Magnitudes and relative orientation of vanadium-51 quadrupole coupling and anisotropic shielding tensors in metavanadates and potassium vanadium oxide (KV3O8) from vanadium-51 MAS NMR spectra. Sodium-23 quadrupole coupling parameters for .alpha.- and .beta.-NaVO3

Skibsted, Joergen; Nielsen, Niels Chr.; Bildsøe, Henrik; Jakobsen, Hans J.

doi:10.1021/ja00069a038

Cited by 105 publications

(156 citation statements)

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“…The MAS spectra are observed to break up into spinning sidebands (ssbs) and the absence of significant quadrupolar secondorder shifts indicates that the quadrupole coupling constant Q CC D e 2 qQ/h is moderate (jQ CC j < 3 MHz). 1,2,22,23 Indeed, the good agreement between the experimental and calculated data (Figs 1 and 2) demonstrates that the complete manifolds of ssbs from all seven 51 V transitions are detected. For simplicity, in Figs 1 and 2, the isotropic peak, determined from spectra employing different spinning speeds, was arbitrarily chosen as the chemical shift reference.…”

Section: Resultssupporting

confidence: 57%

⁵¹V magic angle spinning NMR in VOPO₄ phases

Siegel

Dupré

Quarton

et al. 2004

Magnetic Reson in Chemistry

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51V magic angle spinning NMR was applied to the alpha(II), beta and gamma phases of VOPO4 at three magnetic field strengths (4.7, 7.1, and 11.7 T). The 51V quadrupole and chemical shift tensors were determined by iterative fitting of the NMR lineshapes at the three magnetic field strengths. The applicability of the method is illustrated by comparison with literature data. Although determined chemical shift tensors are completely axially symmetric and of the same magnitude, all studied phases can clearly be distinguished by their quadrupole coupling tensor. Relationships between the 51V NMR data and structural characteristics such as crystal symmetries are discussed.

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Section: Resultssupporting

confidence: 57%

⁵¹V magic angle spinning NMR in VOPO₄ phases

Siegel

Dupré

Quarton

et al. 2004

Magnetic Reson in Chemistry

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“…Spectra were simulated by using the STARS program, integrated within VnmrJ (Varian Inc.). [44] Quantum chemical calculations: Density functional theory (DFT) calculations were performed on representative clusters (taken from X-ray diffraction data) of all compounds (1-6) by using the Amsterdam Density Functional (ADF) package (version ADF 2008.01). [45][46][47] Relativistic effects were accounted for by using the zeroth-order relativistic approximation (ZORA) method including spin-orbit coupling.…”

Section: Methodsmentioning

confidence: 99%

Characterising Lone‐Pair Activity of Lead(II) by ²⁰⁷Pb Solid‐State NMR Spectroscopy: Coordination Polymers of [N(CN)₂]⁻ and [Au(CN)₂]⁻ with Terpyridine Ancillary Ligands

Greer

Michaelis

Katz

et al. 2011

Chemistry A European J

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A series of lead(II) coordination polymers containing [N(CN)(2)](-) (DCA) or [Au(CN)(2)](-) bridging ligands and substituted terpyridine (terpy) ancillary ligands ([Pb(DCA)(2)] (1), [Pb(terpy)(DCA)(2)] (2), [Pb(terpy){Au(CN)(2)}(2)] (3), [Pb(4'-chloro-terpy){Au(CN)(2)}(2)] (4) and [Pb(4'-bromo-terpy)(μ-OH(2))(0.5){Au(CN)(2)}(2)] (5)) was spectroscopically examined by solid-state (207)Pb MAS NMR spectroscopy in order to characterise the structural and electronic changes associated with lead(II) lone-pair activity. Two new compounds, 2 and [Pb(4'-hydroxy-terpy){Au(CN)(2)}(2)] (6), were prepared and structurally characterised. The series displays contrasting coordination environments, bridging ligands with differing basicities and structural and electronic effects that occur with various substitutions on the terpyridine ligand (for the [Au(CN)(2)](-) polymers). (207)Pb NMR spectra show an increase in both isotropic chemical shift and span (Ω) with increasing ligand basicity (from δ(iso) = -3090 ppm and Ω = 389 ppm for 1 (the least basic) to δ(iso) = -1553 ppm and Ω = 2238 ppm for 3 (the most basic)). The trends observed in (207)Pb NMR data correlate with the coordination sphere anisotropy through comparison and quantification of the Pb-N bond lengths about the lead centre. Density functional theory calculations confirm that the more basic ligands result in greater p-orbital character and show a strong correlation to the (207)Pb NMR chemical shift parameters. Preliminary trends suggest that (207)Pb NMR chemical shift anisotropy relates to the measured birefringence, given the established correlations with structure and lone-pair activity.

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“…These quadrupole parameters indicated (1) that Na 2 O increased the electric field gradients at the boron sites of the BO3 structures but reduced the distortion of the gradients and (2) that V 2 O 5 had the opposite effect on the electric field gradients. To remove the overlap of the spinning side bands with any center peaks, spinning rates higher than 29 kHz were required at 9.4 T. Four different center peaks, assigned to VO 6 , VO 5 , and VO 4 structures that were all bonded to neighboring vanadiums and to VO 4 structure with at least one oxygen bonded to boron instead of vanadium, 13,18,19 were obtained from the spectral simulation of the spectra, as shown in Figures 6 and 7. The peaks at -587 ~ -622 ppm were assigned to VO 5 structures as in V 2 O 5 , 14,15,20 those at -564 ~ -618 ppm to VO 4 structures, 15,21,22 those at -520 ~ -536 ppm to VO6, 21,22 and those at -640 ~ -675 ppm to VO4 structures with at least one oxygen bonded to boron instead of vanadium.…”

Section: Resultsmentioning

confidence: 99%

Solid state MAS NMR Investigation on the Local Structures of_xV₂O₅-B₂O₃-_yNa₂O Glasses

Kim¹,

Han

Kang³

et al. 2009

Bulletin of the Korean Chemical Society

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The local structures of the boron and vanadium sites in the ternary glass xV2O5-B2O3-yNa2O were studied by 11 B and 51 V magic angle spinning (MAS) nuclear magnetic resonance (NMR). With increasing x, the mole ratios of the BO3 and BO4 structures were enhanced, as were the quadrupole asymmetry parameters for the BO3 structures, while the quadrupole coupling constants for the sites were reduced. However, the opposite trends were observed with increasing y, implying that V2O5 and Na2O play opposite roles. The VO4, VO5 and VO6 structures with all oxygens bonded to the vanadium neighbors were identified. Vanadiums bonded to the greater number of oxygens were more populated at higher contents of Na2O and V2O5. In addition, the VO4 structures with at least one oxygen bonded to boron instead of vanadium were detected at low Na2O contents. The electron densities of various vanadium oxide structures were affected by the weight densities and vanadium ion densities. The VO4 structures were more likely to be vanadium oxide structures right next to V 4+ ions.

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Magnitudes and relative orientation of vanadium-51 quadrupole coupling and anisotropic shielding tensors in metavanadates and potassium vanadium oxide (KV3O8) from vanadium-51 MAS NMR spectra. Sodium-23 quadrupole coupling parameters for .alpha.- and .beta.-NaVO3

Cited by 105 publications

References 0 publications

⁵¹V magic angle spinning NMR in VOPO₄ phases

⁵¹V magic angle spinning NMR in VOPO₄ phases

Characterising Lone‐Pair Activity of Lead(II) by ²⁰⁷Pb Solid‐State NMR Spectroscopy: Coordination Polymers of [N(CN)₂]⁻ and [Au(CN)₂]⁻ with Terpyridine Ancillary Ligands

Solid state MAS NMR Investigation on the Local Structures of_xV₂O₅-B₂O₃-_yNa₂O Glasses

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Magnitudes and relative orientation of vanadium-51 quadrupole coupling and anisotropic shielding tensors in metavanadates and potassium vanadium oxide (KV3O8) from vanadium-51 MAS NMR spectra. Sodium-23 quadrupole coupling parameters for .alpha.- and .beta.-NaVO3

Cited by 105 publications

References 0 publications

51V magic angle spinning NMR in VOPO4 phases

51V magic angle spinning NMR in VOPO4 phases

Characterising Lone‐Pair Activity of Lead(II) by 207Pb Solid‐State NMR Spectroscopy: Coordination Polymers of [N(CN)2]− and [Au(CN)2]− with Terpyridine Ancillary Ligands

Solid state MAS NMR Investigation on the Local Structures ofxV2O5-B2O3-yNa2O Glasses

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⁵¹V magic angle spinning NMR in VOPO₄ phases

⁵¹V magic angle spinning NMR in VOPO₄ phases

Characterising Lone‐Pair Activity of Lead(II) by ²⁰⁷Pb Solid‐State NMR Spectroscopy: Coordination Polymers of [N(CN)₂]⁻ and [Au(CN)₂]⁻ with Terpyridine Ancillary Ligands

Solid state MAS NMR Investigation on the Local Structures of_xV₂O₅-B₂O₃-_yNa₂O Glasses