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  4. NMR Crystallography of Campho[2,3-c]pyrazole (Z `=6): Combining High-Resolution H-1-C-13 Solid-State MAS NMR Spectroscopy and GIPAW Chemical-Shift Calculations
 
research article

NMR Crystallography of Campho[2,3-c]pyrazole (Z `=6): Combining High-Resolution H-1-C-13 Solid-State MAS NMR Spectroscopy and GIPAW Chemical-Shift Calculations

Webber, Amy L.
•
Emsley, Lyndon  
•
Claramunt, Rosa M.
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2010
The Journal of Physical Chemistry A

H-1-C-13 two-dimensional magic-angle spinning (MAS) solid-state NMR correlation spectra, recorded with the MAS-J-HMQC experiment, are presented for campho[2,3-c]pyrazole. For each C-13 moiety, there are six resonances associated with the six distinct molecules in the asymmetric unit cell (Z' = 6). The one-bond C-H correlations observed in the 2D H-1-C-13 MAS-J-HMQC spectra allow the experimental determination of the H-1 and C-13 chemical shifts associated with the separate CH, CH2, and CH3 groups. H-1 and C-13 chemical shifts calculated by using the GIPAW (Gauge Including Projector Augmented Waves) plane-wave pseudopotential approach are presented. Calculations for the whole unit cell (12 x 29 = 348 atoms, with geometry optimization of all atoms) allow the assignment of the experimental H-1 and C-13 chemical shifts to the six distinct molecules, The calculated chemical shifts for the full crystal structure are compared with those for isolated molecules as extracted from the geometry-optimized crystal structure. In this way, the effect of intermolecular interactions on the observed chemical shifts is quantified. In particular, the calculations are sufficiently precise to differentiate the small (<1 ppm) differences between the H-1 chemical shifts of the six resonances associated with each distinct CH or CH2 moiety.

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Type
research article
DOI
10.1021/jp104901j
Web of Science ID

WOS:000282018200012

Author(s)
Webber, Amy L.
Emsley, Lyndon  
Claramunt, Rosa M.
Brown, Steven P.
Date Issued

2010

Publisher

AMER CHEMICAL SOC

Published in
The Journal of Physical Chemistry A
Volume

114

Issue

38

Start page

10435

End page

10442

Editorial or Peer reviewed

REVIEWED

Written at

OTHER

EPFL units
LRM  
Available on Infoscience
January 8, 2015
Use this identifier to reference this record
https://infoscience.epfl.ch/handle/20.500.14299/110018
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