首页> 外文期刊>Transition Metal Chemistry >Synthesis, spectroscopic characterization and X-ray single crystal structures of trans-bis[4-methoxyphenyl (3-methylbutyl) dithiophosphinato] nickel(II) and bis [4-methoxyphenyl (3-methylbutyl) dithiophosphinato]cobalt(II) complexes
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Synthesis, spectroscopic characterization and X-ray single crystal structures of trans-bis[4-methoxyphenyl (3-methylbutyl) dithiophosphinato] nickel(II) and bis [4-methoxyphenyl (3-methylbutyl) dithiophosphinato]cobalt(II) complexes

机译:反式双[4-甲氧基苯基(3-甲基丁基)二硫代膦酸酯]镍(II)和双[4-甲氧基苯基(3-甲基丁基)二硫代膦酸酯]钴(II)配合物的合成,光谱表征和X射线单晶结构

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摘要

Thionation of 3-methylbutylmagnesium bromide with Lawesson's Reagent (LR) gave 4-methoxyphenyl (3-methylbutyl)dithiophosphinic acid (DTPA), and the latter was converted to the ammonium salt (NH4L = Ammonium 4-methoxyphenyl (3-methylbutyl) dithiophosphinate). The complex, trans-bis[4-methoxyphenyl(3-methylbutyl) dithiophosphinato] nickel(II) [NiL2], was prepared by the reaction of NH4L with NiCl2.6H2O in EtOH. Bis [4-methoxyphenyl (3-methylbutyl) dithiophosphinato]cobalt(II) [(CoL2)2] was also prepared in the same way. The structures of the complexes have been characterized by elemental analysis, FTTR, ~1H, ~(13)C, ~(31)P NMR and X-ray diffraction. The single crystal X-ray structures of [NiL2] and [(CoL2)2] show that the nickel complex is square planar while the cobalt counterpart has tetrahedral coordination with a dimeric structure. Bond lengths, angles, torsion angles and dihedral angles are correlated to the structures and also compared with the literature data on similar compounds.
机译:用Lawesson试剂(LR)对3-甲基丁基溴化镁进行亚硫酰化,得到4-甲氧基苯基(3-甲基丁基)二硫代次膦酸(DTPA),后者转化为铵盐(NH4L = 4-甲氧基苯基铵(3-甲基丁基)二硫代次膦酸铵) 。通过使NH 4 L与NiCl 2·6H 2 O在EtOH中反应来制备复合双-[4-甲氧基苯基(3-甲基丁基)二硫代膦酰基]镍(II)[NiL 2]。还以相同方式制备了双[4-甲氧基苯基(3-甲基丁基)二硫代膦酰基]钴(II)[(CoL2)2]。配合物的结构已通过元素分析,FTTR,〜1H,〜(13)C,〜(31)P NMR和X射线衍射进行了表征。 [NiL2]和[(CoL2)2]的单晶X射线结构表明,镍配合物为正方形平面,而钴对应物具有二聚体结构的四面体配位。键长,角度,扭转角和二面角与结构相关,并与类似化合物的文献数据进行比较。

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