Relaxation-Induced Dipolar Exchange with Recoupling - An MAS NMR Method for Determining Heteronuclear Distances without Irradiating the Second Spin

Journal of Magnetic Resonance

Volumn 145, Issue 2, 2000, Pages 161-172

  Saalwächter, Kay ^a,b   Schmidt Rohr, Klaus ^a,c  

^a UNIVERSITY OF MASSACHUSETTS   (United States)

^b MAX PLANCK INSTITUTE FOR POLYMER RESEARCH   (Germany)

^c IOWA STATE UNIVERSITY   (United States)

Author keywords

CODEX; DEAR; Dipolar couplings; Distance measurements; Recoupling; REDOR; Relaxation

Indexed keywords

EID: 0038158098     PISSN: 10907807     EISSN: None     Source Type: Journal    
DOI: 10.1006/jmre.2000.2085     Document Type: Article

References (27)

1. T. Gullion and J. Schaefer, Detection of weak heteronuclear dipolar coupling by rotational-echo double-resonance nuclear magnetic resonance, Adv. Magn. Reson. 13, 57-83 (1989).
2. M. Hong, J. D. Gross, and R. G. Griffin, Site-resolved determination of peptide torsion angle φ from the relative orientations of backbone N-H and C-H bonds by solid-state NMR, J. Phys. Chem. B 101, 5869-5874 (1997).
3. 13C labeling and two-dimensional solid-state NMR, J. Magn. Reson. 139, 389-401 (1999).
4. K. Saalwächter, R. Graf, and H. W. Spiess, Recoupled polarization transfer heteronuclear multiple-quantum correlation in solids under ultra-fast MAS, J. Magn. Reson. 140, 471-476 (1999).
5. A. Fechtenkötter, K. Saalwächter, M. A. Harbison, K. Müllen, and H. W. Spiess, Highly ordered columnar structures from hexa-perihexabenzocoronenes - Synthesis, X-ray diffraction, and solid-state heteronuclear multiple-quantum NMR investigations, Angew. Chem. Int. Ed. 38, 3039-3042 (1999).
6. 13C solid-state NMR, Chem. Phys. Lett. 300, 213-220 (1999).
7. I. Sack, A. Goldbourt, S. Vega, and G. Buntkowsky, Deuterium REDOR: Principles and applications for distance measurements, J. Magn. Reson. 138, 54-65 (1999).
8. T. Guillion, Measurement of dipolar interactions between spin-1/2and quadrupolar nuclei by rotational-echo, adiabatic-passage, double-resonance NMR, Chem. Phys. Lett. 246, 325-330 (1995).
9. J. R. Sachleben, V. Frydman, and L. Frydman, Dipolar determinations in solids by relaxation-assisted NMR recoupling, J. Am. Chem. Soc. 118, 9786-9787 (1996).
10. E. R. deAzevedo, W.-G. Hu, T. J. Bonagamba, and K. Schmidt-Rohr, Centerband-only detection of exchange: Efficient analysis of dynamics in solids by NMR, J. Am. Chem. Soc. 121, 8411-8412 (1999).
11. E. R. deAzevedo, W.-G. Hu, T. J. Bonagamba, and K. Schmidt-Rohr, Principles of centerband-only detection of exchange in solid-state NMR, and extensions to 4-time CODEX, J. Chem. Phys. 112, 8988-9001 (2000).
12. H. W. Spiess, Rotation of molecules and nuclear spin relaxation, in "NMR Basic Principles and Progress," pp. 55-214, Springer-Verlag, Berlin (1978).
13. J. M. Goetz and J. Schaefer, REDOR dephasing by multiple spins in the presence of molecular motion, J. Magn. Reson. 127, 147-154 (1997).
14. O. W. Sørensen, G. W. Eich, M. H. Levitt, G. Bodenhausen, and R. R. Ernst, Product operator formalism for the description of NMR pulse experiments, Progr. NMR Spectrosc. 16, 163-192 (1983).
15. D. A. Torchia and A. Szabo, Spin-lattice relaxation in solids, J. Magn. Reson. 49, 107-121 (1982).
16. A. Abragam, "The Principles of Nuclear Magnetism," Oxford Univ. Press, Oxford (1961).
17. R. R. Ernst, G. Bodenhausen, and A. Wokaun, "Principles of Nuclear Magnetic Resonance in One and Two Dimensions," Oxford Univ. Press, New York (1987).
18. C. Schmidt, K. J. Kuhn, and H. W. Spiess, Distribution of correlation times in glassy polymers from pulsed deuteron NMR. Progr. Colloid Polym. Sci. 71, 71-76 (1985).
19. K. Schmidt-Rohr and H. W. Spiess, "Multidimensional Solid-State NMR and Polymers," Academic Press, San Diego (1994).
20. T. Terao, H. Miura, and A. Saika, Dipolar SASS NMR spectroscopy: Separation of heteronuclear dipolar powder patterns in rotating solids, J. Chem. Phys. 85, 3816-3826 (1986).
21. 14N relaxation processes. J. Chem. Phys. 81, 1583-1591 (1984).
22. 1 different from ∞.
23. M. S. Lehmann, T. F. Koetzle, and W. C. Hamilton, Precision neutron diffraction structure determination of protein and nucleic acid compounds. I. The crystal and molecular structure of the amino acid L-alanine, J. Am. Chem. Soc. 94, 2657-2660 (1972).
24. R. Destro, R. E. Marsh, and R. Bianchi, A low-temperature (23K) study of L-alanine, J. Phys. Chem. 92, 966-973 (1988).
25. E. R. Henry and A. Szabo, Influence of vibrational motion on solid state line shapes and NMR relaxation, J. Chem. Phys. 82, 4753-4760 (1985).
26. J. L. Derissen, Crystal structure and conformation of methylmalonic acid, Acta Crystallogr. Sect. B 26, 901 (1970).
27. T. Gullion, D. B. Baker, and M. S. Conradi, New, compensated Carr-Purcell sequences, J. Magn. Reson. 89, 479-484, 1990.