The use of Mo Kα radiation in the assignment of the absolute configuration of light-atom molecules; the importance of high-resolution data.

Abstract

Recent studies have confirmed the usefulness of the Hooft and Parsons methodologies for determination of the absolute crystal structures of enantiopure light-atom compounds using Cu Kα radiation. While many single-crystal diffractometers used for small-molecule structure determination are equipped with molybdenum anodes, use of data from such instruments for the absolute structure determination of light-atom crystal structures is rarely documented and has often been found to be unsuccessful. The Hooft and Parsons methodologies have been applied to 44 data sets obtained from single crystals containing light-atom molecules of known chirality using Mo Kα radiation. Several factors influencing the calculation of accurate and precise values for the Hooft and Parsons parameters obtained from these data sets have been identified, the inclusion of high-resolution diffraction data being particularly important. The correct absolute structure was obtained in all cases, with the standard uncertainties of the final absolute structure parameters below 0.1 for the great majority.