Synthesis and separation of the mer and fac isomers of [Rh(bpp)(3)][PF6](3) (bpp equals 2,3-bis(2-pyridyl)pyrazine)

被引:12
作者
Tresoldi, G
LoSchiavo, S
Piraino, P
机构
[1] Dipto. Chim. Inorg., Analitica S., Università di Messina, 98166 Vill. S. Agata, Messina
关键词
isomer separation; rhodium complexes; tris-chelated complexes;
D O I
10.1016/S0020-1693(96)05165-1
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The new complex [Rh(dps)(2)Cl-2]PF6 (1) (dps = di-2-pyridyl sulfide) was prepared by reacting RhCl3 with dps in an ethanol-water-mixture (2:1). As shown by H-1 NMR spectroscopy 1 exhibits a cis geometry. By refluxing 1 with bipy or phen (bipy = 2,2'-bipyridine, phen = 1,10-phenanthroline) in dimethylformamide the complexes [Rh(bipy)(2)Cl-2]PF6 and [Rh(phen)(2)Cl-2]PF6 were respectively obtained. On the contrary the reaction of 1 with bpp (bpp = 2,3-bis(2-pyridyr) pyrazine), carried out in the same experimental conditions, gave [Rh(bpp)3][PF6](3), (2) in high yields. The meridional (mer) and facial (fac) isomers of 2 were separated by chromatography. Despite the complexity of the H-1 and C-13 NMR spectra of the mer isomer, almost complete assignment of the resonances was possible by employment of two-dimensional techniques and by comparison with the resonances of the fac isomer.
引用
收藏
页码:381 / 385
页数:5
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