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在乙腈溶液中,由混合价三核锰配合物[Mn3O(ClCH2COO)6(py)2]?(H2O)(py为吡啶)与2,2′-联吡啶(bipy)反应合成了混合价(Mn3IIIMnII)四核锰配合物[Mn4O2(ClCH2COO)7(bipy)2]?H2O.采用元素分析、红外光谱、热分析和X射线单晶衍射法确定了其组成和结构.标题化合物晶体属于三斜晶系,空间群P-1,晶胞参数:a=0.89854(13)nm,b=1.4027(2)nm,c=1.9037(3)nm,α=93.518(3)°,β=96.736(3)°,γ=94.875(3)°,V=2.3680(6)nm3,Z=2,Dc=1.734g/cm3,F(000)=1238,GOF=1.036,R1=0.0592,wR2=0.1162[I>2σ(I)].在标题化合物中,配位结构单元中心为一蝶型[Mn4(μ3-O)2]7+多核簇,含有2个Mn3(μ3-O)单元,具有近似C2对称轴.4个Mn离子均为六配位,外围配体为7个氯乙酸根和2个2,2′-联吡啶,处于变形的八面体环境.变温磁化率研究表明标题化合物在整体上表现为反铁磁性耦合作用,但在低温下的磁相互作用较为复杂.
In the acetonitrile solution, the mixed valence trinuclear manganese complex [Mn3O (ClCH2COO) 6 (py) 2] (H2O) (py is pyridine) was reacted with 2,2’-bipyridyl Mn3O2IMnII) tetranuclear manganese complex [Mn4O2 (ClCH2COO) 7 (bipy) 2]? H2O was determined by elemental analysis, infrared spectroscopy, thermal analysis and X-ray single crystal diffraction.The title compound belongs to triclin (3) nm, α = 93.518 (3) ° and β = 96.736 (3), respectively. The crystal lattice and the space group P-1 have a unit cell parameter of a = 0.89854 (13) nm and b = 1.4027 , Γ = 94.875 (3) °, V = 2.3680 (6) nm3, Z = 2, Dc = 1.734g / cm3, F (000) = 1238, GOF = 1.036, R1 = 0.0592, wR2 = 0.1162 [I > 2σ (I)]. In the title compound, the center of the coordination unit is a butterfly [Mn4 (μ3-O) 2] 7+ polynuclear cluster with two Mn3 (μ3-O) units with approximately C2 symmetry Axis. All four Mn ions are hexacoordinated and their peripheral ligands are seven chloroacetates and two 2,2’-bipyridyls, which are in the deformed octahedral environment. The study of the temperature-dependent magnetic susceptibility shows that the title compounds are overall as a whole For the anti-ferromagnetic coupling, but the magnetic interaction at low temperatures is more complicated.