Correlated nmr spectroscopy

M Lui, JK Nicholson, JA Parkinson, JC Lindon. Measurement of bimolecular diffusion coefficients in blood plasma using two-dimensional 1II-1 II diffusion-edited total-correlation NMR spectroscopy. Anal Chem 69 1504-1509, 1997. 

Zheng et al. [1] postulated that the driving force for placing Zr and B on the same carbon might stem from interactions between the zirconium and oxygen or boron and chlorine atoms. However, an X-ray analysis of 22 revealed that there are no intra- or intermo-lecular interactions between any of these atoms [35]. Compound 22 was also unambiguously characterized by 1H-1H double quantum filtered COSY [36] and 13C-1H heteronuc-lear chemical shift correlation NMR spectroscopy [37,38]. Considerable differences in the chemical shifts of the diastereotopic Cp groups were found in both the XH and 13C NMR spectra. The NMR study unequivocally showed that the methine proton was at-... 

Additional information on molecular conformation can be obtained by NOE, transfer NOE or 2-D homonuclear correlated NMR spectroscopy (COSY), which is used to measure the distance between nuclei. For detailed information on the various techniques see refs. 86 and 87. 

In a model reaction used to support the structure identification of a neutral polyaza cleft for enolate complexations, the disubstituted dihydropyrrolo[2,3-/i]quinoline (51) was prepared by alkylation of 7-bromo-5,6,7,8-tetrahydro-8-quinolone with ethyl 3,3-diamino-2-propenoate (Equation (24)) <91JA9687>. The regioisomeric residence of the two substituents in this product was supported by 13C—13C shift-correlated NMR spectroscopy. 

Gougeon, R.D., Reinholdt, M., Delmotte, L., Miehe-Brendle, J., Chezeau, J.M., Le Dred, R., Marchal, R., Jeandet, P. (2002). Direct observation of polylysine side-chain interaction with smectites interlayer surfaces through H- Al heteronuclear correlation NMR spectroscopy, Langmuir, 18, 3396-3398. 

Gougeon, R.D., Reinholdt, M., Delmotte, L., Miehe-Brendle, J., Chezeau, J.M., Le Dred, R., Mar-chal, R., Jeandet, P. (2002). Direct observation of polylysine side-chain interaction with smectites interlayer surfaces through H- A1 heteronuclear correlation NMR spectroscopy. Langmuir, the American Chemical Society Journal of Surfaces and Colloids, 18, 3396-3398 Gougeon, R.D., Soulard, M., Reinholdt, M., Miehe-Brendle, J., Chezeau, J.M., Le Dred, R., Mar-chal, R., Jeandet, P. (2003). Polypeptide adsorption onto a synthetic montmoriUonite A combined solid-state NMR, X-ray diffraction, thermal analysis and N2 adsorption study. Eur. J. Inorg. Chem., 2003, 1366-1372... 

A. Bax and S. Subramanian, Sensitivity-enhanced two-dimensional heteronuclear shift correlation NMR spectroscopy, /. Magn. Reson. 67 (1986), 565-569. 

Figure 26. Experimental scheme of two-dimensional NMR spectroscopy, (a) The general scheme of two-dimensional spectroscopy. Here, t, and become two variables of two-dimensional response signals. H and are the Hamiltonians during t, and tj periods,

Ede, R. M., and Brunow, G. (1992) Application of two-dimensional homo- and hetero-nuclear correlation NMR spectroscopy to wood lignin structure determination. J. Org. Chem. 57(5), 1477-1480. 

Palmer, A. G., Cavanagh, 1., Wright, P. E., and Ranee, M. (1991) Sensitivity improvement in proton-detected two-dimensional heteronnelear correlation NMR spectroscopy. J. Magn. Reson. Ser. A 93, 151-170. 

In order to further characterize the key role of the 4 -amino group of ThDP for cofactor activation, the influence of the chemical environment at the active site of pyruvate decarboxylase from Zymomonas mobilis on the electronic properties of the 4 -amino group was studied by two-dimensional proton-nitrogen correlated NMR spectroscopy (Tittmann et al., 2005a). Chemical shift analysis and its pH dependence indicate that the acceleration of C2 deprotonation by 5 orders of magnitude is not mainly of thermodynamic nature caused by a significant increase in basicity... 

In this chapter, using ipsenol and caryophyllene oxide as examples, we turn our attention to correlation NMR spectroscopy most of the useful experiments fall into the category of two-dimensional (2-D) NMR. (The exception is the HOHAHA experiment, a special type of one-dimensional, or 1-D, experiment that has a 2-D analogue.) Other examples will be used to illustrate specific points or types of spectra. 

Bax A, Davis DG (1985) MLEV-17 Based two-dimensional homonuclear magnetization transfer spectroscopy. J Magn Reson 65 355-360 Bax A, Drobny G (1985) Optimization of two-dimensional homonuclear relayed coherence transfer NMR spectroscopy. J Magn Reson 61 306-320 Bax A, Marion D (1988) Improved resolution and sensitivity in H-detected heteronuclear multiple-bond correlation spectroscopy. J Magn Reson 78 186-191 Bax A, Subramanian S (1986) Sensitivity-enhanced two-dimensional heteronuclear chemical shift correlation NMR spectroscopy. J Magn Reson 67 565-569 Bax A, Summers MF (1986) and Assignments from sensitivity-enhanced detection of heteronuclear multiple bond connectivity by 2D multiple-quantum NMR. J Am Chem Soc 108 2093-2094... 

K. Mao, W. Wiench, V.S.Y. Lin, M. Pruski, Indirectly detected through-bond chemical shift correlation NMR spectroscopy in sohds under fast MAS studies of organic-inorganic hybrid materials, J. Magn. Reson. 196 (2009) 92—95. 

Y. Nishiyama, M. Malon, Z. Gan, Y. Endo, T. Nemoto, Proton—nitrogen-14 overtone two-dimensional correlation NMR spectroscopy of solid-sample at very st magic angle sample spinning, J. Magn. Reson. 230 (2013) 160—164. 

G.M. Kirwan, MJ. Adams, Peak width issues with generalised 2D correlation NMR spectroscopy, J. Mol. Struct. 892 (2008) 225. 

M. Coen, Y.-S. Hong, O. Qoarec, C.M. Rhode, M.D. Reily, D.G. Robertson, et al., Heteronuclear H— P statistical total correlation NMR spectroscopy of intact liver for metabolic biomarker assignment application to galactosamine-induced hepatotoxic-ity. Anal. Chem. 79 (2007) 8956. 

C.H. Johnson, T.J. Athersuch, I.D. Wilson, L. Iddon, X. Meng, A.V. Stachulski, et aL, Kinetic and J-resolved statistical total correlation NMR spectroscopy approaches to structural information recovery in complex reacting mixtures apphcation to acyl gju-curonide intramolecular transacylation reactions. Anal. Chem. 80 (2008) 4886. 

G.P. Holland, B.R. Cherry, J.E. Jenkins, J.L. Yarger, Proton-detected heteronuclear single quantum correlation NMR spectroscopy in rigid solids with ultra- st MAS, J. Magn. Reson. 202 (2010) 64-71. 

J.W. Wiench, C.E. Bronnimann, V.S.Y. Lin, M. Pmski, Chemical shift correlation NMR spectroscopy with indirect detection in fast rotating solids studies of organically functionalized mesoporous sihcas, J. Am. Chem. Soc. 129 (2007) 12076—12077. 

Trebosc, J., Wiench, J.W., Huh, S., Lin, V.S.Y, and Pruski, M. 2005b. Studies of organically functionalized mesoporous silicas using heteronuclear solid-state correlation NMR spectroscopy under fast magic angle spinning. J.Am. Chem. Soc. 127 7587-7593. 

Kotyk, J. J. Berger, P. A. Remsen, E. E. Microstructuralcharacterization of poly(methyl methacrylate) using proton-detected heteronuclear shift-correlated NMR spectroscopy. Macromolecules 1990, 23, 5167-5169. 

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