A novel oxamido-bridged trinuclear complex Cu(NiL)2(ClO4)2 (where H2L=2,3-dioxo-5,6,14,15-dibenzo-1,4,8,12-tetraazacyclo-pentadeca-7,3-dien) has been synthesized and characterized by elemental analysis, IR spectrum, UV-Visible spectrum and single crystal X-ray diffraction. It crystallizes in the monoclinic system, space group P21/n. The lattice parameters are: a=1.052 4(6) nm, b=1.182 1(6) nm, c=1.586 2(9) nm, a=91.657(9) and V=1.972 6(19) nm3, Z=2. The results show that the coordination geometry around copper(Ⅱ) in the title complex is hexa-coordinated octahedron. CCDC: 232608.
用分步合成法得到了5对互为对映体的氰根桥连Fe(Ⅲ)-Cu(Ⅱ)-Ln(Ⅲ)异三金属配合物[{Cu(RR-valcy)Ln(H_(2)O)1.5(CH_(3)OH)1.5}{Fe(CN)_(6)}]·4H_(2)O·CH_(3)OH(Ln=Dy,1;Ho,3;Er,5;Tm,7;Yb,9)和[{Cu(SS-valcy)Ln(H_(2)O)1.5(CH_(3)OH)1.5}{Fe(CN)_(6)}]·4H_(2)O·CH_(3)OH(Ln=Dy,2;Ho,4;Er,6;Tm,8;Yb,10)(H_(2)valcy=N,N’-双(3-甲氧基水杨醛)-缩-1,2-环己二胺).X-射线单晶衍射分析表明,5对同构的对映体属于单斜晶系,P2(1)空间群,每个[Fe(CN)_(6)]^(3-)与一个[Cu(RR/SS-valcy)Ln(H_(2)O)_(1.5)(CH_(3)OH)_(1.5)]单元通过Fe-C≡N-Ln桥相连接.圆二色光谱测试证明每对配合物的光学活性和对映异构体性质.配合物1、3、5、7和9在2-300 K的直流变温磁化率数据符合Curis-Weiss定律,Weiss常数θ依次为-0.274、-3.64、-9.83、-7.29和-15.32 K.