, from 0.5 to ca. 10 MHz and chemical shift anisotropy (CSA) ranging from zero to 250 ppm. 33S quadrupolar parameters were calculated by plane wave-pseudopotential density functional theory (DFT) and the results are in good agreement with the values obtained experimentally. An important empirical relationship between the CQ and the M-S-M bond angle was established and such trend was verified by theoretical calculations. |
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