Structural Study of Optical Resolution. IV-b. The Crystal Structure of (+)589-Oxalatobis(ethylenediamine)cobalt(III) Hydrogen-d-tartrate Monohydrate and Its Thermal Behavior

Abstract
The crystal structure of (+)589-oxalatobis(ethylenediamine)cobalt(III) hydrogen-d-tartrate monohydrate, (+)589-[Co(ox)en2]H-d-tart·H2O, has been determined by three-dimensional X-ray analysis. The red crystals are monoclinic, space group P21 with two molecules in a unit cell of dimensions a=8.27(1), b=14.60(1), c=7.02(1) Å, and β=104.8(2)°. The structure was solved by Patterson and Fourier methods, and refined by anisotropic blockdiagonal least-squares to a conventional R-value of 0.100 for the 1265 independent reflections observed. In the diastereoisomer, the optically active complex cation is locked by the {H-d-tart}∞ units of the right-handed spiral chains formed along the b-axis. The TG and DSC measurements have been carried out on both less- and more-soluble diastereoisomers of oxalatobis(ethylenediamine) cobalt (III) hydrogen-d-tartrate; the difference of their thermal behavior is discussed.

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