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Double‐quantum homonuclear rotary resonance: Efficient dipolar recovery in magic‐angle spinning nuclear magnetic resonance
1.E. R. Andrew, S. Clough, L. F. Farnell, T. D. Gledhill, and I. Roberts, Phys. Lett. 21, 505 (1966);
1.D. P. Raleigh, M. H. Levitt, and R. G. Griffin, Chem. Phys. Lett. 146, 71 (1988);
1.M. G. Colombo, B. H. Meier, and R. R. Ernst, Chem. Phys. Lett. 146, 189 (1988); , Chem. Phys. Lett.
1.W. E. J. R. Maas and W. S. Veeman, Chem. Phys. Lett. 149, 170 (1988); , Chem. Phys. Lett.
1.Z.-H. Gan and D. M. Grant, Mol. Phys. 67, 1419 (1989);
1.D. P. Raleigh, F. Creuzet, S. K. Das Gupta, M. H. Levitt, and R. G. Griffin, J. Am. Chem. Soc. 111, 4502 (1989);
1.A. Schmidt and S. Vega, J. Chem. Phys. 96, 2655 (1992);
1.T. Nakai and C. A. McDowell, J. Chem. Phys. 96, 3452 (1992); , J. Chem. Phys.
1.F. Creuzet, D. P. Raleigh, M. H. Levitt, and R. G. Griffin, J. Am. Chem. Soc. (in press).
2.M. H. Levitt, D. P. Raleigh, F. Creuzet, and R. G. Griffin, J. Chem. Phys. 92, 6347 (1990).
3.A. E. McDermott, F. Creuzet, R. G. Griffin, L. E. Zawadzke, Q.-Z. Ye, and C. T. Walsh, Biochemistry 29, 5767 (1990);
3.F. Creuzet, A. McDermott, R. Gebhard, K. Van der Hoef, M. B. Spijker-Assink, J. Herzfeld, J. Lugtenburg, M. H. Levitt, and R. G. Griffin, Science 251, 783 (1991);
3.R. G. S. Spencer, K. J. Halverson, M. Auger, A. E. McDermott, R. G. Griffin, and P. T. Lansbury, Jr., Biochemistry 30, 10 382 (1991);
3.L. K. Thompson, A. E. McDermott, J. Raap, C. M. van der Wielen, J. Lugtenburg, J. Herzfeld, and R. G. Griffin, Biochemistry 31, 7931 (1992); , Biochemistry
3.K. V. Lakshmi, M. Auger, J. Raap, J. Lugtenburg, R. G. Griffin, and J. Herzfeld, J. Am. Chem. Soc. 115, 8515 (1993).
4.N. C. Nielsen, F. Creuzet, and R. G. Griffin, J. Magn. Reson. Ser. A 103, 245 (1993).
5.R. Tycko and G. Dabbagh, Chem. Phys. Lett. 173, 461 (1990).
6.T. G. Oas, R. G. Griffin, and M. H. Levitt, J. Chem. Phys. 89, 692 (1988);
6.M. H. Levitt, T. G. Oas, and R. G. Griffin, Isr. J. Chem. 28, 271 (1988). There are errors in the analytical form for rotary resonance line shape [Eq. (24) and Fig. 3(b)] in the latter paper.
7.T. Gullion and J. Schaefer, J. Magn. Reson. 81, 196 (1989);
7.Y. Pan, T. Gullion, and J. Schaefer, J. Magn. Reson. 90, 330 (1990)., J. Magn. Reson. (1969-1992)
8.A. Wokaun and R. R. Ernst, Chem. Phys. Lett. 52, 407 (1977).
9.A. Bax, R. Freeman, and S. P. Kempsell, J. Magn. Reson. 41, 349 (1980);
9.A. Bax, R. Freeman, and S. P. Kempsell, J. Am. Chem. Soc. 102, 4849 (1980).
10.E. M. Menger, S. Vega, and R. G. Griffin, J. Am. Chem. Soc. 108, 2215 (1986).
11.T. A. Early, B. K. John, and L. F. Johnson, J. Magn. Reson. 75, 134 (1987);
11.R. Benn, H. Grondey, C. Brevard, and A. Pagelot, J. Chem. Soc. Chem. Commun. 1988, 102.
12.B. H. Meier and W. L. Earl, J. Chem. Phys. 85, 4905 (1986);
12.B. H. Meier and W. L. Earl, J. Am. Chem. Soc. 109, 7937 (1987).
13.R. Tycko and G. Dabbagh, J. Am. Chem. Soc. 113, 9444 (1991);
13.R. Tycko and S. O. Smith, J. Chem. Phys. 98, 932 (1993).
14.N. C. Nielsen, F. Creuzet, R. G. Griffin, and M. H. Levitt, J. Chem. Phys. 96, 5668 (1992).
15.A. Wokaun and R. R. Ernst, J. Chem. Phys. 67, 1752 (1977);
15.S. Vega, J. Chem. Phys. 68, 5518 (1978)., J. Chem. Phys.
16.For DRAMA, a weaker dependence on γ may be produced by adjusting the pulse spacing. However, the recoupled dipolar interaction is then smaller.
17.Z.-H. Gan and D. M. Grant, Chem. Phys. Lett. 168, 304 (1990);
17.A. C. Kolbert, D. P. Raleigh, R. G. Griffin, and M. H. Levitt, J. Magn. Reson. 89, 133 (1990).
18.The 2Q nutation frequency of DRAMA may be doubled by bracketing the sequence by two π/2 pulses, out of phase by This leads to an even more rapid 2Q excitation than for 2Q-HORROR, but does not remedy the γ dependence: The maximum achievable 2QF efficiency is unchanged.
19.G. Bodenhausen, H. Kogler, and R. R. Ernst, J. Magn. Reson. 58, 370 (1984).
20.All experiments were performed on a Varian VXR-400 S spectrometer (operating at 100.6 MHz for equipped with a home-built MAS probe using 7 mm rotors (5 mm inner diameter) with enlarged torlon end-caps restricting the sample volume to the central 3.5 mm in the axial dimension in order to reduce effects from rf inhomogeneity (Ref. 25). The experiments used 99% doubly labeled alanine (Figs. 3 and 5) and a mixture (Fig. 4) of 20.2 mg 99% labeled alanine, 20.3 mg L-leucine, and 20.4 mg L-valine (the two latter with in natural abundance). labeled L-alanine compounds were purchased from Isotec, Inc. (Miamisburg, OH) and used without further purification. The carrier frequency were placed at the mean isotropic shift of the L-alanine and CH carbons. rf field strengths of 22.5 and 27.2 kHz were used for cross polarization (100 μs of spin-lock) and πsol;2 pulses, respectively. rf field strengths of 52.1, 22.5, and 52.1 kHz were used for the initial pulse, cross polarization, and decoupling, respectively. The 2Q-HORROR 2QF pulse sequence [Fig. 2(a)] used a 64 step phase cycle constructed according to standard procedures (Ref. 19).
21.The simulations employed the parameters: chemical shift tensor with principal elements (Ref. 26) and ppm, and a CH chemical shift tensor with principal elements and ppm. Euler angles (degrees) for the dipolar, CSA, and CH CSA tensors were (0.0, 78.4, −35.3), (39.5, 77.4, −52.9), and (81.7, 24.5, 29.1). The chemical shift tensors (ppm values relative to liquid benzene) and the bond direction (orientation of dipolar tensor) are taken from Ref. 27. All simulations were performed on a Digital VAX-6210 computer. Calculation of a 2Q-HORROR spectrum typically required 15–20 α and 15–20 β angles equally distributed over their respective ranges and integration of the homogeneous evolution using 20–40 steps per rotor period.
22.M. Mehring, Principles of High Resolution NMR of Solids, 2nd ed. (Springer, New York, 1983).
23.U. Haeberlen and J. S. Waugh, Phys. Rev. 175, 453 (1968);
23.M. H. Levitt, A. C. Kolbert, A. Bielecki, and D. J. Ruben, Solid State Nucl. Magn. Reson. 2, 151 (1993).
24.T. M. Barbara, R. Tycko, and D. P. Weitekamp, J. Magn. Reson. 62, 54 (1985).
25.N. C. Nielsen, H. Bilds/e, and H. J. Jakobsen, J. Magn. Reson. 98, 665 (1992).
26.H. W. Spiess, in NMR Basic Principles and Progress, edited by P. Diehl, E. Fluck, and E. Kosfeld (Springer, Berlin, 1978).
27.A. Naito, S. Ganapathy, K. Akasaka, and C. A. McDowell, J. Chem. Phys. 74, 3190 (1981).
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