Zhang Shuzhuo, Wang Jing, Xu Yun
Department of Material Engineering Invention Examination, Patent Examination Cooperation Center of the Patent Office, SIPO, Beijing, People's Republic of China.
Acta Crystallogr Sect E Struct Rep Online. 2013 Oct 16;69(Pt 11):m605-6. doi: 10.1107/S160053681302583X.
The title compound, Na(C2H10N2)[Co(C2O4)(C2H8N2)2]4[H5(P2W18O62)2]·14H2O, prepared under hydro-thermal conditions, consists of two Dawson-type P2W18O62 anions, four isolated Co(en)2(ox) cations (en = ethyl-enedi-amine and ox = oxalate), one Na(+) cation, one H2en cation, and a number of ordered (14) and disordered solvent water mol-ecules. The P2W18O62 polyoxidometalate anion has site symmetry 1 and contains two structurally distinct types of W atoms: viz. six W atoms on vertical pseudo-mirror planes grouped in two sets of three, and 12 equatorial W atoms that do not lie in the pseudo-mirror planes grouped in two sets of six. In each Co(en)2(ox) cation, the Co(III) ion is coordinated by four N atoms from two en ligands and two O atoms from the ox ligands, completing a distorted octa-hedral structure. The sodium cation lies on an inversion centre and additionally links the complex cations and anions. In the crystal, the various units are linked by N-H⋯O and O-H⋯O hydrogen bonds, which together with C-H⋯O hydrogen bonds form a three-dimensional structure. The contribution of a region of disordered electron density, possibly highly disordered solvent water mol-ecules, to the scattering was removed with the SQUEEZE option of PLATON [Spek (2009 ▶). Acta Cryst. D65, 148-155]. To equilibrate the charges five H(+) ions have been added to the polyoxidometalate. These H(+) ions and the disordered solvent contribution were not included in the reported mol-ecular weight and density.
标题化合物Na(C₂H₁₀N₂)[Co(C₂O₄)(C₂H₈N₂)₂]₄[H₅(P₂W₁₈O₆₂)₂]·14H₂O是在水热条件下制备的,由两个道森型P₂W₁₈O₆₂阴离子、四个孤立的Co(en)₂(ox)阳离子(en = 乙二胺,ox = 草酸根)、一个Na⁺阳离子、一个H₂en阳离子以及一些有序(14个)和无序的溶剂水分子组成。P₂W₁₈O₆₂多金属氧酸盐阴离子具有点群对称性1,包含两种结构不同类型的W原子:即位于垂直假镜面上的六个W原子,分为两组,每组三个;以及12个赤道面W原子,它们不在假镜面上,分为两组,每组六个。在每个Co(en)₂(ox)阳离子中,Co(III)离子由来自两个en配体的四个N原子和来自ox配体的两个O原子配位,形成一个扭曲的八面体结构。钠阳离子位于一个对称中心上,此外还连接着复杂的阳离子和阴离子。在晶体中,各种单元通过N-H⋯O和O-H⋯O氢键相连,这些氢键与C-H⋯O氢键一起形成三维结构。利用PLATON的SQUEEZE选项[Spek (2009 ▶). Acta Cryst. D65, 148 - 155]去除了可能是高度无序的溶剂水分子的无序电子密度区域对散射的贡献。为了平衡电荷,向多金属氧酸盐中添加了五个H⁺离子。这些H⁺离子和无序的溶剂贡献未包含在报道的分子量和密度中。