NMR interaction tensors of 51V and 207Pb in vanadinite, Pb5(VO4)3Cl, determined from DFT calculations and single-crystal NMR measurements, using only one general rotation axis

Zeman, Otto E. O.; Hoch, Constantin; Hochleitner, Rupert; Bräuniger, Thomas

doi:10.1016/j.ssnmr.2017.12.002

Cited by 9 publications

(17 citation statements)

References 43 publications

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“…As for problem (i), the amount of necessary work could be greatly reduced by exploiting internal crystal symmetries, i.e., considering the NMR resonances of symmetry-related atoms in the unit cell as an additional dataset acquired for an independent but virtual rotation axis [12][13][14]. The same concept can be used to address problem (ii) by calculating the exact orientation of the rotation axis from NMR data alone [15][16][17]. Regarding problem (iii), many systems are amenable to crystal growth by methods available in a standard laboratory.…”

Section: Introductionmentioning

confidence: 99%

“…Regarding problem (iii), many systems are amenable to crystal growth by methods available in a standard laboratory. In addition, natural minerals offer a great supply of single crystalline material already prepared by nature, often of sufficient size for NMR investigations [16][17][18][19]. To illustrate how to tackle the above listed problems (i)-(iii), here we present the determination of the full 207 Pb chemical shift tensor of anglesite, PbSO 4 , using a single crystal from a natural mineral deposit, as pictured in Figure 1a.…”

Section: Introductionmentioning

confidence: 99%

“…(iii), many systems are amenable to crystal growth by methods available in a standard laboratory. 51 In addition, natural minerals offer a great supply of single crystalline material already prepared by 52 nature, often of sufficient size for NMR investigations [14][15][16][17]. As a case study to illustrate points , and are co-ordinated by the ten nearest oxygen atoms (red).…”

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confidence: 99%

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Determination of the Full 207Pb Chemical Shift Tensor of Anglesite, PbSO4, and Correlation of the Isotropic Shift to Lead–Oxygen Distance in Natural Minerals

et al. 2019

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The full 207 Pb chemical shift (CS) tensor of lead in the mineral anglesite, PbSO 4 , was determined from orientation-dependent nuclear magnetic resonance (NMR) spectra of a large natural single crystal, using a global fit over two rotation patterns. The resulting tensor is characterised by the reduced anisotropy Δ δ = ( - 327 ± 4 ) ppm, asymmetry η C S = 0 . 529 ± 0 . 002 , and δ i s o = ( - 3615 ± 3 ) ppm, with the isotropic chemical shift δ i s o also verified by magic-angle spinning NMR on a polycrystalline sample. The initially unknown orientation of the mounted single crystal was included in the global data fit as well, thus obtaining it from NMR data only. By use of internal crystal symmetries, the amount of data acquisition and processing for determination of the CS tensor and crystal orientation was reduced. Furthermore, a linear correlation between the 207 Pb isotropic chemical shift and the shortest Pb–O distance in the co-ordination sphere of Pb 2 + solely surrounded by oxygen has been established for a large database of lead-bearing natural minerals.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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confidence: 99%

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Determination of the Full 207Pb Chemical Shift Tensor of Anglesite, PbSO4, and Correlation of the Isotropic Shift to Lead–Oxygen Distance in Natural Minerals

et al. 2019

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“…For 7 Li with spin I = 3/2, the quadrupolar coupling between the non-symmetric charge distribution of the nucleus and its electronic surroundings also needs to be considered [20]. The number of energy levels for a spin I in an external magnetic field is 2I + 1, resulting in 2I NMR transitions, which are classified according to their magnetic quantum number m. With a particular transition |m → |m + 1 designated by the parameter k = m + 1 2 [21,22], the resonance frequency ν m,m+1 of this transition may then be described by adding the contribution of the quadrupolar interaction to Equation (1):…”

Section: LI Nmr Of Ldpmentioning

confidence: 99%

“…Obviously, the effects of the quadrupolar interaction to second order for 7 Li in LDP are negligibly small, especially taking into account the very broad resonance lines. Accordingly, it should now be possible to determine its chemical shift tensor by tracing the variation of the center of the satellite transitions without correcting for second order effects [21]. However, the chemical shift anisotropy of lithium atoms is generally very small (in the range of 5 ppm [2]), making detection of anisotropic effects from resonance lines with a f whm ≈ 28 ppm practically impossible.…”

Section: LI Nmr Of Ldpmentioning

confidence: 99%

Single-Crystal 31P and 7Li NMR of the Ionic Conductor LiH2PO4

Zeman

Kainz²,

Bräuniger

2020

Crystals

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The electronic surroundings of phosphorus and lithium atoms in the ionic conductor lithium dihydrogen phosphate (LDP) have been studied by single-crystal nuclear magnetic resonance (NMR) spectroscopy at room temperature. From orientation-dependent NMR spectra of a large homegrown LDP single crystal, the full 31 P chemical shift (CS) and 7 Li quadrupole coupling (QC) tensor was determined, using a global fit over three rotation patterns. The resulting CS tensor is characterized by its three eigenvalues: δ PAS 11 = (67.0 ± 0.6) ppm, δ PAS 22 = (13.9 ± 1.5) ppm, and δ PAS 33 = (−78.7 ± 0.9) ppm. All eigenvalues have also been verified by magic-angle spinning NMR on a polycrystalline sample, using Herzfeld-Berger analysis of the rotational side band pattern. The resulting 7 Li QC tensor is characterized by its quadrupolar coupling constant χ = Q PAS 33 = (−71 ± 1) kHz and the two eigenvalues Q PAS 11 = (22.3 ± 0.9) kHz, and Q PAS 22 = (48.4 ± 0.8) kHz. The initially unknown orientation of the mounted crystal, expressed by the orientation of the rotation axis in the orthorhombic crystal frame, was included in the global data fit as well, thus obtaining it from NMR data only.Crystals 2020, 10, 302 2 of 12 with four formula units per unit cell [6]. The PO 4 tetrahedra build a three-dimensional framework connected by two different types of hydrogen bonds. The LiO 4 coordination tetrahedra are linked by their vertices forming [100] isolated chains and share each edge with the PO 4 units. All atoms in the unit cell are located at Wyckoff position 4a with the general site symmetry 1 − C 1 [7]. As a result, no symmetry constraints affect the algebraic form of the NMR interaction tensors, as will be explained in the following.Abstract: Last thing to be done...

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

et al. 2021

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Cerussite, $$\hbox {PbCO}_3$$ 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.

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NMR interaction tensors of 51V and 207Pb in vanadinite, Pb5(VO4)3Cl, determined from DFT calculations and single-crystal NMR measurements, using only one general rotation axis

Cited by 9 publications

References 43 publications

Determination of the Full 207Pb Chemical Shift Tensor of Anglesite, PbSO4, and Correlation of the Isotropic Shift to Lead–Oxygen Distance in Natural Minerals

Determination of the Full 207Pb Chemical Shift Tensor of Anglesite, PbSO4, and Correlation of the Isotropic Shift to Lead–Oxygen Distance in Natural Minerals

Single-Crystal 31P and 7Li NMR of the Ionic Conductor LiH2PO4

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

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