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采用水热法合成稀土无机有机杂化化合物[Nd(PW11O39)(H2O)3](H2bpy)2.4H2O。采用NdCl3.6H2O,(NH4)3PW12O40.3H2O,4,4’-联吡啶(bpy),和去离子水(摩尔比为4∶1∶4∶3900,pH=6)在130℃下进行水热反应3天,得到标题化合物的紫红色块状晶体,并进行了红外光谱分析,元素分析。用单晶X射线衍射法测得晶体结构,属三斜晶系,空间群为P-1,晶胞参数为:a=1.18824(9)nm,b=1.35707(10)nm,c=1.77691(13)nm,α=71.551(2)°,β=82.478(2)°,γ=80.568(2)°。该晶体由无机的共价链∞1[Nd(PW11O39)(H2O)3]4-和有机的二质子化的4,4’-联吡啶(H2bpy)2+及结晶水分子堆积而成的,是一个新的稀土磷钨酸盐无机有机杂化化合物。
Hydrothermal synthesis of rare earth inorganic and organic hybrid compounds [Nd (PW11O39) (H2O) 3] (H2bpy) 2.4H2O. Hydrothermal treatment was carried out at 130 ° C using NdCl3.6H2O, (NH4) 3PW12O40.3H2O, 4,4’-bipyridine (bpy), and deionized water (molar ratio of 4: 1: 4: 3900, pH = 6) The reaction was carried out for 3 days to obtain the purple-red lumpy crystals of the title compound, which were analyzed by infrared spectroscopy and elemental analysis. The crystal structure was determined by single crystal X-ray diffraction and belongs to the triclinic system with P-1 space group. The unit cell parameters are: a = 1.18824 (9) nm, b = 1.35707 (10) nm, c = 1.77691 13) nm, α = 71.551 (2) °, β = 82.478 (2) °, γ = 80.568 (2) °. The crystal is composed of an inorganic covalent chain ∞1 [Nd (PW11O39) (H2O) 3] 4- and organic di-protonated 4,4’-dipyridyl (H2bpy) 2+ and crystal water molecules, Is a new rare earth phosphotungstic inorganic inorganic hybrid compounds.