Analyses of the complex proton NMR spectra: Determination of anisotropic proton chemical shifts of oriented molecules by a two dimensional experiment

Journal of Magnetic Resonance

Volumn 185, Issue 2, 2007, Pages 240-246

  Mavinkurve, Raghav G ^a   Deepak, H S Vinay ^a   Ramanathan, K V ^a   Suryaprakash, N ^a  

^a INDIAN INSTITUTE OF SCIENCE   (India)

Author keywords

Decoupling; Dipolar couplings; Iodopropane; Lee Goldburg; Mucononitrile; NMR

Indexed keywords

ANISOTROPY; CHEMICAL SHIFT; COMPUTER SIMULATION; MOLECULAR DYNAMICS; MOLECULAR STRUCTURE; NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY;

DECOUPLING; DIPOLAR COUPLINGS; IODOPROPANE; LEE GOLDBURG; MUCONONITRILE;

PROTONS;

NITRILE; PROTON;

ALGORITHM; ANISOTROPY; ARTICLE; CHEMICAL MODEL; CHEMICAL STRUCTURE; CHEMISTRY; COMPUTER SIMULATION; CONFORMATION; METHODOLOGY; NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY;

ALGORITHMS; ANISOTROPY; COMPUTER SIMULATION; MAGNETIC RESONANCE SPECTROSCOPY; MODELS, CHEMICAL; MODELS, MOLECULAR; MOLECULAR CONFORMATION; NITRILES; PROTONS;

EID: 34247395398     PISSN: 10907807     EISSN: 10960856     Source Type: Journal    
DOI: 10.1016/j.jmr.2006.12.016     Document Type: Article

References (46)

1. Diehl P., and Khetrapal C.L. In: Diehl P., Fluck E., and Kosfeld R. (Eds). NMR Basic Principles and Progress vol. 1 (1969), Springer Verlag, Berlin
2. Suryaprakash N. Structure of molecules by NMR using liquid crystal solvents. Concept. Magnetic Res. 10 (1998) 167
3. Suryaprakash N. Liquid crystals as solvents in NMR Spectroscopy : current developments in structure determination. Curr. Org. Chem. 4 (2000) 85
4. Christy Rani Grace R., and Suryaprakash N. In: Rahman A.-u. (Ed). New Advances in Analytical Techniques vol. 1 (2000), Harwood Academic Press, The Netherlands 441-484
5. Lounila J., and Jokisaari J. Anisotropies in spin-spin coupling constants and chemical shifts as determined from the NMR spectra of molecules oriented by liquid crystal solvents. Prog. Nucl. Mag. Res. Sp. 15 (1982) 249
6. Stephenson D.S., and Binsch G. The molecular structure of cyclopentene in solution as obtained from a nematic phase proton N.M.R. study. Mol. Phys. 43 (1980) 697
7. Field L.D., Pierens G.K., Carpenter T.A., Colebrook L.D., and Hall L.D. Selection of multiple quantum spectra of molecules in liquid crystalline solution using pulsed magnetic field gradients. J. Magn. Reson. 99 (1992) 398
8. 1H NMR study of partially oriented biphenylene. J. Magn. Reson. A106 (1994) 223
9. Rendell J.C.T., and Burnell E.E. Frequency selective excitation in multiple quantum NMR. J. Magn. Reson. A112 (1995) 1
10. 1H-NMR study of conformational biasing of biphenyl in a nematic liquid crystal. J. Magn. Reson. A118 (1996) 264
11. 1H-NMR of butane in a nematic liquid crystal. J. Chem. Phys. 103 (1995) 6891
12. Celebre G., Castiglione F., Longeri M., and Emsley J.W. The NMR spectra of samples dissolved in liquid-crystalline phases automatic analysis with the aid of multiple-quantum spectra. J. Magn. Reson. 121A (1996) 139
13. Frydman L., Rossomando P.C., and Frydman B. Applications of Multi-Pulse sequences to the simplification of Liquid Crystal NMR Spectra. J. Magn. Reson. 95 (1991) 484
14. Lesot P., Ouvrard J.M., Ouvrard B.N., and Courtieu J. Coherent reduction of dipolar interactions in molecules dissolved in anisotropic media using a new multiple-pulse sequence in a COSY experiment. J. Magn. Reson. 107A (1994) 141
15. Nanz D., Ernst M., Hong M., Ziegeweid M.A., Schmidt-Rohr K., and Pines A. Low-power decoupling sequences for high-resolution chemical-shift and local-field NMR spectra of liquid crystals. J. Magn. Reson. A113 (1995) 169
16. Courtieu J., Alderman D.W., Grant D.M., and Bayle J.P. Director dynamics and NMR applications of nematic liquid crystals spinning at various angles from the magnetic field. J. Chem. Phys. 77 (1982) 723
17. Kimura A., Kuni N., and Fujiwara H. Orientation and conformation of Met-enkephalin in a liquid crystal as studied by magic-angle- and near-magic-angle-spinning two-dimensional NMR spectroscopy. J. Phys. Chem. 100 (1996) 14056
18. Vivekanandan S., and Suryaprakash N. Novel method of estimating proton-proton dipolar couplings to aid the analyses of NMR spectra of oriented molecules using two dimensional inverse experiment. Chem. Phys. Lett. 138 (2001) 247
19. Stepehenson D.S., and Binsch G. Automated analysis of high-resolution NMR Spectra I. Principles and computational Strategy. J. Magn. Reson. 37 (1980) 395
20. Stepehenson D.S., and Binsch G. Automated analysis of high-resolution NMR spectra. III. The nematic phase spectra of three allyl halides. Org. Magn. Reson. 14 (1980) 226
21. Pfandler P., and Bodenhausen G. Toward automated analysis of dipole-coupled NMR spectra of solutes in liquid crystals. J. Magn. Reson. 91 (1991) 65
22. Castiglione F., Carravetta M., Celebre G., and Longeri M. Toward a generalized algorithm for the automated analysis of complex anisotropic NMR spectra. J. Magn. Reson. 132 (1998) 1-12
23. Diehl P., and Vogt J. Automatic analysis of NMR spectra: practical application to the spectra of oriented 2,4-dichlorobenzaldehyde and 2-chlorobenzaldehyde. Org. Magn. Reson. 8 (1976) 638
24. Diehl P., Sykora S., and Vogt J. Automatic analysis of NMR spectra: an alternative approach. J. Magn. Reson. 19 (1975) 67
25. Laatikainen R., Niemitz M., Weber U., Sundelin J., Hassinen T., and Vespäläinen J. General strategies for total-lineshape-type spectral analysis of NMR spectra using integral-transform iterator. J. Magn. Reson. 120A (1996) 1
26. Christy Rani Grace R., Suryaprakash N., Kumar A., and Khetrapal C.L. Application of a modified Z-COSY experiment for the analysis of spectra of oriented molecules-The spectrum of cis,cis-mucononitrile. J. Magn. Reson. 107A (1994) 79
27. 1H NMR using a liquid crystal solvent: tolan and trans-azobenzene. J. Phys. Chem. A 105 (2001) 6711 and the references therein
28. Waugh J.S., Huber L.M., and Haeberlen U. Approach to high resolution NMR in solids. Phy. Rev. Lett. 20 (1968) 180
29. Lee M., and Goldburg W.I. Nuclear magnetic resonance line narrowing by a rotating RF field. Phys. Rev. A 140 (1965) 1261
30. Mehring M., and Waugh J.S. Magic-angle NMR experiments in solids. Phys. Rev. B 5 (1972) 3459
31. 13C NMR heteronuclear dipolar-correlation spectroscopy of solids with frequency-switched Lee-Goldburg homonuclear decoupling. J. Magn. Reson. 124 (1997) 516
32. 1H NMR in solids with frequency-switched multiple pulse sequences. Solid State NMR 2 (1993) 151
33. Vinogradov E., Madhu P.K., and Vega S. High-resolution proton solid-state NMR spectroscopy by phase-modulated Lee-Goldburg experiment. Chem. Phys. Lett. 314 (1999) 443-450
34. Ramamoorthy A., Wu C.H., and Opella S.J. Resolved two-dimensional anisotropic-chemical-shift/heteronuclear dipolar coupling powder-pattern spectra by three-dimensional solid-state NMR spectroscopy. J. Magn. Reson. B110 (1999) 102
35. Wu C.H., Ramamoorthy A., and Opella S.J. High-resolution heteronuclear dipolar solid-state NMR spectroscopy. J. Magn. Reson. A109 (1994) 270
36. Nishimura K., and Naito A. Dramatic reduction of the RF power for attenuation of sample heating in 2D-separated local field solid-state NMR spectroscopy. Chem. Phys. Lett. 402 (2005) 245
37. Lee D.K., Narasimhaswamy T., and Ramamoorthy A. PITANSEMA, a low-power PISEMA solid state NMR experiment. Chem. Phys. Lett. 399 (2004) 359
38. Yamamoto K., Ermakov L., Lee D.K., and Ramamoorthy V.A. PITANSEMA-MAS, a solid state NMR method to measure heteronuclear dipolar couplings under MAS. Chem. Phys. Lett. 408 (2005) 118
39. Ramamoorthy A., Wei Y., and Lee D.K. PISEMA solid-state NMR spectroscopy. Annu. Rep. NMR Spectroscopy 52 (2004) 1
40. Schmidt-Rohr K., Nanz D., Emsley L., and Pines A. NMR measurement of resolved heteronuclear dipole couplings in liquid crystals and lipids. J. Phys. Chem. 98 (1994) 6668
41. Hong M., Schmidt-Rohr K., and Pines A. NMR measurement of signs and magnitudes of C-H dipolar couplings in lecithin. J. Am. Chem. Soc. 117 (1995) 3310
42. Hong M., Pines A., and Caldarelli S. Measurement and assignment of long-range C-H dipolar couplings in liquid crystals by twodimensional NMR spectroscopy. J. Phys. Chem. 100 (1996) 14815
43. Caldarelli S., Hong M., Emsley L., and Pines A. Measurement of carbon-proton dipolar couplings in liquid crystals by local dipolar field NMR spectroscopy. J. Phys. Chem. 100 (1996) 18696
44. Marjanska M., Castiglione F., Walls J.D., and Pines A. Measurement of dipolar couplings in partially oriented molecules by local field NMR spectroscopy with low power decoupling. J. Magn. Reson. 158 (2002) 52
45. 13C MAS NMR Spectra of cis,cis-Mucononitrile in liquid crystalline media and the solid state - orientation of the carbon chemical shift tensors. J. Magn. Reson. Ser. A 123 (1996) 196
46. Diehl P., Khetrapal C.L., and Kellerhals H.P. The N.M.R. spectrum of pyridine oriented in the nematic phase. Mol. Phys. 15 (1968) 333