Chromatographic,spectroscopic, topographic,and X-ray crystallographic studies of the solid solution formed by racemic 3-carboxy-2,2,5,5-tetramethyl-1-pyrrolidinyloxy (3-carboxy-proxyl) |
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Authors: | Philip J. Cox Susan Blaney Steve W. Love Norman Shankland David B. Sheen |
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Affiliation: | (1) School of Pharmacy, The Robert Gordon University, Schoolhill, AB9 1FR Aberdeen, Scotland;(2) Department of Pharmaceutical Sciences, University of Strathclyde, Royal College, 204 George Street, G1 1XW Glasgow, Scotland;(3) Department of Pure and Applied Chemistry, University of Strathclyde, 295 Cathedral Street, G1 1XL Glasgow, Scotland |
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Abstract: | The solid solution formed by the title compound, C9H16NO3, has been examined by a variety of techniques and shown to be an equi-molecular mixture of the two enantiomers. Refinement of the disordered structure was based on the orthorhombic space groupPnma witha=8.023(2),b=10.030(3), andc=12.352(2)Å, finalR=0.055. The oxygens of the carboxyl group are disordered and both enantiomers can occupy the same, rather than alternate, crystallographic sites. Results from studies involving IR, GC-MS, and chiral chromatography are also presented. In addition we report on the use of synchrotron X-ray topography to investigate strain in crystals of the solid solution. |
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Keywords: | Solid solution enantiomers disorder X-ray topography |
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