以二乙酰草酰二苯胺,水合醋酸镍和乙二胺为原料,在甲醇中回流反应制得大环草酰胺镍单核配合物(L);以L为配体,采用溶剂热法通过草酰胺桥上的两个氧原子进行桥联配位合成了一个新型的Ni(Ⅱ)-Co(Ⅱ)-Ni(Ⅱ)三核配合物{[(NiL)2 Co(CH3OH)2](ClO4)2·2CH3OH(1)},其结构经IR,元素分析和X-射线单晶衍射表征.1属单斜晶系,空间群P2/n,晶胞参数a=1.203 0(2) nm,b=1.447 5(2)nm,c=1.455 0(2)nm,β =93.954(3)°,V=2.527 4(7) nm3,Z=4,Dc =1.572 g·cm-3,F(000) =1 234,R1=0.042 2,wR2=0.097 7.
A macrocyclic oxamide-Ni(Ⅱ) complex(L) was synthesized by reflux of 2,3-dioxo-5,6 ∶ 13,14-dibenzo-7,12-dimethyl-1,4,8,1 1-tetraazacyclopentadeca-7,12-diene,nickel acetate and ethylenediamine in methanol.A novel Ni (Ⅱ)-Co (Ⅱ)-Ni (Ⅱ) trinuclear complex { [(NiL)2Co (CH3 OH)2](ClO4)2 · 2CH3 OH(1)} was synthesized by solvent thermal method using L as the ligand.The structure was characterized by IR,elemental analysis and X-ray single-crystal diffraction.1 belongs to monoclinic,space group P2/n with a =1.203 0(2) nm,b =1.447 5(2) rnn,c =1.455 0(2) nm,β=93.954(3)°,V=2.527 4(7) nm3,Z=4,Dc=1.572 g· cm-3,F(000) =1 234,R1 =0.042 2,wR2 =0.097 7 .