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首页> 外文期刊>International Journal of Quantum Chemistry >AMORPHOUS PRECURSORS FOR LOW-TEMPERATURE PREPARATION OF CHEVREL PHASES M(X)MO(6)S(8) AND THEIR TUNGSTEN ANALOGUES
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AMORPHOUS PRECURSORS FOR LOW-TEMPERATURE PREPARATION OF CHEVREL PHASES M(X)MO(6)S(8) AND THEIR TUNGSTEN ANALOGUES

机译：雪佛兰相M（X）MO（6）S（8）的低温制备及其钨类似物的非晶态前兆

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High-yield preparations of the amorphous ternary salts Na-2x(Mo6S8)Sx . yMeOH (with x = 1.0 to 1.5, y = 4 to 5) and Na-2.1 (W6S8)S-1.05. 5.4MeOH have been devised by reaction of M(6)Cl(12) (M = Mo or W) with NaSH and NaOBu in various ratios in refluxing n-BuOH for M = Mo and in refluxing MeCN for M = W. Characterization of these amorphous materials by chemical and spectroscopic methods (IR, Raman, PES) shows that the (M(6)S(8))(0) cluster units are present. Vacuum thermolysis of the amorphous Na-2x(Mo6S8)S-x . yMeOH first produces poorly crystalline NaMo6S8 by disproportionation at 800 degrees C and well-crystallized NaMo6S8 at greater than or equal to 900 degrees C. The amorphous tungsten compound disproportionates to W and WS2 at greater than or equal to 200 degrees C. Ion exchange of the sodium material in methanol with soluble M(2+) and M(3+) salts (M = Sn, Co, Ni, Pb, La, Ho) produces the M(2x)(n+)(Mo6S8)S-x . yMeOH compounds. For tungsten, only exchange with SnCl2 in THF was examined and resulted in Sn-x change with SnCl2 in THF was examined and resulted in Sn-x (W6S8)S-x . yMeOH. Conversion of Sn-x(Mo6S8)S-x . yMeOH to poorly crystalline Chevrel phase, SnMo6S8, was achieved by reduction under H-2 at 600 degrees C. Well-crystallized SnMo6S8 resulted at higher temperatures. Conversion of Sn-x(W6S8)S-x . yMeOH to SnW6S8 was not successful. (C) 1995 Academic Press, Inc. [References: 21]
机译：非晶态三元盐Na-2x（Mo6S8）Sx的高产率制备。 yMeOH（x = 1.0至1.5，y = 4至5）和Na-2.1（W6S8）S-1.05。通过将M（6）Cl（12）（M = Mo或W）与NaSH和NaOBu以不同的比例在回流的正丁醇中将M = Mo和在回流的MeCN中将M = W反应来设计5.4MeOH。这些无定形材料通过化学和光谱方法（IR，Raman，PES）表明存在（M（6）S（8））（0）簇单元。真空热解无定形Na-2x（Mo6S8）S-x。 yMeOH首先通过在800摄氏度歧化产生结晶度差的NaMo6S8，并在大于或等于900摄氏度结晶出良好结晶的NaMo6S8。在大于或等于200摄氏度时非晶态钨化合物歧化为W和WS2。含有可溶性M（2+）和M（3+）盐（M = Sn，Co，Ni，Pb，La，Ho）的甲醇中的钠材料可生成M（2x / n）（n +）（Mo6S8）Sx。 yMeOH化合物。对于钨，仅检查了与在THF中的SnCl 2的交换，并检查了与在THF中的SnCl 2的Sn-x变化，并检查了Sn-x（W6S8）S-x。甲醇。 Sn-x（Mo6S8）S-x的转换。通过在600°C下在H-2下还原将yMeOH转变为结晶度不佳的Chevrel相SnMo6S8。结晶度较高的SnMo6S8在较高的温度下产生。 Sn-x（W6S8）S-x的转换。 yMeOH转化为SnW6S8失败。 （C）1995 Academic Press，Inc. [参考：21]

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