以四齿席夫碱配体甲氧基水杨醛肟构筑了2个新型的六核Tb(Ⅲ)和Dy(Ⅲ)配合物[Tb_6(HL)_8L_4(EtOH)_2(NO_3)_2(4,4-bpy)]·2(4,4-bpy)(1)和[Dy_6(HL)_8L_4(EtOH)_2(NO_3)_2(4,4-bpy)]·2(4,4-bpy)(2)(L为3-甲氧基水杨醛肟).晶体结构分析表明,配合物1与2均属于三斜晶系,P-1空间群,配合物1的晶胞参数:a=1.097 3(2)nm,b=1.700 6(3)nm,c=2.045 3(4)nm,Z=2,配合物2的晶胞参数:a=1.097 3(2)nm,b=1.700 6(3)nm,c=2.045 3(4)nm,Z=2.配合物由甲氧基水杨醛肟与稀土离子构筑三核单元,通过4,4-bpy桥联成为稀土六核簇合物,并研究了配合物的荧光性质. Two novel six-core Tb (Ⅲ) and Dy (Ⅲ) complexes [Tb_6 (HL) _8L_4 (Et_OH) _2 (NO_3) _2 -bpy) 2 · (4,4-bpy) (1) and [Dy 6 (HL) 8L_4 (EtOH) 2 ) (L is 3-methoxy salicylaldoxime) .The crystal structure analysis showed that the complexes 1 and 2 belong to the triclinic system, P-1 space group, the unit cell parameters of complex 1: a = 1.097 3 (2 (2) nm, b = 1.700 6 (3) nm, b = 1.700 6 (3) nm, c = 2.045 3 (4) nm and Z = , c = 2.045 3 (4) nm, Z = 2. The complex was composed of methoxy salicylaldehyde oxime and rare earth ions to form a trinuclear unit, through the 4,4-bpy bridge to become a rare earth hexanuclear cluster, and studied the coordination Fluorescent properties of matter.