؊1 , respectively. The results for the residual dipolar interactions were verified by repeating the above measurements at a temperature of 1.5°C, where the spectra of the H 2 O molecules were well resolved, so that the 1 H-1 H dipolar interaction could be determined directly from the observed splitt
High-Resolution1H Multiple-Quantum Spectra in Solids with Strong Dipolar Interactions
✍ Scribed by Shangwu Ding; Charles A. McDowell
- Publisher
- Elsevier Science
- Year
- 1996
- Tongue
- English
- Weight
- 65 KB
- Volume
- 120
- Category
- Article
- ISSN
- 1064-1858
No coin nor oath required. For personal study only.
✦ Synopsis
Much progress has been made in solid-state multiquantum dimensions is highly resolved so detailed information, espe-(MQ) spectroscopy over the past two decades following cially quantitative data, cannot be obtained. the realization of two-dimensional spectroscopic techniques Several solutions have been proposed, including the use associated with multipulse selective excitation and multiof high-speed MAS while employing DRAMA during prepaquantum separation and filtering schemes (1). Although inration of the MQ coherences (8). This method, which is direct dipolar interaction (J-coupling) mediated MQ spectra one of direct detection, is feasible, as shown by the proposers were reported in favorable cases (2), MQ coherences in (8), and holds potential for further development. It can, solids are mostly created by (direct) dipolar interactions however, usually only create low orders of MQ coherences because the J couplings are usually much weaker than the because DRAMA can only partly recover the dipolar coudipolar couplings, which are anisotropic. For nuclei with plings which had been averaged by MAS. Another method low gyromagnetic ratios such as spin-1 2 nuclei 13 C, 31 P, 29 Si, (9) proposed is indirect and incorporates cross polarization and quadrupole nuclei 2 D, 23 Na, 13 Al, or for nuclei with and MAS (CPMAS). This method can yield high-resolution high gyromagnetic ratios, such as 1 H and 19 F, but with rapid MQ spectra with moderate spinning speed MAS and can molecular motion or when diluted, high resolution can be create high orders of MQ coherences ( 9), but MQ spectra achieved because the dipolar interactions among the nuclei obtained by this method are subject to the peculiarities of the are relatively weak and can be averaged out by magic-angle dynamic processes; e.g., the protons which are not directly spinning at low or moderate spinning speeds. For those spinbonded to any carbon ( 13 C) nuclei will have lower sensitivi-* To whom correspondence should be addressed.
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## Abstract Splittings in the ^13^C cross‐polarization magic angle spinning spectra of 1, 4‐dibromobenzene and 4‐bromo‐3, 5‐dimethylpyrazole are reported. They arise from (^79,81^Br, ^13^C) interactions influenced by the quadrupolar nature of the bromine nuclei. They are analysed using both ‘invers