2,6-二甲基苯基-β-二亚胺配合物的合成及表征
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摘要
通过液相扩散法得到了2,6-二甲基苯基-β-二亚胺的铜、镍配合物,配合物的结构通过红外光谱,X-粉末衍射及元素分析表征,X射线单晶衍射进一步确定配合物的结构。单晶结构显示,配合物为三斜晶系,空间群Pī,分子式为C_(44)H_(54)MN_4O_4(M∶Cu,Ni),空气中的O原子,甲醇分子的CH_3O-插入到β-二亚胺的亚甲基上,导致了两分子配体的两个N原子,插入的O原子与金属中心配位,生成了双配体四齿单金属配合物,形成了新颖的配位模式。在铜、镍配合物中,面与面之间依靠C-H…π键弱的相互作用力构建成二维层状结构。
The 2,6-dimethyl phenyl β-diketiminato copper,nickel complexes were synthesized by liquidliquid diffusion method. The complexes were characterized by IR spectroscopy,powder X-ray diffraction,elemental analysis,and their structures were comfirmed by X-ray single crystal diffraction. The crystals belonged to the triclinic system,space group Pī. The molecular formula is C_(44)H_(54)MN_4O_4( M∶ Cu,Ni). It was found that O of atmosphere,CH_3O-of MeOH were inserted into CH_2 of β-diketimine. The structures were special and were consisted by one metal centre,two ligands and coordinated by two N and two O atoms. The two-dimensional layers of the compounds were formed through C-H … π bond stacking interactions.
The 2,6-dimethyl phenyl β-diketiminato copper,nickel complexes were synthesized by liquidliquid diffusion method. The complexes were characterized by IR spectroscopy,powder X-ray diffraction,elemental analysis,and their structures were comfirmed by X-ray single crystal diffraction. The crystals belonged to the triclinic system,space group Pī. The molecular formula is C_(44)H_(54)MN_4O_4( M∶ Cu,Ni). It was found that O of atmosphere,CH_3O-of MeOH were inserted into CH_2 of β-diketimine. The structures were special and were consisted by one metal centre,two ligands and coordinated by two N and two O atoms. The two-dimensional layers of the compounds were formed through C-H … π bond stacking interactions.
引文
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[3]Venugopal A,Ghosh M K,Jürgens H,et al.(β-Diketiminato)dimethylgold(III):Synthesis,Structure,and Reactivity[J].Organometallics,2010,29(10):2248-2253.
[4]Ding Y,Roesky H W,Noltemeyer M,et al.Synthesis and Structures of Monomeric Divalent Germanium and Tin Compounds Containing a Bulky Diketiminato Ligand[J].Organometallics,2001,20(6):1190-1194.
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[7]Spencer D J E,Aboelella N W,Reynolds A M,et al.β-Diketiminate Ligand Backbone Structural Effects on Cu(I)/O2Reactivity:Unique Copper-Superoxo and Bis(μ-oxo)Complexes[J].J.Am.Chem.Soc.,2002,124(10):2108-2109.
[8]赵志鹏.功能性镧系配合物的可控制备及性能研究[D].南昌:江西师范大学,2018.
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[11]Sheldrick G M.Crystal Structure Refinement with SHELXL[J].Acta Cryst.C,2015,71(1):3-8.
[12]Azoulay J D,Rojas R S,Serrano A V,et al.Nickelα-Keto-β-Diimine Initiators for Olefin Polymerization[J].Angew.Chem.Int.Ed.,2009,48(6):1089-1092.
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