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NMR crystallography of campho[2,3-c]pyrazole (Z '=6): combining high-resolution H-1-13-C solid-state MAS NMR spectroscopy and GIPAW chemical-shift calculations
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Webber, Amy L., Emsley, Lyndon, Claramunt, Rosa M. and Brown, Steven P. (2010) NMR crystallography of campho[2,3-c]pyrazole (Z '=6): combining high-resolution H-1-13-C solid-state MAS NMR spectroscopy and GIPAW chemical-shift calculations. Journal of Physical Chemistry A, Vol.114 (No.38). pp. 10435-10442. doi:10.1021/jp104901j ISSN 1089-5639.
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Official URL: http://dx.doi.org/10.1021/jp104901j
Abstract
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.
| Item Type: | Journal Article | ||||
|---|---|---|---|---|---|
| Subjects: | Q Science > QD Chemistry Q Science > QC Physics |
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| Divisions: | Faculty of Science, Engineering and Medicine > Science > Physics | ||||
| Journal or Publication Title: | Journal of Physical Chemistry A | ||||
| Publisher: | American Chemical Society | ||||
| ISSN: | 1089-5639 | ||||
| Official Date: | 30 September 2010 | ||||
| Dates: |
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| Volume: | Vol.114 | ||||
| Number: | No.38 | ||||
| Number of Pages: | 8 | ||||
| Page Range: | pp. 10435-10442 | ||||
| DOI: | 10.1021/jp104901j | ||||
| Status: | Peer Reviewed | ||||
| Publication Status: | Published | ||||
| Access rights to Published version: | Restricted or Subscription Access | ||||
| Funder: | Engineering and Physical Sciences Research Council (EPSRC), MEC (Spain) | ||||
| Grant number: | CTQ2007-62113 |
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