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Thiocarbonyl Complexes of Rhenium. Part I. Synthesis, Characterization and X-Ray Structures of and
Abram, Ulrich,Lorenz, Bernd
, p. 771 - 777 (2007/10/02)
Novel rhenium complexes with terminal thiocarbonyl gropus have been synthesized from ReCl3(Me2PhP)3 and sodium diethyl dithiocarbamate. mer-(Diethyldithiocarbamato)tris(dimethylphenylphosphine)(thiocarbonyl)rhenium(I), mer-, and tris(diethyldithiocarbamato)(thiocarbonyl)rhenium(III), have been studied by infrared and NMR spectroscopy, mass spectrometry and X-ray diffraction. mer- crystallizes orthorhombic in the space group Pna21 with a = 1516.1(2), b = 2189.8(2) and c = 1035.6(1) pm.Structure solutions and refinement converged at R = 0.042.The coordination geometry is a distorted octahedron.The Re-C bond length is found to be 184(2) pm. crystallizes monoclinic in the space group P21/c with a = 962.2(6), b = 1744.0(2), c = 1537.4(6) pm and β = 96.21(1) deg.The final R value is 0.028.In the monomeric complex the rhenium atom is seven-coordinate with an approximate pentagonal-bipyramidal coordination sphere and a rhenium-carbon distance of 181(1) pm. Key words: Rhenium compounds; thiocarbonyl complexes; crystal structure; mass spectra; X-ray.
