Complete Dipolar Decoupling of 13C and Its Use in Two-Dimensional Double-Quantum Solid-State NMR for Determining Polymer Conformations

Journal of Magnetic Resonance

Volumn 131, Issue 2, 1998, Pages 209-217

  Schmidt Rohr, K ^a  

^a UNIVERSITY OF MASSACHUSETTS   (United States)

Author keywords

Double quantum NMR; Magic sandwich echo; Multiple pulse decoupling; Polymer conformation; Torsion angles

Indexed keywords

EID: 0000729546     PISSN: 10907807     EISSN: None     Source Type: Journal    
DOI: 10.1006/jmre.1998.1360     Document Type: Article

References (34)

1. E. M. Menger, S. Vega, and R. G. Griffin, Double-quantum observation of carbon-carbon dipolar couplings in solids, J. Magn. Reson. 56, 338-342 (1984).
2. R. Tycko and G. Dabbagh, Double-quantum filtering in MAS NMR spectroscopy: An approach to spectral simplification and molecular structure determination, J. Am. Chem. Soc. 113, 9444-9448 (1991).
3. N. C. Nielsen, H. Bildsoe, H. J. Jacobsen, and M. Levitt, Double-quantum homonuclear rotary resonance: Efficient dipolar recovery in MAS NMR, J. Chem. Phys. 101, 1805-1812 (1994).
4. D. M. Gregory, D. J. Mitchell, J. A. Stringer, S. Kiihne, J. C. Shiels, J. Calahan, M. A. Mehta, and G. P. Drobny, Windowless dipolar recoupling: The detection of weak dipolar couplings between spin 1/2 nuclei with large chemical-shift anisotropies, Chem. Phys. Lett. 246, 654-663 (1995).
5. K. Schmidt-Rohr, A double-quantum solid-state NMR technique for determining torsion angles in polymers, Macromolecules 29, 3975-3981 (1996).
6. 13C-labeled amino acids and peptides by separated-local-field double-quantum NMR, J. Am. Chem. Soc. 118, 7601-7603 (1996).
7. X. Feng, Y. K. Lee, D. Sandström, M. Edén, H. Maisel, A. Sebald, and M. Levitt, Direct determination of a molecular torsional angle by solid-state NMR, Chem. Phys. Lett. 257, 314-320 (1996).
8. T. Nakai and C. A. McDowell, INADEQUATE NMR spectra of extremely strongly coupled spin systems, Mol. Phys. 79, 965-983 (1993).
9. T. Nakai and C. A. McDowell, Characterization of homonuclear spin pairs from 2D spin-echo NMR powder patterns, J. Am. Chem. Soc. 116, 6373-6383 (1994).
10. U. Haeberlen and J. S. Waugh, Coherent averaging effects in magnetic resonance, Phys. Rev. 175, 453-467 (1968); U. Haeberlen, "High Resolution NMR of Solids," Advances in Magnetic Resonance, Supplement 1, Academic Press, San Diego (1976).
11. U. Haeberlen and J. S. Waugh, Coherent averaging effects in magnetic resonance, Phys. Rev. 175, 453-467 (1968); U. Haeberlen, "High Resolution NMR of Solids," Advances in Magnetic Resonance, Supplement 1, Academic Press, San Diego (1976).
12. J. S. Waugh, L. M. Huber, and U. Haeberlen, Approach to high-resolution NMR in solids, Phys. Rev. Lett. 20, 180-182 (1968).
13. W.-K. Rhim, D. D. Elleman, and R. W. Vaughan, Analysis of multiple-pulse NMR in solids, J. Chem. Phys. 59, 3740-3749 (1973).
14. D. P. Burum and W.-K. Rhim, Analysis of multiple pulse NMR in solids. III, J. Chem. Phys. 71, 944-956 (1979).
15. W.-K. Rhim, A. Pines, and J. S. Waugh, Time-reversal experiments in dipolar-coupled spin systems, Phys. Rev. 63, 684-695 (1971).
16. K. Schmidt-Rohr and H. W. Spiess, "Multidimensional Solid-State NMR and Polymers," Academic Press, London/San Diego (1994).
17. S. Matsui, Y. Ogasawara, and T. Inouye, Proton images of elastomers by solid-state NMR imaging, J. Magn. Reson. A 105, 215-218 (1993).
18. W. A. Anderson and R. Freeman, Influence of a second rf field on high-resolution NMR spectra, J. Chem. Phys. 37, 85-103 (1962).
19. A. E. Bennett, C. M. Rienstra, M. Auger, K. V. Lakshmi, and R. G. Griffin, Heteronuclear decoupling in rotating solids, J. Chem. Phys. 103, 6951-6958 (1995).
20. U. Haeberlen, "High Resolution NMR of Solids," Advances in Magnetic Resonance, Supplement 1, p. 86, Academic Press, San Diego (1976).
21. J. D. Ellett and J. S. Waugh, Chemical shift concertina, J. Chem. Phys. 51, 2851-2858 (1969).
22. W. P. Aue, D. J. Ruben, and R. G. Griffin, Uniform chemical shift scaling: Application to 2D resolved NMR spectra. J. Chem. Phys. 80, 1729-1738 (1985).
23. E. L. Hahn, Spin echoes, Phys. Rev. 80, 580-594 (1950).
24. J. G. Powles and J. H. Strange, Zero time resolution nuclear magnetic transients in solids, Proc. Phys. Soc. 82, 60 (1963).
25. 13C NMR spectra via double-quantum coherence, J. Magn. Reson. 43, 478-483 (1981).
26. 13C NMR spectra via double-quantum coherence, J. Magn. Reson. 43, 478-483 (1981).
27. R. R. Ernst, G. Bodenhausen, and A. Wokaun, "Nuclear Magnetic Resonance in One and Two Dimensions," Oxford Univ. Press, Oxford (1987).
28. 13C spin exchange in crystalline polyethylene, J. Am. Chem. Soc. 106, 1515-1517 (1984).
29. 13C spin diffusion in the determination of intermolecular structure in solids, J. Magn. Reson. 58, 458-461 (1984).
30. 2H 2D exchange NMR in solids, Chem. Phys. Lett. 130, 84-89 (1986).
31. G. Dabbagh, D. P. Weliky, and R. Tycko, Determination of monomer conformation in noncrystalline solid polymers by 2D NMR exchange spectectroscopy, Macromolecules 27, 6183-6191 (1994).
32. M. Linder, A. Höhener, and R. R. Ernst, Orientation of tensorial interactions determined from 2D NMR powder spectra, J. Chem. Phys. 73, 4959-4970 (1980).
33. 42, J. Chem. Phys. 64, 830-834 (1976).
34. K. Schmidt-Rohr, M. Wilhelm, A. Johansson, and H. W. Spiess, Determination of chemical-shift tensor orientations in methylene groups by separated-local-field NMR, Magn. Reson. Chem. 31, 352-356 (1993).