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Novel Rhenium(III IV and V) Tetradentate N2O2 Schiff Base Mononuclear and Dinuclear Complexes

机译:新型R(IIIIV和V)四齿N2O2希夫碱单核和双核配合物

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摘要

Reaction of (Bu4N)[ReOCl4] with the tetradentate Schiff base ligand α, α’-[(1,1-dimethylethylene)dinitrilo]di-o-cresol (sal2ibnH2) yields cis-[ReVOCl(sal2ibn)], which quickly forms trans-[μ-O(ReVO(sal2ibn))2] in solution. The dinuclear complex can also be isolated by the addition of base (Et3N) to the reaction mixture. Conversely, the mononuclear complex can be trapped as cis-[ReVO(NCS)(sal2ibn)] by addition of (Bu4N)SCN to the reaction mixture. Reduction of cis-[ReVO(NCS)sal2ibn] with triphenylphosphine gives the unique trans-[ReIII(NCS)(PPh3)(sal2ibn)] and rare μ-oxo Re(IV) dimer trans-[μ-O(ReIV(NCS)(sal2ibn))2]. All of the complexes were characterized by 1H and 13C NMR, FT-IR spectroscopy, electrospray ionization mass spectrometry (ESI-MS), cyclic voltammetry and single crystal X-ray diffraction.
机译:(Bu4N)[ReOCl4]与四齿席夫碱配体α,α'-[(1,1-二甲基乙烯)二腈]二-邻甲酚(sal2ibnH2)的反应生成顺-[Re V OCl(sal2ibn)],可在溶液中快速形成反式[μ-O(Re V O(sal2ibn))2]。也可以通过向反应混合物中加入碱(Et3N)来分离双核配合物。相反,通过向反应混合物中添加(Bu4N)SCN,可以将单核络合物捕获为顺式[Re V O(NCS)(sal2ibn)]。用三苯基膦还原顺式[Re V O(NCS)sal2ibn]可得到独特的反式-[Re III (NCS)(PPh3)(sal2ibn)]和稀有的μ -oxo Re(IV)二聚体反式-[μ-O(Re IV (NCS)(sal2ibn))2]。所有配合物的特征均通过 1 H和 13 C NMR,FT-IR光谱,电喷雾电离质谱(ESI-MS),循环伏安法和单晶X-射线衍射。

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