Spectral distortion effects due to finite pulse widths in deuterium nuclear magnetic resonance spectroscopy

Bloom, Myer; Davis, James H.; Valic, M.I.

doi:10.1139/p80-196

Cited by 250 publications

(123 citation statements)

References 5 publications

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“…The program was run on the Dalhousie University VAX 8800 mainframe computer. With the exception of the T 1Z simulations, the simulated solid echo spectra were not corrected for finite pulse length distortions [27].…”

Section: Methodsmentioning

confidence: 99%

“…The relaxation times were obtained at the "0 = 90°" and 9 = 0° orientations in the powder patterns. Due to insufficient excitation, resulting from the finite length of the applied pulses [23,27], and the applied line broadening of 0.5 kHz, the edges of the spectra were not always accurately defined. This prompted us to measure the relaxation times in a window of 9 = 0°-5°, an approximation which is adequate for our purposes.…”

Section: Ii) Reorientational Dynamics Of the -Nd 3 Group Obtained Fromentioning

confidence: 99%

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Molecular Motion in Phenpropylammonium Chloride Studied by Deuterium NMR

Gruwel

Wasylishen

1992

Zeitschrift Für Naturforschung A

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Cation dynamics in phenpropylammonium chloride, C 6 H 5 (CH 2 ) 3 NH 3 Cr, were studied in three different solid phases by means of 2 H nmr. Both 2 H nmr line shapes and spin-lattice relaxation studies were performed on the ammonium head group, the adjacent methylene group and the phenyl-ring. In the low temperature phase, solid III, the -ND 3 group dynamics were dominated by C 3 jumps about the C-N axis. From the observed minima in T 1Z and T 1Q a quadrupole coupling constant of 165 ± 5 kHz was obtained. The 2 H nmr line shapes of the methylene group indicate that this group does not execute any large amplitude motion in the low temperature phase. In contrast, the phenyl ring deuterium nuclei give rise to line shapes characteristic of C 2 ring flips about the Cpara~C ipso aX * S "In the solid II phase the 2 H nmr line shapes of both the -ND ? and -CD 2 -groups are characterized by asymmetric Pake powder patterns. Since one of the principal components of the electric field gradient tensor remains temperature independent for both groups, it was concluded that these groups perform planar large-amplitude motions between two sites.Axially symmetric spectra were obtained for all three groups in the high temperature phase, solid I. The 2 H nmr line shapes indicate the presence of whole ion reorientation about a molecular axis. In addition, the -ND 3 groups perform C 3 jumps about the C-N axis and the -C 6 D 5 group display line shapes characteristic for rotational diffusion about the C para -C ipso axis.

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Section: Methodsmentioning

confidence: 99%

Section: Ii) Reorientational Dynamics Of the -Nd 3 Group Obtained Fromentioning

confidence: 99%

Molecular Motion in Phenpropylammonium Chloride Studied by Deuterium NMR

Gruwel

Wasylishen

1992

Zeitschrift Für Naturforschung A

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“…300 (1)(2)(3)(4). These studies also have provided strong evidence that the amino acid side chains exhibit extensive internal motions in the fibrils (3,5 (9) that accounts for spectral distortion due to a finite pulse width. Lorentzian line broadening was used.…”

mentioning

confidence: 89%

Characterization of leucine side-chain reorientation in collagen-fibrils by solid-state 2H NMR.

Batchelder¹,

Sullivan²,

Jelinski³

et al. 1982

Proc. Natl. Acad. Sci. U.S.A.

109

135

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We have used 2H quadrupole-echo NMR spectroscopy to study the molecular dynamics of the leucine side chain in collagen fibrils labeled with [2H10]leucine. X-ray crystallographic studies ofleucine and small leucyl-containing peptides and proteins [Benedetti, C. (1977) at 313 nm to establish purity. The percentage incorporation of deuterium (43%) was determined by chemical ionization gas chromatography/mass spectrometry of N-acetylmethyl ester derivatives of the hydrolyzed protein. Radiotracer (3H and 14C) analysis showed that leucine was the only amino acid labeled during biosynthesis.2H NMR spectra were observed for polycrystalline D,L-[2H10]leucine over the temperature range -45°C to + 100°C (Fig. 2). Because of the size ofthe methylene and methine deuteron quadrupolar splitting, Avq(120 kHz), only a part of the spectrum arising from these deuterons is shown. Rapid threefold rotation of the methyl groups in leucine averages Avq to 38 kHz at -45°C, and these six deuterons display the classic axially symmetric quadrupolar powder pattern. Over the temperature range studied, very little additional side chain motion

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“…power r.f. at the center of a doublet of frequencies š was calculated by Bloom et al: 27 F , seq D sin[2 r.f.…”

Section: Appendix B Influence Of the Finite Pulse Power On The Measumentioning

confidence: 99%

Single‐crystal ²H NMR of deuterated 1,10‐decanedicarboxylic acid included in hydrogenated urea channels

Odin

Garcia

2004

Magnetic Reson in Chemistry

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The intergrowth of 1,10-decanedicarboxylic acid and urea give infinite hydrogen-bonded chains of the guest included in the hexagonal urea host. A deuterium high-resolution solid-state NMR study of the selectively deuterated intergrowth compound 1,10-decanedicarboxylic acid/hydrogenated urea at variable temperature in the range 90 ≤ T ≤ 300 K was performed on a single crystal. The analysis of the second moment as a function of temperature is shown to be compatible with the known phase transition occurring near T c = 203 K. Moreover, the spectra indicate that the orientational disorder is strong, and is compared to an axial uniform disorder. For this purpose, the general equation for the second moment of a system with uniform two-dimensional axial orientational disorder is given, and a method to take into account the non-uniform excitation of the pulse sequence is proposed.

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Spectral distortion effects due to finite pulse widths in deuterium nuclear magnetic resonance spectroscopy

Cited by 250 publications

References 5 publications

Molecular Motion in Phenpropylammonium Chloride Studied by Deuterium NMR

Molecular Motion in Phenpropylammonium Chloride Studied by Deuterium NMR

Characterization of leucine side-chain reorientation in collagen-fibrils by solid-state 2H NMR.

Single‐crystal ²H NMR of deuterated 1,10‐decanedicarboxylic acid included in hydrogenated urea channels

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Spectral distortion effects due to finite pulse widths in deuterium nuclear magnetic resonance spectroscopy

Cited by 250 publications

References 5 publications

Molecular Motion in Phenpropylammonium Chloride Studied by Deuterium NMR

Molecular Motion in Phenpropylammonium Chloride Studied by Deuterium NMR

Characterization of leucine side-chain reorientation in collagen-fibrils by solid-state 2H NMR.

Single‐crystal 2H NMR of deuterated 1,10‐decanedicarboxylic acid included in hydrogenated urea channels

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Single‐crystal ²H NMR of deuterated 1,10‐decanedicarboxylic acid included in hydrogenated urea channels