The129Xe Chemical Shift Tensor in a Silicalite Single Crystal from Hyperpolarized129Xe NMR Spectroscopy

2001 ◽  
Vol 123 (42) ◽  
pp. 10399-10400 ◽  
Author(s):  
Victor V. Terskikh ◽  
Igor L. Moudrakovski ◽  
Hongbin Du ◽  
Christopher I. Ratcliffe ◽  
John A. Ripmeester
Keyword(s):  
Nmr Spectroscopy ◽  
Chemical Shift ◽  
Single Crystal ◽  
Chemical Shift Tensor

scholarly journals Characterisation of contact twinning for cerussite, $$\hbox {PbCO}_3$$, by single-crystal NMR spectroscopy

2021 ◽  
Vol 48 (11) ◽  
Author(s):  
Otto E. O. Zeman ◽  
Jennifer Steinadler ◽  
Rupert Hochleitner ◽  
Thomas Bräuniger
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Chemical Shift ◽  
Single Crystal ◽  
Room Temperature ◽  
Relative Orientation ◽  
Chemical Shift Tensor ◽  
Global Fit

AbstractCerussite, $$\hbox {PbCO}_3$$ PbCO 3 , like all members of the aragonite group, shows a tendency to form twins, due to high pseudo-symmetry within the crystal structure. We here demonstrate that the twin law of a cerussite contact twin may be established using only $$^{207}$$ 207 Pb-NMR spectroscopy. This is achieved by a global fit of several sets of orientation-dependent spectra acquired from the twin specimen, allowing to determine the relative orientation of the twin domains. Also, the full $$^{207}$$ 207 Pb chemical shift tensor in cerussite at room temperature is determined from these data, with the eigenvalues being $$\delta _{11} = (-2315\pm 1)$$ δ 11 = ( - 2315 ± 1 )  ppm, $$\delta _{22} = (-2492 \pm 3)$$ δ 22 = ( - 2492 ± 3 )  ppm, and $$\delta _{33} = (-3071 \pm 3)$$ δ 33 = ( - 3071 ± 3 )  ppm.

Intermolecular Interactions of Xe Atoms Confined in One-dimensional Nanochannels of Tris(o-phenylenedioxy)cyclotriphosphazene as Studied by High-pressure 129Xe NMR

2003 ◽  
Vol 58 (12) ◽  
pp. 727-734 ◽  
Author(s):  
Hirokazu Kobayashi ◽  
Takahiro Ueda ◽  
Keisuke Miyakubo ◽  
Taro Eguchi
Keyword(s):  
High Pressure ◽  
Nmr Spectroscopy ◽  
Chemical Shift ◽  
Pressure Dependence ◽  
Average Distance ◽  
Chemical Shift Tensor ◽  
Axially Symmetric ◽  
One Dimensional ◽  
129Xe Nmr ◽  
The One

The pressure dependence of the 129Xe chemical shift tensor confined in the Tris(o-phenylenedioxy) cyclotriphosphazene (TPP) nanochannel was investigated by high-pressure 129Xe NMR spectroscopy. The observed 129Xe spectrum in the one-dimensional TPP nanochannel (0.45 nm in diameter) exhibits a powder pattern broadened by an axially symmetric chemical shift tensor. As the pressure increases from 0.02 to 7.0 MPa, a deshielding of 90 ppm is observed for the perpendicularcomponent of the chemical shift tensor δ⊥, whereas a deshielding of about 30 ppm is observed for the parallel one, δ‖. This suggests that the components of the chemical shift tensor, δ‖ and δ⊥, are mainly dominated by the Xe-wall and Xe-Xe interaction, respectively. Furthermore, the effect of helium, which is present along with xenon gas, on the 129Xe chemical shift is examined in detail. The average distance between the Xe atoms in the nanochannel is estimated to be 0.54 nm. This was found by using δ⊥ at the saturated pressure of xenon, and comparing the increment of the chemicalshift value in δ⊥ to that of a β -phenol/Xe compound.

scholarly journals The Chemical Shift of the 29Si Nuclear Magnetic Resonance in a Synthetic Single Crystal of Mg2SiO4

1985 ◽  
Vol 40 (2) ◽  
pp. 126-130 ◽  
Author(s):  
N. Weiden ◽  
H. Rager
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Chemical Shift ◽  
Single Crystal ◽  
Angular Dependence ◽  
Room Temperature ◽  
Bond Distance ◽  
Chemical Shift Tensor ◽  
The Individual ◽  
Nuclear Magnetic

The angular dependence of the chemical shift of the 29Si nuclear magnetic resonance has been measured in a synthetic single crystal of Mg2SiO4 (space group Pbnm, Z = 4). The measurements were performed at room temperature at a frequency of 39.758 MHz using the FT-NMR technique. The eigenvalues of the shift tensor with respect to 29Si in TMS are δx = - 38.8 ppm, δv = -55.3 ppm and δz = - 95.4 ppm, with the eigenvector y parallel to c and the eigenvector z forming an angle of 7.5° with a. The results show clearly the influence of the individual S i - O bonds on the chemical shift tensor. The chemical shift along the S i -O bond depends in good approximation exponentially on the S i - O bond distance.

Single Crystal Solid-State NMR of Magnetically Oriented Powder

2014 ◽  
Vol 70 (a1) ◽  
pp. C1086-C1086
Author(s):  
Ryosuke Kusumi ◽  
Fumiko Kimura ◽  
Tsunehisa Kimura
Keyword(s):  
Magnetic Field ◽  
Solid State ◽  
Chemical Shift ◽  
Single Crystal ◽  
Solid State Nmr ◽  
Chemical Shift Tensor ◽  
Magic Angle ◽  
Full Information ◽  
Crystal Rotation ◽  
Rotation Method

Solid-state NMR spectroscopy is one of the most widely used methods for investigating crystal structures, along with the X-ray and neutron diffraction methods. Solid-state NMR can provide structural information including isotropic chemical shift, dipolar and quadrupolar couplings, spin diffusion, and chemical shift tensor. Among these, the chemical shift tensor is of particular significance because the electronic environment around a nucleus is directly reflected on the chemical shift tensor. However, full information of the chemical shift tensor, including principal values and axes, is difficult to obtain experimentally because a large single crystal is required for the measurement. On the other hand, we have proposed the use of a magnetically oriented microcrystal array (MOMA) as an alternative to a single crystal.[1,2] A MOMA is a composite in which microcrystals are aligned three-dimensionally, prepared by using a time-dependent magnetic field. We recently demonstrated that the13C chemical shift tensors of L-alanine crystal can be completely determined by application of the standard procedure in the single-crystal rotation method to a MOMA of L-alanine microcrystals,[3] as shown in Figure 1. The L-alanine MOMA produces sharp resonance peaks without resolution enhancement by magic angle spinning (MAS). In addition, we observed that the positions of the13C resonance peaks vary systematically as a function of the angle ψ that is the sample-rotation angle about the axis inclined by the magic angle with respect to the NMR magnetic field. From the ψ-dependence of the chemical shifts,13C chemical shift tensor was completely determined. We confirmed that the combination of MOMA with the single-crystal rotation method can be applied to other nuclei such as31P and15N. These results clearly show that the MOMA method is a powerful tool for obtaining full information of the chemical shift tensor from a microcrystalline powder without MAS.

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