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以碘化氮甲基喹啉和钼磷酸为原料合成了混合价化合物[C10 H10 N]4 PMo12 O4 0 ,在DMF溶液中用水蒸气扩散法进行了重结晶,得到了分子组成为[C10 H10 N]4 PMo12 O4 0 (CH3 )2 NH的晶体.测定了化合物的分子结构,属单斜晶系,空间群P2 1/n,a =14.846(4),b =12.5 0 8(2 ),c =1.75 89(3)nm,β =97.98(2)°,V =3.2 35 (1)nm3 ,Mr =2 44 4.10,Dcald=2.5 1g·cm-3 ,μ =2 3.15cm-1,F(0 0 0 ) =2 34 6,Z =2.结构由直接法解出.对 4375个可观察到的衍射点[(I>3σ(I))]进行最小二乘法修正后得R =0.0 6 0.阴离子具有Keggin结构,但还原后阴离子中的MoO6八面体在z-轴方向上伸长且Mo原子向Od原子移动大约 0.0 0 45nm.
A mixed valence compound [C10 H10 N] 4 PMo12 O4 0 was synthesized from iodine methylquinoline and molybdophosphoric acid by using water vapor diffusion method in DMF solution. The molecular composition of [C10 H10 N ] 4 PMo12 O4 0 (CH3) 2 NH. The molecular structure of the compound is determined and it belongs to the monoclinic system. The space group P2 1 / n, a = 14.846 (4), b = 12.5 0 8 = 1.75 89 (3) nm, β = 97.98 (2) °, V = 3.2 35 (1) nm3, Mr = 2 44 4.10, Dcald = 2.5 1 g · cm -3, μ = 2 3.15 cm -1, F 0 0 0) = 2 34 6, Z = 2. The structure is solved by the direct method. After the least squares correction of 4375 observable diffraction points [(I> 3σ (I) 0. The anions have a Keggin structure, but the MoO6 octahedrons in the anions after the reduction elongate in the z-axis direction and the Mo atoms move toward the Od atoms by about 0.0455 nm.