以Fe(ClO4)2.6H2O和N,N',N'',N'''-四(2-吡啶甲基)-1,4,8,11-四氮杂环十四烷(tpmc)为原料,采用溶液界面扩散法,在二氯甲烷与乙醇两相溶剂的界面上制得Fe(Ⅱ)的双核配合物[Fe2(μ2-OH)(C34H44N8)](ClO4)3.EtOH(1),其结构经X-射线单晶衍射表征。1属正交晶系,Pbcm空间群,晶胞参数a=11.652(2),b=17.505(4),c=22.256(5),α=β=γ=90°,V=453 9.7(16)3,Z=4,Dc=1.519 g.cm-3,μ=0.887 mm-1,F(000)=2 152,R1=0.058 3,ωR2=0.175 8。1中的Fe(Ⅱ)分别与外向型配体tpmc的十四元环上的两个氮原子,两个吡啶环上的氮原子和μ2-OH上的氧原子配位,形成一个畸变的三角双锥几何构型。连接两个Fe(Ⅱ)核中心的μ2-OH氧桥以及分子内和分子间的氢键缔合作用,增强了晶体结构的稳定性。
Hydroxo-bridged binuclear complex,[Fe2(μ2-OH)(tpmc)](ClO4)3·EtOH(1),was synthesized through by reaction of N,N',N'',N'''-tetrakis(2-pyridylmethyl)-1,4,8,11-tetraazacyclotetradecane(tpmc) with ferrous perchiorate hexahydrated by the liquid diffusion method,at the interface of dichloromethane and ethanol solvent.The structure was characterized by X-ray single crystal diffraction.1 belongs to orthorhombic system,space group Pbcm with a=11.652(2),b=17.505(4) ,c=22.256(5),α=β=γ=90°,V=4 539.7(16)3,Z=4,Dc=1.519 g·cm-3,μ=0.887 mm-1,F(000)=2 152,R1=0.058 3,ωR2=0.175 8.Each iron(Ⅱ) ion is coordinated with four nitrogen atoms in an exo arrangement of tpmc groups while the additional μ2-hydroxo bridges metal-ion centers.The coordination geometry about the Fe(Ⅱ) atoms may be regarded as a distorted trigonal bipyramid.The crystal structure is stabilized by the μ2-OH which bridges two Fe(Ⅱ) centers and intra-and inter-molecular hydrogen bond association function.