Germanium-containing, extra-large pore molecular sieve CIT-13 is synthesized without the use of fluoride. After the removal of occluded organics, CIT-13 obtained from fluoride-free preparation shows significant differences from CIT-13 samples prepared in the presence of fluoride. CIT-13 prepared using a fluoride-free method is able to undergo inverse sigma transformation to yield CIT-14 and transforms into a CIT-5-type germanosilicate much faster than Ge-CIT-13 of similar Si/Ge ratios from a fluoride-containing synthesis. A Rietveld-refined structure solution for CIT-14 reveals that this new molecular sieve possesses 12- and 8-membered ring channels. Results from ¹⁹F magic-angle spinning (MAS) and ¹H–²⁹Si cross-polarized MAS nuclear magnetic resonance spectroscopy reveal that CIT-13 crystallized without fluoride has germanium siting which is different from CIT-13 synthesized in the presence of fluoride.

中文翻译：

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锗硅酸盐CIT-13的无氟合成及其反Sigma转化形成CIT-14

含锗超大孔分子筛CIT-13的合成无需使用氟化物。除去被封堵的有机物后，从无氟制剂获得的CIT-13与在氟化物存在下制备的CIT-13样品有显着差异。使用无氟化物的方法制备的CIT-13能够进行反sigma转换以生成CIT-14，并且比具有类似Si / Ge比的Ge-CIT-13的氟化物转化成CIT-5型锗硅酸盐的速度要快得多。包含合成。Rietveld改进的CIT-14结构解决方案表明，这种新的分子筛具有12和8元环通道。从结果¹⁹ ˚F魔角旋转（MAS）和¹ H- ²⁹Si交叉极化MAS核磁共振波谱表明，没有氟化物结晶的CIT-13的锗位置与在氟化物存在下合成的CIT-13不同。