Sideband Patterns from Rotor-Encoded Longitudinal Magnetization in MAS Recoupling Experiments

Journal of Magnetic Resonance

Volumn 146, Issue 1, 2000, Pages 140-156

  De Paul, Susan M ^a   Saalwächter, Kay ^a   Graf, Robert ^a   Spiess, Hans W ^a  

^a MAX PLANCK INSTITUTE FOR POLYMER RESEARCH   (Germany)

Author keywords

Heteronuclear dipolar coupling; Longitudinal magnetization; Magic angle spinning; Recoupling; Rotational echo double resonance (REDOR); Spinning sideband patterns

Indexed keywords

ALANINE; TRICHLOROACETIC ACID; TYROSINE;

ANISOTROPY; ARTICLE; CHEMISTRY; METHODOLOGY; NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY;

ALANINE; ANISOTROPY; MAGNETIC RESONANCE SPECTROSCOPY; TRICHLOROACETIC ACID; TYROSINE;

EID: 0034267896     PISSN: 10907807     EISSN: None     Source Type: Journal    
DOI: 10.1006/jmre.2000.2119     Document Type: Article

References (64)

1. E. R. Andrew, The narrowing of NMR spectra of solids by high-speed specimen rotation and the resolution of chemical shift and spin multiplet structures for solids, Prog. NMR Spectrosc. 8, 1-39 (1971).
2. M. M. Maricq and J. S. Waugh, NMR in rotating solids, J. Chem. Phys. 70, 3300-3316 (1979).
3. J. Herzfeld and A. E. Berger, Sideband intensities in NMR spectra of samples spinning at the magic angle, J. Chem. Phys. 73, 6021-6030 (1980).
4. C. Filip, S. Hafner, I. Schnell, D. E. Demco, and H. W. Spiess, Solid-state nuclear magnetic resonance spectra of dipolar-coupled multi-spin systems under fast magic-angle spinning, J. Chem. Phys. 110, 423-440 (1999).
5. H. Geen, J. J. Titman, J. Gottwald, and H. W. Spiess, Solid-state proton multiple-quantum NMR spectroscopy with fast magic angle spinning, Chem. Phys. Lett. 227, 79-86 (1994).
6. J. Gottwald, D. E. Demco, R. Graf, and H. W. Spiess, High-resolution double-quantum NMR spectroscopy of homonuclear spin pairs and proton connectivities in solids, Chem. Phys. Lett. 243, 314-323 (1995).
7. R. Graf, D. E. Demco, J. Gottwald, S. Hafner, and H. W. Spiess, Dipolar couplings and internuclear distances by double-quantum nuclear magnetic resonance spectroscopy of solids, J. Chem. Phys. 106, 885-895 (1997).
8. U. Friedrich, I. Schnell, D. E. Demco, and H. W. Spiess, Triple-quantum NMR spectroscopy in dipolar solids, Chem. Phys. Lett. 285, 49-58 (1998).
9. U. Friedrich, I. Schnell, S. P. Brown, A. Lupulescu, D. E. Demco, and H. W. Spiess, Spinning-sideband patterns in multiple-quantum magic-angle spinning NMR spectroscopy, Mol. Phys. 95, 1209-1227 (1998).
10. K. Saalwächter, R. Graf, D. E. Demco, and H. W. Spiess, Heteronuclear double-quantum MAS NMR spectroscopy in dipolar solids, J. Magn. Reson. 139, 287-301 (1999).
11. 13C multiple-quantum correlation in solids under ultra-fast MAS, J. Magn. Reson. 140, 471-476 (1999).
12. L. Marinelli and L. Frydman, On the origin of spinning sidebands in MQMAS NMR experiments, Chem. Phys. Lett. 275, 188-198 (1997).
13. J.-P. Amoureux, M. Pruski, D. P. Lang, and C. Fernandez, The effect of RF power and spinning speed on MQMAS NMR, J. Magn. Reson. 131, 170-175 (1998).
14. T. Charpentier, C. Fermon, and J. Virlet, Numerical and theoretical analysis of multiquantum magic-angle spinning experiments, J. Chem. Phys. 109, 3116-3130 (1998).
15. A. F. de Jong, A. P. M. Kentgens, and W. S. Veeman, Two-dimensional exchange NMR in rotating solids: A technique to study very slow molecular reorientations, Chem. Phys. Lett. 109, 337-342 (1984).
16. A. Hagemeyer, K. Schmidt-Rohr, and H. W. Spiess, Two-dimensional nuclear magnetic resonance experiments for studying molecular order and dynamics in static and in rotating solids, Adv. Magn. Reson. 13, 85-130 (1989).
17. R. Tycko and A. E. Berger, Dual processing of two-dimensional exchange data in magic angle spinning NMR of solids, J. Magn. Reson. 141, 141-147 (1999).
18. 1H NMR imaging of residual dipolar couplings in cross-linked elastomers: Dipolar-encoded longitudinal magnetization, double-quantum, and triple-quantum filters, J. Magn. Reson. 140, 432-441 (1999).
19. R. R. Ernst, G. Bodenhausen, and A. Wokaun, "Principles of Nuclear Magnetic Resonance in One and Two Dimensions," 2nd ed., Clarendon Press, Oxford (1991).
20. T. Gullion and J. Schaefer, Rotational-echo double-resonance NMR, J. Magn. Reson. 81, 196-200 (1989).
21. R. Tycko and G. Dabbagh, Double-quantum filtering in magic-angle-spinning NMR spectroscopy: An approach to spectral simplification and molecular-structure determination, J. Am. Chem. Soc. 113, 9444-9448 (1991).
22. M. Feike, D. E. Demco, R. Graf, J. Gottwald, S. Hafner, and H. W. Spiess, Broadband multiple-quantum NMR spectroscopy, J. Magn. Reson. A 122, 214-221 (1996).
23. Y. K. Lee, N. D. Kurur, M. Helmle, O. G. Johannessen, N. C. Nielsen, and M. H. Levitt, Efficient dipolar recoupling in the NMR of rotating solids. A sevenfold symmetric radiofrequency pulse sequence, Chem. Phys. Lett. 242, 304-309 (1995).
24. 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).
25. A. E. Bennett, R. G. Griffin, and S. Vega, Recoupling of homo- and heteronuclear dipolar interactions in rotating solids, NMR Basic Principles Prog. 33, 1-77 (1994).
26. 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).
27. C. A. Michal and L. W. Jelinski, REDOR 3D: Heteronuclear distance measurements in uniformly labeled and natural abundance solids, J. Am. Chem. Soc. 119, 9059-9060 (1997).
28. M. Abramowitz and I. A. Stegun (Eds.), "Handbook of Mathematical Functions," Dover, New York (1972).
29. J. M. Goetz and J. Schaefer, REDOR dephasing by multiple spins in the presence of molecular motion, J. Magn. Reson. 127, 147-154 (1997).
30. 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).
31. C. Schmidt, K. J. Kuhn, and H. W. Spiess, Distribution of correlation times in glassy polymers from pulsed deuteron NMR, Prog. Colloid Polym. Sci. 71, 71-76 (1985).
32. 13C NMR, Macromolecules 17, 1479-1489 (1984).
33. K. Saalwächter and K. Schmidt-Rohr, Relaxation-induced dipolar exchange with recoupling: An MAS NMR method for determining heteronuclear distances without irradiating the second spin, J. Magn. Reson., in press.
34. H. W. Spiess, Rotation of molecules and nuclear spin relaxation, NMR Basic Principles Prog. 15, 55-214 (1978).
35. 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).
36. W. H. Press, S. A. Teukolsky, W. T. Vetterling, and B. P. Flannery, "Numerical Recipes in C: The Art of Scientific Computing," 2nd ed., Cambridge Univ. Press, Cambridge (1992).
37. S. A. Smith, T. O. Levante, B. H. Meier, and R. R. Ernst, Computer simulations in magnetic resonance: An object-oriented programming approach, J. Magn. Reson. A 106, 75-105 (1994).
38. V. B. Cheng, H. H. Suzakawa, Jr., and M. Wolfsberg, Investigations of a non-random numerical method for multidimensional integration, J. Chem. Phys. 59, 3992-3999 (1973).
39. "Matlab Reference Guide," The Mathworks Inc., Natick, MA (1992).
40. 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).
41. M. Munowitz, W. P. Aue, and R. G. Griffin, Two-dimensional separation of dipolar and scaled isotropic chemical-shift interactions in magic-angle NMR spectra, J. Chem. Phys. 77, 1686-1689 (1982).
42. 13C NMR of polymers, J. Magn. Reson. 52, 123-129 (1983).
43. M. Linder, A. Höhener, and R. R. Ernst, Orientation of tensorial interactions determined from two-dimensional NMR powder spectra, J. Chem. Phys. 73, 4959-4970 (1980).
44. E. R. Henry and A. Szabo, Influence of vibrational motion on solid state line shapes and NMR relaxation, J. Chem. Phys. 82, 4753-4761 (1985).
45. T. Nakai, J. Ashida, and T. Terao, Influence of small-amplitude motions on two-dimensional powder patterns: Anisotropic vibrations in calcium formate, Mol. Phys. 67, 839-847 (1989).
46. D. W. Alderman, G. McGeorge, J. Z. Hu, R. J. Pugmire, and D. M. Grant, A sensitive high resolution magic angle turning experiment for measuring chemical shift tensor principle values, Mol. Phys. 95, 1113-1126 (1998).
47. 13C heteronuclear correlation in the limit of fast MAS, in preparation.
48. S. M. De Paul, unpublished results.
49. T. Gullion, M. D. Poliks, and J. Schaefer, Extended dipolar modulation and magic-angle spinning, J. Magn. Reson. 80, 553-558 (1988).
50. A. W. Hing, S. Vega, and J. Schaefer, Transferred-echo double-resonance NMR, J. Magn. Reson. 96, 205-209 (1992).
51. A. W. Hing, S. Vega, and J. Schaefer, Measurement of heteronuclear dipolar coupling by transferred-echo double-resonance NMR, J. Magn. Reson. A 103, 151-162 (1993).
52. W. S. Warren, S. Sinton, D. P. Weitekamp, and A. Pines, Selective excitation of double-quantum coherence in nuclear magnetic resonance, Phys. Rev. Lett. 43, 1791-1794 (1979).
53. J. Baum, M. Munowitz, A. N. Garroway, and A. Pines, Multiple-quantum dynamics in solid-state NMR, J. Chem. Phys. 83, 2015-2025 (1985).
54. P.-G. Jönsson and W. C. Hamilton, Hydrogen bond studies. LX. A single crystal neutron diffraction study of trichloroacetic acid dimer, J. Chem. Phys. 56, 4433-4439 (1972).
55. C. R. Dybowski, B. C. Gerstein, and R. W. Vaughan, The proton chemical shift tensor in trichloroacetic acid, J. Chem. Phys. 67, 3412-3415 (1977).
56. A. Stöckli, B. H. Meier, R. Kreis, R. Meyer, and R. R. Ernst, Hydrogen bond dynamics in isotopically substituted benzoic acid dimers, J. Chem. Phys. 93, 1502-1520 (1990).
57. A. Heuer and U. Haeberlen, The dynamics of hydrogens in double well potentials: The transition of the jump rate from the low temperature quantum-mechanical to the high temperature activated regime, J. Chem. Phys. 95, 4201-4214 (1991).
58. M. Neumann, D. F. Brougham, C. J. McGloin, M. R. Johnson, A. J. Horsewill, and H. P. Trommsdorf, Proton tunneling in benzoic acid crystals at intermediate temperatures: Nuclear magnetic resonance and neutron scattering studies, J. Chem. Phys. 109, 7300-7311 (1998).
59. 31P cross-polarization magic-angle spinning nuclear magnetic resonance studies on two-spin systems with homonuclear dipolar coupling and J coupling, J. Chem. Phys. 92, 7156-7170 (1990).
60. R. Tycko and S. O. Smith, Symmetry principles in the design of pulse sequences for structural measurements in magic angle spinning nuclear magnetic resonance, J. Chem. Phys. 98, 932-943 (1993).
61. I. Schnell, Doppelquantenspektroskopie an polykristallinen Phosphaten, Diploma thesis, Johannes Gutenberg University, Mainz, Germany (1996).
62. 31P NMR: A new approach to structural studies of thiophosphates, Chem. Eur. J. 4, 1762-1767 (1998).
63. K. T. Mueller, Analytic solutions for the time evolution of dipolar-dephasing NMR signals, J. Magn. Reson. A 113, 81-93 (1995).
64. T. Gullion, D. B. Baker, and M. S. Conradi, New compensated Carr-Purcell sequences, J. Magn. Reson. 89, 479-484 (1990).