通过在水和乙醇混合物中以1:5的摩尔比在0°C下将1-甲基-4-[(三甲氧基锗基)甲基]哌嗪(8)与氢氟酸反应,制备了带有分子式λ6Ge-锗酸盐五氟[(4-甲基-1,4-双偶氮环己基)甲基]锗酸盐(5)并以水合物5·H2O的形式分离。这个带有偶极性的分子5由一个六配位(形式上是双负电荷)的锗原子和两个四配位(形式上是正电荷)的氮原子组成。化合物5·H2O通过单晶X射线衍射进行了结构表征。晶体数据如下:C6H17F5GeN2O,三斜晶系空间群P1̄(2),a=7.5228(11) Å,b=12.174(2) Å,c=12.3041(14) Å,α=73.74(2)°,β=82.44(2)°,γ=74.762(10)°,V=1041.7(2) Å3,T=173(2) K,Z=4,R1=0.0227。在不对称单元中有一对晶体学独立的带偶极性的分子5和水分子,其结构非常相似。它们在锗原子周围的配位多面体略有扭曲。
The zwitterionic (molecular) λ6Ge-germanate pentafluoro[(4-methyl-1,4-bisazoniacyclohexl-yl)methyl]germanate (5) was synthesized by reaction of 1-methyl-4-[(trimethoxygermyl) methyl]piperazine (8) with HF (molar ratio 1:5) in a mixture of water and ethanol at 0 °C and isolated as the hydrate 5 · H2O. The zwitterion 5 is characterized by the presence of a hexacoordinate (formally twofold negatively charged) germanium atom and two tetracoordinate (formally positively charged) nitrogen atoms. Compound 5 · H2O was structurally characterized by single-crystal X-ray diffraction. Crystal data are as follows: C6H17F5GeN2O , triclinic space group P1̄ (no. 2), a = 7.5228(11) Å, b = 12.174(2) Å, c = 12.3041(14) Å, α = 73.74(2)°, β = 82.44(2)°, γ = 74.762(10)°, V = 1041.7(2) Å3, T = 173(2) K, Z = 4, R1 = 0.0227. There are one pair each of crystallographically independent zwitterions 5 and water molecules in the asymmetric unit, the structures of the zwitterions being very similar. Their coordination polyhedra around the germanium atoms are slightly distorted octahedra.
通过在水和乙醇混合物中以1:5的摩尔比在0°C下将1-甲基-4-[(三甲氧基锗基)甲基]哌嗪(8)与氢氟酸反应,制备了带有分子式λ6Ge-锗酸盐五氟[(4-甲基-1,4-双偶氮环己基)甲基]锗酸盐(5)并以水合物5·H2O的形式分离。这个带有偶极性的分子5由一个六配位(形式上是双负电荷)的锗原子和两个四配位(形式上是正电荷)的氮原子组成。化合物5·H2O通过单晶X射线衍射进行了结构表征。晶体数据如下:C6H17F5GeN2O,三斜晶系空间群P1̄(2),a=7.5228(11) Å,b=12.174(2) Å,c=12.3041(14) Å,α=73.74(2)°,β=82.44(2)°,γ=74.762(10)°,V=1041.7(2) Å3,T=173(2) K,Z=4,R1=0.0227。在不对称单元中有一对晶体学独立的带偶极性的分子5和水分子,其结构非常相似。它们在锗原子周围的配位多面体略有扭曲。