一种新型硅酸铟K2In(OH)(Si4O10)的水热合成、晶体结构及固体核磁共振光谱

Hydrothermal synthesis, crystal structure, and solid-state NMR spectroscopy of a new indium silicate: K2In(OH)(Si4O10).

作者信息

Hung Ling-I, Wang Sue-Lein, Kao Hsien-Ming, Lii Kwang-Hwa

机构信息

Department of Chemistry, National Tsing Hua University, Hsinchu, Taiwan 300, R.O.C.

出版信息

Inorg Chem. 2003 Jun 30;42(13):4057-61. doi: 10.1021/ic020718a.

DOI:10.1021/ic020718a

PMID:12817961

Abstract

A new indium(III) silicate, K(2)In(OH)(Si(4)O(10)), has been synthesized by a high-temperature, high-pressure hydrothermal method. It crystallizes in the monoclinic space group P2(1)/m (No. 11) with a = 11.410(1) A, b = 8.373(1) A, c = 11.611(1) A, beta = 112.201(2) degrees, and Z = 4. The structure, which is analogous to that of K(2)CuSi(4)O(10), consists of unbranched vierer 4-fold chains of corner-sharing SiO(4) tetrahedra running along the b axis linked together via corner sharing by chains of trans-corner-sharing InO(4)(OH)(2) octahedra to form a 3-D framework which delimits 8-ring and 6-ring channels to accommodate K(+) cations. The presence of hydroxyl groups is confirmed by IR spectroscopy. The (29)Si MAS NMR exhibits four resonances at -88.6, -90.1, -97.4, and -98.2 ppm corresponding to four distinct crystallographic Si sites. A (1)H --> (29)Si CP/MAS NMR experiment was performed to assign the four resonances.

摘要

通过高温高压水热法合成了一种新型铟（III）硅酸盐K₂In(OH)(Si₄O₁₀)。它结晶于单斜空间群P2(1)/m（编号11），a = 11.410(1) Å，b = 8.373(1) Å，c = 11.611(1) Å，β = 112.201(2)°，Z = 4。其结构与K₂CuSi₄O₁₀的结构类似，由沿b轴延伸的由角共享SiO₄四面体组成的无分支四元4重链通过反角共享InO₄(OH)₂八面体链的角共享连接在一起，形成一个三维框架，该框架界定了8元环和6元环通道以容纳K⁺阳离子。通过红外光谱证实了羟基的存在。²⁹Si MAS NMR在-88.6、-90.1、-97.4和-98.2 ppm处表现出四个共振峰，对应于四个不同的晶体学Si位点。进行了¹H→²⁹Si CP/MAS NMR实验以确定这四个共振峰。