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Synthesis and Characterization of -[(C5H4SiMe2^tBu)2Ln(μ-S^nBu)]2 (Ln = Y,Er)
作者姓名:LI  Yan-Rong  ZHANG  Zheng-Xing  CHEN  Zhen-Xia  LIU  Rui-Ting  ZHOU  Xi-Geng
作者单位:Department of Chemistry Molecular Catalysis and Innovative Material Laboratory Fudan University,Department of Chemistry Molecular Catalysis and Innovative Material Laboratory Fudan University,Department of Chemistry Molecular Catalysis and Innovative Material Laboratory Fudan University,Department of Chemistry Molecular Catalysis and Innovative Material Laboratory Fudan University,Department of Chemistry Molecular Catalysis and Innovative Material Laboratory Fudan University,Shanghai 200433 China Shanghai 200433 China Shanghai 200433 China Shanghai 200433 China Shanghai 200433 China
基金项目:This work was supported by the National Natural Science Foundation of China (No. 20572014)
摘    要:(C5H4SiMe2^tBu)2Ln^nBu reacted with 1 equiv, of elemental sulfur in toluene at ambient temperature to yield the corresponding lanthanocene thiolates (C5H4SiMe2^tBu)2Ln(μ-S^nBu)]2 (Ln = Y (1), Er (2)). Complexes 1 and 2 have been characterized by elemental analysis, IR, mass spectroscopy and X-ray single-crystal diffraction analysis. Both complexes are of monoclinic with space group P21/c, formula C52H94S2Si4Y2 1 (C52H94S2Si4Er2 2) Mr = 1073.57 (1230.27), a = 8.495(2) (8.41(2)), b = 26.913(8) (26.67(7)), c = 13.756(4) (13.68(4)) A, α = 90(90), β = 101.184(5) (101.57(4)), γ = 90 (90)°, V= 3085.1(15) (3007(14)) A^3, Dc = 1.156 (1.359) g·cm^-3, Z= 2 (2), F(000) = 1144 (1260), μ = 2.046 (2.951) cm^-1, R = 0.0687 (0.0749) and wR = 0.1306 (0.1507) for observed reflections with I 〉 2σ(I). X-ray structures of 1 and 2 definitively prove that only one sulfur atom is inserted into the Ln-C(^nBu) bond, forming a thiolate ligand.

关 键 词:有机镧系元素  晶体结构  插入  硫磺  硫醇盐  合成  表征
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