SU-77: An Open-Framework Germanate Containing 12 脳 10 脳 10-Ring Channels Solved by Combining Rotation Electron Diffraction and Powder X-ray Diffraction

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• 作者：Liang Fang ; Leifeng Liu ; Yifeng Yun ; A. Ken Inge ; Wei Wan ; Xiaodong Zou ; Feifei Gao
• 刊名：Crystal Growth & Design
• 出版年：2014
• 出版时间：October 1, 2014
• 年：2014
• 卷：14
• 期：10
• 页码：5072-5078
• 全文大小：449K
• ISSN：1528-7505

文摘

A novel open-framework germanate, denoted as SU-77, was prepared by hydrothermal synthesis using ethylenediamine as the structure directing agent. The as-synthesized SU-77 is monoclinic with space group P2₁/a and a = 13.52427(5) 脜, b = 12.64862(5) 脜, c = 9.60578(3) 脜, 尾 = 92.8599(4)掳. The structure of SU-77 is built from a novel Ge₆O₁₇(C₂H₈N₂)F (Ge₆) cluster building unit. The Ge₆ clusters are connected to form chains along the c-axis. These chains are further connected in the [110] and [1鈥?0] directions to form a three-dimensional framework with 12 脳 10 脳 10-ring channels. The as-synthesized monoclinic SU-77 became orthorhombic while being observed in a transmission electron microscope (TEM) or when heated to 200 掳C in air. The orthorhombic structure of SU-77 was solved from micrometer-sized crystals by rotation electron diffraction (RED). The monoclinic structure was built from the orthorhombic structure and subsequently refined against synchrotron powder X-ray diffraction data. SU-77 is the first example of an open-framework germanate with mixed coordination polyhedra solved by electron diffraction.