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常磁性 Rhenium, rhodium 및 Iridium 化合物의 合成 및 分析
金大洙 韓國敎員大學校 大學院 1992 국내석사
Paramagnetic 19-electron rhenium carbonyl complex,Re(CO)_(4)L_(2)[L_(2)=2,3-bis(diphenylphosphino)maleic anhydride],was obtained via chemical method using synthesized bidentate ligand,2,3-bis(diphenylphosphino)maleic anhydride. This complex was characterized by IR, ^(31)P NMR,Cyclovoltammetry and ESR spectrscopy. The most efficient route to synthesize this complex was as follows. 1) Re(CO)_(5)OSO_(2)CF_(3) is obtained from Re(CO)_(5)Br and AgSO_(3)CF_(3) in CH(2)Cl_(2). 2) Re(CO)_(5)OSO_(2)CF_(3) thus abtained reacts with L_(2) that has π orbital of low energy to give [Re(CO)_(4)L_(2)](OSO_(2)CF_(3)) in toluene. 3)[Re(CO)_(4)L_(2)](OSO_(2)CF_(3)) is reduced chemically by reducing agents such as sodium naphthalenide or cobaltocene. ESR spectrum of Re(CO)_(4)L_(2) complex obtained by reduction shows that 19th electron is primarily delocalized over the π orbital of the ligand. We expect that CO groups in Re(CO)_(4)L_(2) complex will be easily substituted with other ligands such as phosphine. Then, we synthesized CpM(1,4-N_(4)Ph_(2) (M=Rh,Ir) complexes via [CpMCl_(2)]_(2) and bidentate tetrazene ligand,[Li(THF)_(x)]_(2)[PhNN=NNPh]. Also, we identified photochemically substituted reaction products in the reaction of CpIr(1,4-N_(4)Ph_(2)) and some unsaturated compounds such as diphenylacetylene and fumaronitrile using Mass spectroscopy.
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