Abstract
The low temperature phase of 4,7-Dioxatricyclo[3.2.1.03.6]octane (I) has been characterized by X-ray diffraction at four temperatures from 190 to 268 K. Over this range, the monoclinic (space group C2/m) unit cell volume changes linearly with temperature. At 268 K a phase change is observed to give a cubic unit cell (space group Fm3m) with a 10% increase in cell volume. The scattered X-ray intensities and solid state NMR data are in close agreement with a cubic close packed structure of isotropically rotating molecules, however, there is evidence for some deviation from free rotation.
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