【摘要】 用丙酮和乙二胺在高氯酸催化下合成了四氮杂十四元环席夫碱(1),并用1与碱式碳酸铜和叠氮化钠反应,生成铜的双核大环配合物。通过X-射线单晶衍射和红外光谱对其进行了结构表征。该配合物属单斜晶系,P2(1)空间群,晶胞参数为a=0.93214(8)nm,b=2.03665(17)nm,c=2.6540(2)nm;β=99.6590(10)°;V=4.9670(7)nm3,Z=2,Dc=1.387mg/m3,Mr=2074.76,F(000)=2172,最终R=0.0557,wR=0.1241。该配合物包括2个不对称的双核结构、6个高氯酸根和1个水分子。每一个双核结构中的铜原子都是五配位,它们分别和大环配体上的4个氮原子及叠氮根两端的氮原子配位形成畸变的四方锥构型。更多还原

【Abstract】 A tetraaza macrocyclic Schiff base was synthesized through the reaction of acetone and ethylenediamine under catalysis of perchloric acid. Then the Schiff base was reacted with Cu2 (OH)2 CO3 and NaN3 to form binuclear copper ( Ⅱ ) macrocyclic complex. The characterization of IR and X-Ray single crystal diffraction showed that the prepared complex belongs to monoclinic system with space group P2(1),a = 0. 93214(8) nm,b = 2. 03665(17)nm,c = 2. 6540(2) nm; β = 99. 6590(10)°; V = 4. 9670(7) nm3 ,Z = 2,Dc = 1. 387Mg /m3 ,Mr = 2074. 76,F ( 000 ) = 2172,final R = 0. 0557,wR = 0. 1241. The complex consists of two asymmetry binuclear structures,six ClO 4- and one water molecule. The copper atom in each binuclear structure is five-coordinated by five nitrogen atoms (four nitrogen atoms come from the Schiff base and one nitrogen atom comes from the azido anion). As result,a slightly distorted square pyramid geometry is formed.更多还原