Application of Solid-State <sup>209</sup>Bi NMR to the Structural Characterization of Bismuth-Containing Materials
Hamaed, H; Laschuk, MW; Terskikh, VV; Schurko, RW
| HERO ID | 607364 |
|---|---|
| In Press | No |
| Year | 2009 |
| Title | Application of Solid-State <sup>209</sup>Bi NMR to the Structural Characterization of Bismuth-Containing Materials |
| Authors | Hamaed, H; Laschuk, MW; Terskikh, VV; Schurko, RW |
| Journal | Journal of the American Chemical Society |
| Volume | 131 |
| Issue | 23 |
| Page Numbers | 8271-8279 |
| Abstract | Herein, we report the first detailed study of <sup>209</sup>Bi solid-state NMR (SSNMR) spectroscopy of extremely broad central transition powder patterns. <sup>209</sup>Bi ultrawideline SSNMR spectra of several bismuth-containing materials (bismuth oxyhalides, bismuth nitrate pentahydrate, nonaaquabismuth triflate, and bismuth acetate) were acquired at field strengths of 9.4 and 21.11 using frequency-stepped techniques. The <sup>209</sup>Bi SSNMR experiments at 9.4 T yield powder patterns with breadths ranging from 0.9 to 14.6 MHz, from which quadrupolar coupling constants, CQ<sup>209</sup>Bi), between 78 and 256 MHz, were extracted via analytical simulations. The breadths of the quadrupolar-dominated spectra and overall experimental times are greatly reduced for experiments conducted at 21.1 T, which yield high signal-to-noise spectra in which the smaller effects of bismuth chemical shift anisotropy can be clearly observed. The <sup>209</sup>Bi electric field gradient (EFG) and chemical shift (CS) tensor parameters extracted from these spectra are correlated to the molecular structures at the bismuth sites, via first principles calculations of <sup>209</sup>Bi EFG and CS tensors performed using CASTEP for periodic solids and Gaussian 03 for molecular clusters. The rapidity with which <sup>209</sup>Bi SSNMR spectra can be acquired at ultrahigh fields, the sensitivity of the <sup>209</sup>Bi NMR parameters to the bismuth environment, and the predictive power of theoretically calculated NMR interaction tensors suggest that <sup>209</sup>Bi SSNMR may be useful for the characterization of a variety of Bi-containing materials and compounds. [ABSTRACT FROM AUTHOR] Copyright of Journal of the American Chemical Society is the property of American Chemical Society and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.) |
| Doi | 10.1021/ja901347k |
| Pmid | 19462954 |
| Wosid | WOS:000267623100048 |
| Is Certified Translation | No |
| Dupe Override | No |
| Is Public | Yes |
| Language Text | English |
| Keyword | BISMUTH; ELECTRIC fields; ANISOTROPY; MOLECULAR structure; MATTER -- Properties; SPECTRUM analysis; NUCLEAR magnetic resonance |
| Is Qa | No |