Rapid Analysis of Organic Compounds by Proton‐Detected Heteronuclear Correlation NMR Spectroscopy with 40 kHz Magic‐Angle Spinning

Zhou, Donghua H.; Rienstra, Chad M.

doi:10.1002/ange.200802108

Cited by 26 publications

(76 citation statements)

References 30 publications

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“…Black and gray lines respectively identify the experimental spectra and the spectra simulated using Equations (1) and (9) and following the assignments of refs. [6] (left) and [16] (right). energy for the isobutyl methyl groups.…”

Section: Fast Motion Regimementioning

confidence: 97%

“…Line broadening effects due to the exchange phenomenon, visible in the 13 C CP-MAS spectra at temperatures higher than 10 8C, were simulated using Equations (1) and (9). Since two different assignments of the peaks to tertiary aromatic carbon atoms have been reported in the literature, [6,16] the simulation was performed for both the assignments. The best simulations were obtained with E a = 24.5 kJ mol À1 and t 1 = 6.3 10 À7 s, and with E a = 24.8 kJ mol…”

Section: Slow Motion Regimementioning

confidence: 99%

“…Experimental and simulated spectra for both the assignments are reported in Figure 4. It is worth noticing that the correlation time for this motion, calculated at 11 8C, is about 20 ms, in full agreement with the previous estimate based on 13 C-1 H heteronuclear correlation spectroscopy (HETCOR) experiments, thus limiting this value in the range 1-270 ms. [16] …”

mentioning

confidence: 97%

“…[6] and [16], respectively. Both the simulations satisfactorily reproduce the experimental spectra with very similar motional parameters, even though a slightly better reproduction of the experimental data was obtained using the assignment of ref.…”

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confidence: 98%

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Detailed Characterization of the Dynamics of Ibuprofen in the Solid State by a Multi‐Technique NMR Approach

2011

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The internal rotations and interconformational jumps of ibuprofen in the solid state are fully characterized by the simultaneous analysis of a variety of low- and high-resolution NMR experiments for the measurement of several (13)C and (1)H spectral and relaxation properties, performed at different temperatures and, in some cases, frequencies. The results are first qualitatively analyzed to identify the motions of the different molecular fragments and to assign them to specific frequency ranges (slow, <10(3) Hz; intermediate, 10(3)-10(6) Hz; and fast, >10(6) Hz). In a second step, a simultaneous fit of the experimental data sets most sensitive to each frequency range is performed by means of suitable motional models to obtain, for each motion, values of correlation times and activation energies. The rotations of the three methyl groups around their ternary symmetry axes, which occur in the fast regime, are characterized by slightly different activation energies. Thanks to the simultaneous analysis of (1)H and (13)C data, the π-flip of the dimeric structure made by the acidic groups is also identified and seen to occur in the fast regime. On the contrary, the π-flip of the phenyl ring is found to occur in the slow motional regime, while the rotations of the isobutyl and propionic groups are frozen. The approach used appears to be of general applicability for studying the dynamics of small organic molecules.

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Section: Fast Motion Regimementioning

confidence: 97%

Section: Slow Motion Regimementioning

confidence: 99%

mentioning

confidence: 97%

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confidence: 98%

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Detailed Characterization of the Dynamics of Ibuprofen in the Solid State by a Multi‐Technique NMR Approach

2011

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“…Most importantly, it helps to reduce or, in some cases, eliminate the strong homonuclear dipolar couplings between high-c nuclei ( 1 H and 19 F). Indeed, fast MAS by itself enabled the acquisition of directly detected (also referred to as X-detected or X{ 1 H}) and indirectly detected ( 1 H-detected or 1 H{X}) multi-dimensional heteronuclear correlation (HETCOR) NMR spectra of organic materials in which 1 H spin systems were isotopically diluted, exhibited some degree of motional narrowing, or were fully coupled [4,[6][7][8][9][10]. In our studies, MAS at 40 kHz was used to achieve high 1 H resolution in mesoporous organic-inorganic hybrid materials [4].…”

Section: Introductionmentioning

confidence: 99%

Directly and indirectly detected through-bond heteronuclear correlation solid-state NMR spectroscopy under fast MAS

Mao

Pruski

2009

Journal of Magnetic Resonance

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Proton‐Detected Solid‐State NMR Spectroscopy of Natural‐Abundance Peptide and Protein Pharmaceuticals

et al. 2009

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Keine Anreicherung nötig: Eine empfindliche NMR‐Spektroskopiemethode wurde entwickelt, die gut aufgelöste 2D‐Spektren (15N‐1H und 13C‐1H) von großen Molekülen (wie Biopharmazeutika) liefert, ohne dass eine Isotopenanreicherung erforderlich ist. Diese Methode gab Einblicke in die Strukturen zweier lyophilisierter Aprotininproben sowie dreier Insulinproben in lyophilisierter, mikrokristalliner Suspension (rot; siehe Bild) und Fibrillenformen (grün).

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Rapid Analysis of Organic Compounds by Proton‐Detected Heteronuclear Correlation NMR Spectroscopy with 40 kHz Magic‐Angle Spinning

Cited by 26 publications

References 30 publications

Detailed Characterization of the Dynamics of Ibuprofen in the Solid State by a Multi‐Technique NMR Approach

Detailed Characterization of the Dynamics of Ibuprofen in the Solid State by a Multi‐Technique NMR Approach

Directly and indirectly detected through-bond heteronuclear correlation solid-state NMR spectroscopy under fast MAS

Proton‐Detected Solid‐State NMR Spectroscopy of Natural‐Abundance Peptide and Protein Pharmaceuticals

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