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一种具有三元环和七元环的新型有机模板开放骨架锆锗酸盐的合成与表征

Synthesis and characterization of a novel organically templated open framework zirconogermanate with three- and seven-membered rings.

作者信息

Liu Zhicheng, Weng Linhong, Chen Zhenxia, Zhao Dongyuan

机构信息

Laboratory of Molecular Catalysis and Innovative Materials, Department of Chemistry, Fudan University, Shanghai 200433, P. R. China.

出版信息

Inorg Chem. 2003 Sep 22;42(19):5960-5. doi: 10.1021/ic0343612.

Abstract

A new organically templated microporous zirconogermanate, (C(2)H(10)N(2))H(2)O[ZrGe(3)O(9)] (denoted as FDZG-3), with a low framework density of 13.6 T/1000 A(3), has been solvo/hydrothermally synthesized by using ZrO(NO(3))(2).2H(2)O as a zirconium source and triethylenetetramine (TETA) as a structure direct agent. This compound was characterized by means of single-crystal X-ray diffraction analysis, thermogravimetrical analysis, and IR and UV-vis spectra. Its three-dimensional (3D) framework is built up by 1D sinusoidal germanate chains cross-linked by ZrO(6) octahedra, which forms a network containing three- and seven-membered rings (MRs). Four intersecting 7-MR channels can be observed along the b axis, c axis, [110], and [-110] directions, respectively. Charge-balancing (C(2)H(10)N(2))(2+) and extraframework water molecules are encapsulated within 7-MR channels and form hydrogen bonds with framework oxygen atoms. Crystal data for FDZG-3: M = 533.13, monoclinic, space group Cc (No.9), a = 11.299(3) A, b = 7.7649(19) A, c = 13.835(3) A, beta = 104.826(3) degrees, V = 1173.4(5) A(3), Z = 4, R1 = 0.0263, wR2 = 0.0529.

摘要

一种新型的有机模板微孔锆锗酸盐(C₂H₁₀N₂)H₂O[ZrGe₃O₉](记为FDZG - 3),其骨架密度低至13.6 T/1000 ų,已通过以ZrO(NO₃)₂·2H₂O作为锆源、三乙烯四胺(TETA)作为结构导向剂,采用溶剂热/水热法合成。该化合物通过单晶X射线衍射分析、热重分析以及红外和紫外可见光谱进行了表征。其三维(3D)骨架由通过ZrO₆八面体交联的一维正弦锗酸盐链构成,形成了一个包含三元环和七元环(MRs)的网络。沿b轴、c轴、[110]和[-110]方向分别可观察到四个相交的七元环通道。电荷平衡的(C₂H₁₀N₂)²⁺和骨架外水分子被包裹在七元环通道内,并与骨架氧原子形成氢键。FDZG - 3的晶体数据:M = 533.13,单斜晶系,空间群Cc(编号9),a = 11.299(3) Å,b = 7.7649(19) Å,c = 13.835(3) Å,β = 104.826(3)°,V = 1173.4(5) ų,Z = 4,R1 = 0.0263,wR2 = 0.0529。

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