Synthesis of[(C_5H_5)Y(η~2-PzMe_2)(μ-PzMe_2)]_2 and [Y(η~2-PzMe_2)_2(μ-PzMe_2)(μ-THF)]_2 and the insertion of Me_2SiO into the Y-N bond  

Synthesis of [(C_5H_5)Y(η~2-PzMe_2)(u-PzMe_2)]_2 and [Y(η~2-PzMe^2)~2(μ-PzMe_2)(μ- THF)]_2 and the insertion of Me_2SiO into the Y-N bond

作　　者：ZHOU Xigeng, ZHANG Libei, RUAN Ruyi, ZHANG Lixin , CAI Ruifang & WENG LinhongDepartment of Chemistry, Fudan University, Shanghai 200433, China State Key Laboratory of Elemental Organic Chemistry, Nankai University, Tianjin 300071, China 

出　　处：《Chinese Science Bulletin》2001年第9期723-726,共4页

基　　金：This work was supported by the National Natural Science Foundation of China (Grant No. 29872009); the Shanghai Shu-guang Foundation and the Open Laboratory of Organometallic Chemistry, the Chinese Academy of Sciences.

摘　　要：3,5-Dimethylpyrazole (HPzMe2) reacted with (C5H5)3Y in THF to yield dinuclear complexes [(C5H5)Y-(η2-PzMe2)(μ-PzMe2)]2 ( I ) and [Y(η2-PzMe2)2(μ-PzMe2)-(μ-THF)]2 (II), revealing a new method for synthesizing tris(pyrazolate) complexes of lanthanide metals. The X-ray crystallographic analysis showed that complex II crystallizes in space group P 1 , with unit cell dimensions a = 1.0798(1), b = 1.0818(1), c = 1.1313(1) nm, a = 76.914(2)°,(B = 68.940(2)°, γ= 60.510(2)°, V = 1.0715(2) nm3, Z = 1. The final R factor is 0.0445. The investigation results showed that Me2SiO can only be inserted into the Y-N (bridging) bond of complex I to form [(C5H5)Y(η2-PzMe2)(μ-OSiMe2 PzMe2)]2 (Ⅲ), but cannot be inserted into the Y-N (bridging) bond of complex II due to the bulky crowding of the tetraple bridge structure.3,5-Dimethylpyrazole (HPzMe2) reacted with (C5H5)3Y in THF to yield dinuclear complexes [(C5H5)Y-(η2-PzMe2)(μ-PzMe2)]2 (I) and [Y(η 2-PzMe2)2(μ-PzMe2)-(μ-THF)]2 (II), revealing a new method for synthesizing tris(pyrazolate) complexes of lanthanide metals. The X-ray crystallographic analysis showed that complex II crystallizes in space group P 1 , with unit cell dimensions a = 1.0798(1), b = 1.0818(1), c = 1.1313(1) nm, α= 76.914(2)°, β= 68.940(2)°, (R= 60.510(2)°, V = 1.0715(2) nm3, Z = 1. The final R factor is 0.0445. The investigation results showed that Me2SiO can only be inserted into the Y-N (bridging) bond of complex I to form [(C5H5)Y(η 2-PzMe2)(μ-OSiMe2 PzMe2)]2 (Ⅲ), but cannot be inserted into the Y-N (bridging) bond of complex Ⅱ due to the bulky crowding of the tetraple bridge structure.

关 键 词：YTTRIUM PYRAZOLATE crystal structure synthesis INSERTION cyclopentadienyl. 

分 类 号：O641.4[理学—物理化学]