The new monomeric complexes of[M(MPA)2(Im)2]·2H2O(1:M=Co; 2:M=Ni)(HMPA=5-methyl-1H-pyrazole-3-carboxylic acid,Im=imidazole)were synthesized by the reaction of HMPA and Im with M(OAc)2·4H2O (M=Co,Ni),respectively.The compounds were characterized by elemental analysis,IR spectra,single crystal Xray diffraction,thermogravimetric analysis and cyclic voltammetry.The structural parameters of 1 and 2 were analyzed as follows:1,monoclinic,P21,a=0.84702(16)nm,b=1.4615(3)nm,c=0.89967(17)nm,β=101.759(6)°,V=1.0903(4)nm3,Z=2; 2,monoclinic,P21,a=0.85359(6)nm,b=1.45177(9)nm,c=0.88983(6)nm,β=102.3820(10)°,V=1.07704(12)nm3,Z=2.Metal ions have all octahedral geometry coordinated by two nitrogen atoms from two Im molecules,two nitrogen atoms and two oxygen atoms from two MPA-ligands.In both complexes,the independent components[M(MPA)2(Im)2]· 2H2O are connected by two kinds of intermolecular hydrogen bonds (N-H…O and C-H…O)to form a three-dimensional supramolecular architecture.Electrochemical property of the complex shows that electron transfer of M(Ⅱ)between M(Ⅲ)(M=Co,Ni)in electrolysis is quasi-reversible process.CCDC:848231,1; 848232,2.%利用5-甲基-3-吡唑甲酸、咪唑和相应醋酸盐在乙醇和水混合溶剂中反应,得到了配合物[M(MPA)2(Im)2]· 2H2O(1:M=Co;2:M=Ni)(HMPA=5-甲基-3-吡唑甲酸,Im=咪唑).用元素分析、红外光谱、X-单晶衍射结构分析、热重分析、循环伏安等对其进行了表征.配合物1和2的晶体结构参数如下:配合物1和2的晶体都属于单斜晶系,空间群为P21.配合物1的晶胞参数为a=0.84702(16)nm,b=1.4615(3)nm,c=0.89967(17)nm,β=101.759(6)°,V=1.0903(4)nm3,Z=2；配合物2的晶胞参数为a=0.85359(6)nm,b=1.45177(9)nm,c=0.88983(6)nm,β=102.3820(10)°,V=1.07704(12)nm3,Z=2.金属离子与来自2个5-甲基-3-吡唑甲酸配体中的2个氮原子及2个氧原子,2个咪唑分子中的2个氮原子配位,形成八面体配位构型.配合物中的独立结构单元[M(MPA)2(Im)2]· 2H2O通过2种分子间氢键(N-H…O和C-H…O)形成三维超分子.循环伏安性质测试表明配合物1和2的电解过程均为准可逆过程.
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