Issue 9, 2009

The crystal structure and evidence of the phase transition in d-amphetamine sulfate, as studied by X-ray crystallography, DSC and NMR spectroscopy

Abstract

X-Ray crystallography, DSC and NMR spectroscopy methods have been used to study the phase transition of D-amphetamine sulfate. The phase transition temperature occurs at about 325 K, and belongs to the discontinuous type with a large temperature hysteresis. A change in the space group is observed from monoclinic P21 in the low temperature phase to monoclinic C2 in the high temperature phase. The transformation from phase I to phase II is a result of the ordering of the SO42−groups, allowing a T-shape interaction between D-amphetamine molecules. Proton relaxation rate data obtained for the studied compound have been analysed by assuming two dynamically-inequivalent methyl groups below the phase transition and only one type of ammonium group above the phase transition. The activation energies for the C3 reorientation of the methyl groups have been determined to be 7.31 and 11.89 kJ mol−1, whereas for the ammonium group it is 27.29 kJ mol−1.

Graphical abstract: The crystal structure and evidence of the phase transition in d-amphetamine sulfate, as studied by X-ray crystallography, DSC and NMR spectroscopy

Supplementary files

Article information

Article type
Paper
Submitted
03 Sep 2008
Accepted
01 Jun 2009
First published
03 Jul 2009

New J. Chem., 2009,33, 1894-1900

The crystal structure and evidence of the phase transition in D-amphetamine sulfate, as studied by X-ray crystallography, DSC and NMR spectroscopy

K. Pogorzelec-Glaser, J. Kaszyńska, A. Rachocki, J. Tritt-Goc, N. Piślewski and A. Pietraszko, New J. Chem., 2009, 33, 1894 DOI: 10.1039/B815325F

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