LiSbS2-mC16: Structure Determination from X-ray Powder Diffraction Data
LiSbS2-mC16: Structure Determination from X-ray Powder Diffraction Data
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DOI：
10.1002/zaac.201400058
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发表时间：
2014-07
期刊：
影响因子：
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通讯作者：
Sebastian Huber;A. Pfitzner
中科院分区：
文献类型：
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作者：
Sebastian Huber;A. Pfitzner
以Li2S、Sb、S为原料，在900℃的温度下以1:2:5的比例固相反应合成单斜晶型LiSbS2-mC16。过量的硫作为一种助熔剂，不纳入结构。该产品对空气和水分敏感。用293k的x射线粉末衍射数据测定了深红色产物的晶体结构。LiSbS2-mC16在C2/c空间群中结晶。a = 8.0205(8) a, b = 7.9243(8) a, c = 6.6987(7) a, β = 126.303(6)°，V = 343.11(7) A3, Z = 4。它形成了有序的NaCl型上部结构，有两个不同的阳离子位置，而立方高温改性的cF8只有一个位置，锂和锑混合占据。锂的八面体配位与硫有轻微的扭曲。在锑的情况下，八面体配位多面体的畸变要强得多。因此，更恰当地描述为2 + 2 + 2的协调模式。
Monoclinic LiSbS2-mC16 was synthesized by solid-state reaction of Li2S, Sb, and S in the ratio 1:2:5 at a temperature of 900 °C. The excess of sulfur serves as a kind of flux and is not incorporated in the structure. The product is air and moisture sensitive. The crystal structure of the dark red product was determined from X-ray powder diffraction data at 293 K. LiSbS2-mC16 crystallizes in the space group C2/c (no. 15) with a = 8.0205(8) A, b = 7.9243(8) A, c = 6.6987(7) A, β = 126.303(6)°, V = 343.11(7) A3, and Z = 4. It forms an ordered NaCl type superstructure, which shows two different sites for the cations, whereas the cubic high temperature modification cF8 exhibits only one position with a mixed occupation by lithium and antimony. Lithium has a slightly distorted octahedral coordination by sulfur. The distortion of the octahedral coordination polyhedron is much stronger in the case of antimony. Therefore it is better described as a 2 + 2 + 2 coordination mode.