Interrupted silicogermanate with 10-ring channels: synthesis and structure determination by combining rotation electron diffraction and powder X-ray diffraction,Inorganic Chemistry Frontiers

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Interrupted silicogermanate with 10-ring channels: synthesis and structure determination by combining rotation electron diffraction and powder X-ray diffraction
Inorganic Chemistry Frontiers ( IF 6.1 ) Pub Date : 2017-08-02 00:00:00 , DOI: 10.1039/c7qi00309a
Yilin Wang _{1,

2,

3,

4,

5} , Yunchen Wang _{6,

7,

8,

9,

10} , Jie Su _{6,

7,

8,

9,

10} , Xiaowei Song _{1,

2,

3,

4,

5} , Wei Wan _{6,

7,

8,

9,

10} , Jihong Yu _{1,

2,

3,

4,

5}

Affiliation

Silicogermanate (JU110) with an interrupted open-framework has been synthesized by using a hydrothermal method using 1,1′-(1,4-phenylenebis(methylene))bis(1-methylpyrrolidin-1-ium) hydroxide as an organic structure-directing agent (OSDA). Silicon and fluoride anions were introduced to the concentrated-gel synthesis system, and different synthetic parameters influencing the synthesis were discussed. The structure of JU110 was characterised by using rotation electron diffraction (RED) and high-resolution powder X-ray diffraction. JU110 crystallizes in the space group Fm2m (No. 42) with a = 13.9117(2) Å, b = 18.2980(3) Å and c = 32.7800(6) Å. The structure is constructed by the sti layers found in the STI framework that are pillared by D4R/Ge₇ units to form a large cavity, showing 10-ring openings along [100] and 9-ring openings along [110]. Thermal stability studies showed that the framework was maintained with the loss of water molecules, but collapsed with the removal of charge-compensating cations.

中文翻译：

具有10个环通道的间断硅锗酸盐：结合旋转电子衍射和粉末X射线衍射的合成和结构确定

通过使用1,1'-（1,4-亚苯基双（亚甲基））双（1-甲基吡咯烷-1-基）氢氧化物作为有机结构的水热法合成了具有间断开放骨架的硅锗锗酸盐（JU110）-导向剂（OSDA）。将硅和氟阴离子引入到浓缩凝胶合成系统中，并讨论了影响合成的不同合成参数。JU110的结构通过旋转电子衍射（RED）和高分辨率粉末X射线衍射进行了表征。JU110在a = 13.9117（2），b = 18.2980（3），c = 32.7800（6）的空间群Fm 2 m（No. 42）中结晶。该结构由在由D4R / Ge ₇单元支撑的STI框架形成一个大空腔，在[100]上显示10个环的开口，在[110]上显示9个环的开口。热稳定性研究表明，骨架保留了水分子的丢失，但由于去除了电荷补偿阳离子而崩溃了。

更新日期：2017-08-22

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