Synthesis and crystal structure of a novel germanate: (NH4)4[(GeO2)3(GeO1.5F3)2].0.67H2O.
Synthesis and crystal structure of a novel germanate: (NH4)4[(GeO2)3(GeO1.5F3)2].0.67H2O.
复制标题
新型锗酸盐的合成和晶体结构：(NH4)4[(GeO2)3(GeO1.5F3)2].0.67H2O。
作者：
T. Conradsson;Xiaodong Zou;M. Dadachov
以二氧化锗、吡啶、氢氟酸和2，6-二氨基吡啶为模板剂，在水溶液中合成了新型微孔锗酸盐（NH 4）4[（GeO 2）3（GeO1.5F3）2].0.67H2O。将溶液在165 ℃下在特氟隆衬里的高压釜中保持4天。通过X射线粉末衍射、FTIR、热分析和元素分析，制备并研究了大晶体。通过单晶X射线衍射确定了其结构。晶体为正交晶系，空间群Pbcn，a = 7.0065（4）A，B = 11.7976（6）A，c = 19.5200（14）A，Z = 4。该结构是由GeO 4四面体和GeO 3F 3八面体单元组成的层状骨架。多面体单元以这样的方式连接，使得它们形成具有三元环和九元环的沸石状多孔结构。一半的铵离子位于九元环内。另一半在三元环的上方和下方。锗多面体单元的连通性被插入层之间的铵离子和水分子沿c轴沿着中断。
The novel microporous germanate (NH4)4[(GeO2)3(GeO1.5F3)2].0.67H2O was prepared from an aqueous solution containing germanium dioxide, pyridine, hydrofluoric acid, and 2,6-diaminopyridine as a template. The solution was kept at 165 degrees C in a Teflon-lined autoclave for 4 days. Large crystals were produced and studied by X-ray powder diffraction, FTIR, thermal analysis, and elemental analysis. The structure was determined by single-crystal X-ray diffraction. The crystal is orthorhombic, space group Pbcn, with a = 7.0065(4) A, b = 11.7976(6) A, c = 19.5200(14) A, and Z = 4. The structure is a layered framework built up from GeO4 tetrahedral and GeO3F3 octahedral units. The polyhedral units are connected in such a way that they form a zeolite-like porous structure with three- and nine-membered rings. Half of the ammonium ions are located inside the nine-membered rings. The other half are above and below the three-membered rings. The connectivity of the germanium polyhedral units is interrupted along the c axis by ammonium ions and water molecules inserted between the layers.