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Flux Synthesis, Crystal Structures, and Solid-State NMR Spectroscopy of Two Indium Silicates Containing Varied In−O Coordination Geometries

Supporting Info

Ling-I Hung,^† Sue-Lein Wang,^‡ Hsien-Ming Kao,^† and Kwang-Hwa Lii*^†^§

Department of Chemistry, National Central University, Chungli, Taiwan 320, ROC, Department of Chemistry, National Tsing Hua University, Hsinchu, Taiwan 300, ROC, and Institute of Chemistry, Academia Sinica, Nankang, Taipei, Taiwan 115, ROC

Inorg. Chem., 2007, 46 (8), pp 3301–3305

DOI: 10.1021/ic0700349

Publication Date (Web): March 20, 2007

†

National Central University.

‡

National Tsing Hua University.

To whom correspondence should be addressed. E-mail: liikh@ cc.ncu.edu.tw.

Academia Sinica.

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) Å, b = 16.8849(3) Å, c = 10.2275(2) Å, V = 2157.1(1) Å³ and Z = 4; 2, monoclinic, P2₁/n (No. 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 and Z = 2.

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Published In Issue April 16, 2007
Received January 9, 2007

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Article

Flux Synthesis, Crystal Structures, and Solid-State NMR Spectroscopy of Two Indium Silicates Containing Varied In−O Coordination Geometries