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31P and 13C chemical shielding tensors in the phosphoenolpyruvate moiety from rotary resonance recoupling 13C and 31P MAS and single crystal 31P NMR.

MPG-Autoren
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Haeberlen,  Ulrich
Research Group Prof. Dr. Haeberlen, Max Planck Institute for Medical Research, Max Planck Society;

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Stumber,  Michael
Research Group Prof. Dr. Haeberlen, Max Planck Institute for Medical Research, Max Planck Society;

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Zitation

Bechmann, M., Dusold, S., Förster, H., Haeberlen, U., Lis, T., Sebald, A., et al. (2000). 31P and 13C chemical shielding tensors in the phosphoenolpyruvate moiety from rotary resonance recoupling 13C and 31P MAS and single crystal 31P NMR. Molecular Physics, 98(9), 605-617. doi:10.1080/00268970009483327.


Zitierlink: https://hdl.handle.net/11858/00-001M-0000-0028-3556-5
Zusammenfassung
A 31P and 13C NMR study of powder and single crystal samples of two phosphoenolpyruvate (PEP) compounds, the tris-ammonium salt monohydrate (NH4)3(PEP)·H2O (1), and the mono-ammonium-salt (NH4)(H2PEP) (2) is presented. The P chemical shielding tensors in 1 are measured by 31P single crystal NMR on four minuscule samples and assigned without ambiguity by exploiting the orientation-dependent 31P-31p dipolar splittings of the resonance lines. The orientation of the 31P chemical shielding tensor is discussed in terms of the C2v — and C3-type distortions of the phosphate PO4-coordination sphere. From 13C MAS NMR experiments with 31P rotary resonance recoupling on polycrystalline powder samples the orientations of the 31P chemical shielding tensors in 1 and 2 are obtained, for 1 in very good agreement with the 31P single crystal NMR results. Only some of the orientational parameters of the three 13C chemical shielding tensors in the PEP moiety of 1 could be derived from 13C MAS NMR experiments with 31P rotary resonance recoupling.