Register      Login
Australian Journal of Chemistry Australian Journal of Chemistry Society
An international journal for chemical science
RESEARCH ARTICLE

Structural studies of technetium complexes. V. The preparation and crystal structure of Dichlorobis(diethyldithiocarbamato)thionitrosyltechnetium(III)

J Baldas, J Bonnyman, MF Mackay and GA Williams

Australian Journal of Chemistry 37(4) 751 - 759
Published: 1984

Abstract

Dichlorobis(diethyldithiocarbamato)thionitrosyltechnetium(III), [Tc(S2CNEt2)2Cl2(NS)], has been prepared by the reaction of [Tc(S2CNEt2)2N] with either disulfur dichloride or thionyl chloride. The crystal structure of [TC(S2CNEt2)2Cl2(NS)] has been determined by single-crystal X-ray diffraction methods at 15ºC. Crystals are orthorhombic, space group Pcmn, with a 8.936(1), b 15.681(1), c 28.445(7) Å, and Z 8. Automatic diffractometry has provided significant Bragg intensities for 2078 independent reflections, and the structure has been refined by full-matrix least-squares methods to R 0.078. The crystal lattice is disordered across a non-crystallographic mirror plane, the degree of disorder being 4.0(2)% for the crystal described above, and 21.9(7)% for another crystal initially used to obtain an intensity data set. There are two independent molecules of [Tc(S2CNEt2)2Cl2(NS)] in the asymmetric unit, and in each the technetium atom is seven-coordinate with a pentagonal-bipyramidal coordination environment. The Tc=N=S bonding is linear with Tc=N c. 1.75 and N=S c. 1.52 Å, which indicates that the thionitrosyl group is a three-electron donor with a formal positive charge. This is only the third crystal structure of a complex containing the thionitrosyl group to be determined, and the first for technetium.

https://doi.org/10.1071/CH9840751

© CSIRO 1984

Committee on Publication Ethics


Export Citation Get Permission

View Dimensions

View Altmetrics