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2005 | 3 | 2 | 245-251
Tytuł artykułu

2H Chemical-shift resolution and dipolar2H-1H,2H-15N correlations in solid-state MAS NMR spectroscopy for structure determination and distance measurements in hydrogen-bonded systems

Treść / Zawartość
Warianty tytułu
Języki publikacji
EN
Abstrakty
EN
In solid-state NMR, deuteron (2H) spectroscopy can be performed in full analogy to1H spectroscopy, including2H chemical-shift resolution and2H-X dipolar correlation schemes, when the NMR experiments are conducted in a “rotor-synchronized” fashion under fast magic-angle spinning. Here, 2H-X NMR experiments of this type, including2H-15N and2H-1H chemical-shift correlations and distance measurements, are introduced and demonstrated on cytosine monohydrate, whose acidic protons can readily be replaced by deuterons by recrystallization from D2O. In this way,2H NMR spectroscopy provides information complementary to1H NMR data, which is particularly useful for studying hydrogen bonds in supra- or biomolecular systems.
Wydawca

Czasopismo
Rocznik
Tom
3
Numer
2
Strony
245-251
Opis fizyczny
Daty
wydano
2005-06-01
online
2005-06-01
Twórcy
  • Max Planck Institute for Polymer Research, Postfach 3148, 55021, Mainz, Germany
autor
Bibliografia
  • [1] I. Schnell, S.P. Brown, H.Y. Low, H. Ishida and H.W. Spiess: “An investigation of hydrogen bonding in benzoxazine dimers by fast magic-angle spinning and doublequantum1H NMR spectroscopy”,J. Am. Chem. Soc., Vol. 120, (1998), 11784. http://dx.doi.org/10.1021/ja982766t[Crossref]
  • [2] M. Ernst, M.A. Meier, T. Tuherm, A. Samoson and B.H. Meier: “Low-power high-resolution solid-state NMR of peptides and proteins”,J. Am. Chem. Soc., Vol. 126, (2004), p. 4764. http://dx.doi.org/10.1021/ja0494510[Crossref]
  • [3] A. Lesage, L. Duma, D. Sakellariou and L. Emsley: “Improved resolution in proton NMR spectroscopy of powdered solids”,J. Am. Chem. Soc., Vol. 123, (2001), p. 5747. http://dx.doi.org/10.1021/ja0039740[Crossref]
  • [4] P.K. Madhu, E. Vinogradov and S. Vega: “Multiple-pulse and magic-angle spinning aided double-quantum proton solid-state NMR spectroscopy”,Chem. Phys. Lett., Vol. 394, (2004), p. 423. http://dx.doi.org/10.1016/j.cplett.2004.07.034[Crossref]
  • [5] I. Schnell: “Dipolar recoupling under fast MAS conditions”,Progr. NMR Spectr., Vol. 145, (2004), p. 45.
  • [6] K. Schmidt-Rohr and H.W. Spiess:Multidimensional Solid State NMR and Polymers, Academic Press, New York, 1994.
  • [7] C. Müller, W. Schajor, H. Zimmermann and U. Haeberlen: “Deuteron chemical shift and EFG tensors in α-glycine”,J. Magn. Reson., Vol. 56, (1984), p. 235.
  • [8] H. Schmitt, H. Zimmermann, O. Korner, M. Stumber, C. Meinel and U. Haeberlen: “Precision measurement of the quadrupole coupling and chemical shift tensors of the deuterons in alpha-calcium formates”,J. Magn. Reson., Vol. 151, (2001), p. 65. http://dx.doi.org/10.1006/jmre.2001.2345[Crossref]
  • [9] S. Antonijevic and S. Wimperis: “Refocusing of chemical and paramagnetic shift anisotropies in2H NMR using the quadrupolar-echo experiment”,J. Magn. Reson., Vol. 164, (2003), p. 343. http://dx.doi.org/10.1016/S1090-7807(03)00272-6[Crossref]
  • [10] A. Hoffmann and I. Schnell: “Two-dimensional double-quantum2H NMR spectroscopy in the solid state under OMAS conditions: Correlating2H chemical shifts with quasistatic lineshapes”,Chem.Phys.Chem., Vol. 5, (2004), p. 966.
  • [11] M.M. Maricq and J.S. Waugh: “NMR in rotating solids”,J. Chem. Phys., Vol. 70, (1979), p. 3300. http://dx.doi.org/10.1063/1.437915[Crossref]
  • [12] I.G. Shenderovich, H.H. Limbach, S.N. Smirnov, P.M. Tolstoy, G.S. Denisov and N.S. Golubev: “H/D isotope effects on the low-temperature NMR parameters and hydrogen bond geometries of (FH)(2)F- and (FH)(3)F- dissolved in CDF3/CDF2Cl”,Phys. Chem. Chem. Phys., Vol. 4 (2002), p. 5488. http://dx.doi.org/10.1039/b206323a[Crossref]
  • [13] T. Gullion: “Introduction to rotational-echo, double-resonance NMR”,Concepts Magn. Reson., Vol. 10, (1998), p. 277. http://dx.doi.org/10.1002/(SICI)1099-0534(1998)10:5<277::AID-CMR1>3.0.CO;2-U[Crossref]
  • [14] I. Sack, A. Goldbourt, S. Vega and G.J. Buntkowsky: “Deuterium REDOR: Principles and applications for distance measurements”,J. Magn. Reson., Vol. 138, (1999), p. 54. http://dx.doi.org/10.1006/jmre.1999.1710[Crossref]
  • [15] H.P. Weber, B.M. Craven and R.K. McMullan: “The structure of deuterated cytosine monohydrate at 82 K by neutron diffraction”,Acta Cryst. B, Vol. 36, (1980), p. 645. http://dx.doi.org/10.1107/S0567740880003986[Crossref]
  • [16] K. Saalwächter and I. Schnell: “REDOR-based heteronuclear dipolar correlation experiments in multi-spin systems: Rotor-encoding, directing, and multiple distance and angle determination”,Solid State NMR, Vol. 22, (2002), p. 157. http://dx.doi.org/10.1006/snmr.2002.0079[Crossref]
  • [17] D.A. Case: “Calculations of NMR dipolar coupling strengths in model peptides”,J. Biomol. NMR, Vol.15, (1999), p. 95. http://dx.doi.org/10.1023/A:1008349812613[Crossref]
Typ dokumentu
Bibliografia
Identyfikatory
Identyfikator YADDA
bwmeta1.element.-psjd-doi-10_2478_BF02551530
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