Synthesis, spectroscopic investigation and molecular structure of pentacarbonyl-5-t-butyl-5-aza-2,8-dithia-1-stannobicyclo[3.3.01,5]octanechromium(0)

Abstract

The compound pentacarbonyl-5-t-butyl-5-aza-2,8-dithia-1-stannobicyclo-[3.3.01,5]octanechromium(0) was prepared in good yield by the reaction of 5-t-butyl-5-aza-2,8-dithia-1-stannobicyclo[3.3.01,5]octane with Cr(CO)6 in THF under UV-irradiation. The crystal and molecular structure was determined from three-dimensional X-ray data. The crystals are monoclinic, space group P21/c. The unit cell, with dimensions a 14.963(9), b 10.026(5), c 13.565(5)Å, β 114.68°(5), contains 4 molecules. The structure was solved by the Patterson-method. The full-matrix refinement with the 2734 independent reflexions gave a final R value of 0.034. The eight-membered ring adopts an asymmetric boat-boat conformation with a tin-nitrogen bond lenght of 2.40 Å; the tin-chromium bond length is 2.62 Å.