Synthesis and Characterization of Cs4Ga6Q11 (Q = S, Se): Chalcogenometalates with Exotic Polymeric Anions

被引：2
|
作者：
Friedrich, Daniel [1 ]
Greim, Dominik [2 ]
Schlosser, Marc [1 ]
Siegel, Renee [2 ]
Senker, Juergen [2 ]
Pfitzner, Arno [1 ]
机构：
[1] Univ Regensburg, Inst Anorgan Chem, Univ Str 31, D-93040 Regensburg, Germany
[2] Univ Bayreuth, Lehrstuhl Anorgan Chem 3, D-95440 Bayreuth, Germany
来源：
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION | 2018年 / 57卷 / 49期
关键词：
azide route; chalcogenogallates; NMR spectroscopy; quantum-chemical calculations; semiconductors; ONE-DIMENSIONAL INDIUM; SINGLE-CRYSTAL GROWTH; STRUCTURAL-CHARACTERIZATION; SOLVOTHERMAL SYNTHESIS; PHYSICAL-PROPERTIES; HEXASODIUM DI-MU-THIO-BIS(DITHIOGALLATE); TERNARY CHALCOGENIDES; ELECTRONIC-STRUCTURE; X-RAY; GALLIUM;
D O I：
10.1002/anie.201805239
中图分类号：
O6 [化学];
学科分类号：
0703 ;
摘要：
Two new chalcogenogallates Cs(4)Ga(6)Q(11) (Q = S, Se) were obtained by a controlled thermal treatment of CsN3 in the presence of stoichiometric amounts of Ga(2)Q(3) and the elemental chalcogens at elevates temperatures. Both isotypic compounds crystallize in the space group P (1) over bar (no. 2). The most prominent structural feature in these chalcogenogallates are the complex anionic Dreier double chains (1)(infinity)[Ga(6)Q(11)(4-)] formed by condensed GaQ(4) tetrahedra. The semiconductors Cs4Ga6S11 (E-g = 3.14 eV) and Cs4Ga6Se11 (E-g = 2.41 eV) were further studied by using UV/Vis, Cs-133 and Ga-71 solid-state NMR spectroscopy, and complementary DFT calculations. The Cs-133 MAS NMR spectra are characteristic for cationic cesium and vibrational spectra show two distinct regions, attributed to the Ga-Q valence and deformation vibrations, respectively. High-temperature studies revealed incongruent melting of both solids, which is also depicted in updated binary phase-diagrams Cs(2)Q-Ga(2)Q(3) (Q = S, Se).
引用
收藏
页码：16210 / 16214
页数：5
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