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3,5-二甲基吡唑(HPzMe2)在THF溶液中和(C5H5)3Y反应,制得了双核钇配合物[(C5H5)-Y(η2-PzMe2)(μ-PzMe2)]2(I)和[Y(η2-PzMe2)2(μ-PzMe2)(μ-THF)]2(Ⅱ),后者揭示了一种合成三吡唑基稀土化合物的新方法.化合物11的X射线单晶衍射分析显示,该晶体属三斜晶系,空间群P1,晶胞参数: a= 1.079 8(1) n m, b= 1.081 8(1) nm, c= 1.1313(1) nm, a= 76.914(2)°,β= 68.940(2)°, γ=60.510(2)°,V=1.0715(2)nm3,Z=1.最后的一致性因子R=0.044 5.研究表明,由于四重桥结构的位阻太大,Me2SiO只能单插入化合物I中的Ln—N(桥)键,生成[(C5H5)Y-(η2-PzMe2)(μ-OSiMe2PzMe2)]2(Ⅲ),但不能插入化合物Ⅱ中的 Ln—N(桥)键.
(C5H5) -Y (η2-PzMe2) (μ-PzMe2)] 2 (I) was synthesized by the reaction of 3,5-dimethylpyrazole (HPzMe2) And [Y (η2-PzMe2) 2 (μ-PzMe2) (μ-THF)] 2 (Ⅱ) which revealed a new method for the synthesis of trispyrazole based rare earth compounds. The X-ray diffraction analysis of compound 11 showed that the crystal belongs to the triclinic system with space group P1 and unit cell parameters: a = 1.079 8 (1) n m, b = 1.081 8 (1) nm, a = 76.914 (2) °, β = 68.940 (2) °, γ = 60.510 (2) °, V = 1.0715 (2) nm3, Z = 1. The final concordance factor R = 0.044 5. The results show that due to the steric hindrance of tetrabasic bridge, Me2SiO can only insert the Ln-N (bridge) bond in compound I to generate [(C5H5) Y- (η2-PzMe2) (μ-OSiMe2PzMe2)] 2 (III), but not the Ln-N (bridge) bond in compound II.