作者:Wenerios Tsagkalidis、Claus Woitha、Dieter Rehder
DOI:10.1016/s0020-1693(00)85544-9
日期:1993.3
The reaction of VCl3(thf)3 (1) with NN-dimethylhydrazine yields VCl3(thf)2(H2NNMe2) (2) or, with excess hydrazine, VCl3(NH2NMe2)2 (4). In the presence of 1,2-bis(dimethylphosphino)ethane (dmpe), VCl3(dmpe)(NH2NMe2).0.5thf (7) is obtained. As 1 is reacted with tris(3-dimethylphosphinopropyl)phosphine (tdmp) and lithium hydrazide, the V(II) species VCl2(tdmp)(NH2NMe2) (10) and VC]2(tdmp) (11) are formed. While H2NNMe2 coordinates end-on via its NH2 group in the case of 2, 7 and 10, 4 probably contains the two hydrazine ligands in a side-on bonding mode. The compounds were characterized by elemental analyses, IR, H-1 NMR and susceptibility measurements. The NH2 Protons are deshielded with respect to the free hydrazine by 3.8 to 5.6 ppm. For comparison, the complexes VCl3(amine)x(thf), (amine = ethylenediamine, x and y = l, 5; tetramethylethylenediamine, x = 2, y = 0, 6; N-aminopiperidine, x = 1, y = 2, 3) have also been prepared.