Wang Chih-Min, Liao Chia-Hsien, Kao Hsien-Ming, Lii Kwang-Hwa
Institute of Chemistry, Academia Sinica, Nankang, Taipei, Taiwan 115, ROC.
Inorg Chem. 2005 Sep 5;44(18):6294-8. doi: 10.1021/ic0507060.
A mixed-metal uranyl aquofluoride, [(UO2)2F8(H2O)2Zn2(4,4'-bpy)2].(4,4'-bpy), has been synthesized under hydrothermal conditions and has been structurally characterized by single-crystal X-ray diffraction, infrared spectroscopy, thermogravimetric analysis, emission spectroscopy, and solid-state NMR spectroscopy. It is one of the few uranium fluoride-organic framework solids in which an organic molecule is directly incorporated into the extended structure of the metal fluoride and is the first example of mixed-metal uranium oxyfluoride incorporating an organic ligand. The structure consists of neutral layers of edge- and corner-sharing uranium-centered pentagonal bipyramids and zinc-centered octahedra, which are linked through 4,4'-bpy ligands into a 3-D framework. The 1H MAS NMR spectrum is in support of the conclusion that the occluded 4,4'-bpy molecules in the structural channels are not protonated. Crystal data: monoclinic, space group P2(1)/c, a = 9.4630(5) A, b = 22.384(1) A, c = 16.7534(8) A, beta = 91.899(2) degrees , V = 3546.7(4) A(3) and Z = 4.
一种混合金属铀酰水氟化物[(UO₂)₂F₈(H₂O)₂Zn₂(4,4'-联吡啶)₂].(4,4'-联吡啶)已在水热条件下合成，并通过单晶X射线衍射、红外光谱、热重分析、发射光谱和固态核磁共振光谱对其结构进行了表征。它是少数几种有机分子直接并入金属氟化物扩展结构中的氟化铀-有机骨架固体之一，也是混合金属铀酰氟化物中包含有机配体的首个例子。该结构由以铀为中心的五角双锥体和以锌为中心的八面体通过边和角共享形成的中性层组成，这些层通过4,4'-联吡啶配体连接成三维骨架。¹H MAS NMR光谱支持结构通道中封闭的4,4'-联吡啶分子未质子化这一结论。晶体数据：单斜晶系，空间群P2(1)/c，a = 9.4630(5) Å，b = 22.384(1) Å，c = 16.7534(8) Å，β = 91.899(2)°，V = 3546.7(4) ų，Z = 4。
