NMR measurements of scalar-coupling distributions in disordered solids
作者： Sylvian Cadars , Anne Lesage , Michel Trierweiler , Laurent Heux , Lyndon Emsley
DOI: 10.1039/B611096G
关键词: Dipole 、 Analytical chemistry 、 Scalar (physics) 、 Scalar coupling 、 Chemical physics 、 Chemistry
摘要: The measurement of scalar (J) couplings by solid-state NMR is a field great interest, since this interaction rich source local structural information, complementary to dipolar and chemical shift interactions. Here, we first demonstrate that J-coupling distributions exist can be observed in disordered solids, as illustrated with the observation pair-specific distribution 2J(31P–N–31P) bis-phosphino amine, investigate potential effects such on average constants. Second, show two-dimensional (2D) J-couplings provides much richer probe disorder than one-dimensional distributions, introduce new methods provide different (selective or non-selective) ways measuring 2D J wide range systems. These are finally applied slightly polymorphic sample fully 13C-enriched cellulose, then amine sample, from which 2JPP-coupling clearly identified interpreted.
rsc.org
harvard.edu
archives-ouvertes.fr
sci-hub.se 参考文章(62)
S. P. Brown, M. Pérez-Torralba, D. Sanz, R. M. Claramunt, L. Emsley, Determining hydrogen-bond strengths in the solid state by NMR: the quantitative measurement of homonuclear J couplings Chemical Communications. pp. 1852- 1853 ,(2002) , 10.1039/B205324A
Franck Fayon, Ian J King, Robin K Harris, John S.O Evans, Dominique Massiot, Application of the through-bond correlation NMR experiment to the characterization of crystalline and disordered phosphates Comptes Rendus Chimie. ,vol. 7, pp. 351- 361 ,(2004) , 10.1016/J.CRCI.2003.10.019
Denes Konya, Frédéric Robert, Yves Gimbert, Andrew E. Greene, Asymmetric Pauson–Khand reaction with chiral, electron-deficient mono- and bis-phosphine ligands Tetrahedron Letters. ,vol. 45, pp. 6975- 6978 ,(2004) , 10.1016/J.TETLET.2004.07.091
Steven P. Brown, Marta Pérez-Torralba, Dionísia Sanz, Rosa María Claramunt, Lyndon Emsley, The Direct Detection of a Hydrogen Bond in the Solid State by NMR through the Observation of a Hydrogen-Bond Mediated 15N−15N J Coupling Journal of the American Chemical Society. ,vol. 124, pp. 1152- 1153 ,(2002) , 10.1021/JA0172262
Hiroyuki Kono, Yukari Numata, Tomoki Erata, Mituo Takai, 13C and 1H Resonance Assignment of Mercerized Cellulose II by Two-Dimensional MAS NMR Spectroscopies Macromolecules. ,vol. 37, pp. 5310- 5316 ,(2004) , 10.1021/MA030465K
G. De Paëpe, N. Giraud, A. Lesage, P. Hodgkinson, A. Böckmann, L. Emsley, Transverse Dephasing Optimized Solid-State NMR Spectroscopy Journal of the American Chemical Society. ,vol. 125, pp. 13938- 13939 ,(2003) , 10.1021/JA037213J
Hiroyuki Kono, Yukari Numata, Tomoki Erata, Mitsuo Takai, Structural analysis of cellulose triacetate polymorphs by two-dimensional solid-state 13C–13C and 1H–13C correlation NMR spectroscopies Polymer. ,vol. 45, pp. 2843- 2852 ,(2004) , 10.1016/J.POLYMER.2004.01.075
Gaël De Paëpe, Anne Lesage, Stefan Steuernagel, Lyndon Emsley, Transverse Dephasing Optimised NMR Spectroscopy in Solids: Natural-Abundance 13C Correlation Spectra ChemPhysChem. ,vol. 5, pp. 869- 875 ,(2004) , 10.1002/CPHC.200301062
Didier Y. GAGNAIRE, Francois R. TARAVEL, Biosynthèse de cellulose bactérienne à partir de D-glucose uniformément enrichi en 13C. FEBS Journal. ,vol. 103, pp. 133- 143 ,(1980) , 10.1111/J.1432-1033.1980.TB04297.X
Gaël De Paëpe, Anne Lesage, Lyndon Emsley, The performance of phase modulated heteronuclear dipolar decoupling schemes in fast magic-angle-spinning nuclear magnetic resonance experiments The Journal of Chemical Physics. ,vol. 119, pp. 4833- 4841 ,(2003) , 10.1063/1.1595088