两种具有不同铟 - 氧配位几何结构的硅酸铟的通量合成、晶体结构及固态核磁共振光谱研究

Flux synthesis, crystal structures, and solid-state NMR spectroscopy of two indium silicates containing varied In-O coordination geometries.

作者信息

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

机构信息

Department of Chemistry, National Central University, Chungli, Taiwan 320, ROC.

出版信息

Inorg Chem. 2007 Apr 16;46(8):3301-5. doi: 10.1021/ic0700349. Epub 2007 Mar 20.

DOI:10.1021/ic0700349

PMID:17371016

Abstract

Two novel indium silicates, K5In3Si7O21 (1) and K4In2Si8O21 (2), have been synthesized by a flux-growth method and characterized by single-crystal X-ray diffraction. The structure of 1 consists of siebener single chains of corner-sharing SiO4 tetrahedra running along the b axis linked via corner-sharing by In2O9 face-sharing octahedral dimers and InO5 trigonal bipyramids to form a 3D framework. The structure of 2 consists of a 3D silicate framework containing 6- and 14-ring channels. InO5 square pyramids are located within the 14-ring channels sharing corners with the silicate framework. The solid-state 29Si MAS NMR spectrum of compound 1 was recorded; it shows the influence of the indium atoms in the second coordination sphere of the silicon on the chemical shift. Crystal data: 1, orthorhombic, Pna21 (No. 33), a = 12.4914(3) A, b = 16.8849(3) A, c = 10.2275(2) A, V = 2157.1(1) A3 and Z = 4; 2, monoclinic, P21/n (No. 14), a = 8.4041(3) A, b = 11.4919(4) A, c = 10.4841(3) A, beta = 90.478(2) degrees , V = 1012.5(1) A3 and Z = 2.

摘要

通过助熔剂生长法合成了两种新型铟硅酸盐K5In3Si7O21（1）和K4In2Si8O21（2），并通过单晶X射线衍射对其进行了表征。化合物1的结构由沿b轴延伸的由共角SiO4四面体组成的七元单链构成，这些单链通过In2O9共面八面体二聚体和InO5三角双锥共角连接，形成三维骨架。化合物2的结构由一个包含6元和14元环通道的三维硅酸盐骨架组成。InO5方锥位于14元环通道内，与硅酸盐骨架共角。记录了化合物1的固态29Si MAS NMR谱；该谱显示了硅的第二配位球中的铟原子对化学位移的影响。晶体数据：1，正交晶系，Pna21（编号33），a = 12.4914(3) Å，b = 16.8849(3) Å，c = 10.2275(2) Å，V = 2157.1(1) Å3，Z = 4；2，单斜晶系，P21/n（编号14），a = 8.4041(3) Å，b = 11.4919(4) Å，c = 10.4841(3) Å，β = 90.478(2)°，V = 1012.5(1) Å3，Z = 2。