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Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
Published on: September 17, 2017
Effects of polymorphic differences for sulfanilamide, as seen through 13C and 15N solid-state NMR, together with
Alessia Portieri1, Robin K Harris, Richard A Fletton
1Chemistry Department, Durham University, South Road, Durham DH1 4LE, UK.
Abstract:
We recorded both carbon-13 and nitrogen-15 NMR spectra of the three solid forms of sulfanilamide most commonly known. This study led to an interpretation of the solid-state effects seen in cross-polarization magic angle spinning spectra. Relaxation times for the different forms were measured. These show different behaviour for the three forms, arising from mobility variations. To obtain information on local environments, static spectra and spinning sideband manifolds were recorded and analysed for the 15N resonances, using isotopically enriched samples. Shielding asymmetries and anisotropies for the two nitrogen nuclei were obtained, showing very different behaviour for the two sites. Shielding calculations were carried out for both 13C and 15N nuclei, and the results are discussed in relation to the experimental values.
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