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化学学报
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化学学报 ›› 1989, Vol. 47 ›› Issue (9): 853-860. 上一篇    下一篇

研究论文

含金双硫螯合配体簇合物的研究 II: [Mo2Fe2(μ3-S)4(S2CNEt2)5]·CH3CN的合成, 结构和性质

徐吉庆;千吉松;魏诠;胡宁海;金钟声;卫革成   

  1. 吉林大学化学系;中国科学院长春应用化学研究所
  • 发布日期:1989-09-15

A study on the cluster compounds with all-dithio-chelate ligands II: Synthesis, structure and properties of [Mo2Fe2(μ3-S)4(S2CNEt2)5]·CH3CN

XU JIQING;QIAN JISONG;WEI QUAN;HU NINGHAI;JIN ZHONGSHENG;WEI GECHENG   

  • Published:1989-09-15

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在无氧非水介质中, 以(NH4)2MoS4, FeCl3和NaS2CNEt2为原料合成了簇合物[Mo2Fe2S4(S2CNEt2)5]·CH3CN。X射线单晶结构测定表明, 它具有[Mo2Fe2S4]^5^+类立方烷核心骨架。每个金属原子有一螯合基团S2CNEt2配位。第五个S2CNEt2基团在两个Mo原子间跨桥配位。XPS和Mossbauer谱的测定及M-S(M=Fe或Mo)键长比较表明, 簇合物中Fe原子的氧化态是不同的, 而两个Mo原子则具有相同的氧化态, 该簇合物为顺磁性物质, μm=4.27μs。此外, 还测定了它的红外光谱, 紫外-可见光谱和催化乙炔还原活性。

关键词: 紫外分光光度法, 晶体结构测定, 红外分光光度法, 铁络合物, 磁导率, 钼络合物, Ｘ射线光电子谱法, 氧化态, 簇状化合物, 硫络合物

In anaerobic and nonaq. system, the cluster [Mo2Fe2S4(S2CNEt2)5].MeCN (I) was prepared from (NH4)2MoS4, FeCl3 and NaS2CNEt2. I contains a [Mo2Fe2S4]5+ cubane-like core with a chelating ligand S2CNEt2 per metal atom, and both Mo atoms are bridged by the 5th S2CNEt2 group. XPS and Moessbauer spectral study and comparison of M-S (M = Fe or Mo) bond lengths show that both Fe atoms display different oxidation states, but both Mo atoms have the same oxidation state. The compound is paramagnetic matter, mm = 4.27 mB. In addition, IR, UV-visible spectra and catalytic activity of I in C2H2 reduction were also determine I is monoclinic, space group P21/c, a 19.397(7), b 10.891(7), c 24.302(8) ? b 108.95(2)? dc = 1.66 g cm-3, Z = 4, R = 0.045, Rw = 0.036.

Key words: ULTRAVIOLET SPECTROPHOTOMETRY, CRYSTAL STRUCTURE DETERMINATION, INFRARED SPECTROPHOTOMETRY, IRON COMPLEX, MAGNETIC PERMEABILITY, MOLYBDENUM COMPLEX, X-RAY PHOTOELECTRON SPECTROMETRY, OXIDATION STATE, CLUSTER COMPOUND, SULFIDE COMPLEX

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