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Issue 17, 2013
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NMR characterisation of dynamics in solvates and desolvates of formoterol fumarate

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Abstract

Solid-state NMR is used to characterise dynamics in the ethanol solvate of the pharmaceutical material formoterol fumarate and its associated desolvate. Jump rates and activation barriers for dynamic processes such as phenyl ring rotation and methyl group rotational diffusion are derived from 1D-EXSY and 13C spin–lattice relaxation times respectively. 2H and 13C spin–lattice relaxation times measured under magic-angle spinning conditions are used to show that the fumarate ion in the desolvate is undergoing small-amplitude motion on a frequency scale of 100s of MHz at ambient temperature with an activation parameter of about 32 kJ mol−1. Exact calculations of relaxation times under MAS provide a simple and robust means to test motional models in cases where relaxation rate maxima are observed, including for systems where the crystal structure of the material is unknown.

Graphical abstract: NMR characterisation of dynamics in solvates and desolvates of formoterol fumarate

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Article information


Submitted
15 Jan 2013
Accepted
12 Mar 2013
First published
25 Mar 2013

Phys. Chem. Chem. Phys., 2013,15, 6422-6430
Article type
Paper

NMR characterisation of dynamics in solvates and desolvates of formoterol fumarate

D. C. Apperley, A. F. Markwell, I. Frantsuzov, A. J. Ilott, R. K. Harris and P. Hodgkinson, Phys. Chem. Chem. Phys., 2013, 15, 6422
DOI: 10.1039/C3CP50180A

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