新型双核二甲基氨基-3,5-二甲基吡唑基和四核二甲基氨基-3,5-二甲基吡唑基-多氧锆（IV）配合物。合成与结构表征。

Novel dinuclear dimethylamido-3,5-dimethylpyrazolato and tetranuclear dimethylamido-3,5-dimethylpyrazolato-polyoxo zirconium(IV) complexes. Synthesis and structural characterisation.

作者信息

Sanz Martial, Mosquera Marta E G, Cuenca Tomás

机构信息

Departamento de Química Inorgánica, Universidad de Alcalá, Facultad de Farmacia, Campus Universitario, E-28871, Alcalá de Henares, Spain.

出版信息

Dalton Trans. 2009 Apr 14(14):2616-22. doi: 10.1039/b817574h. Epub 2009 Feb 18.

DOI:10.1039/b817574h

PMID:19319407

Abstract

The dinuclear dimethylamido-tris(3,5-dimethylpyrazolato)-zirconium(IV) complex [Zr(3,5-Me2Pz)3(NMe2)]2 1 is prepared by treatment of [Zr(NMe2)4] with 3 equivalents of 3,5-dimethylpyrazole (3,5-Me2PzH) with elimination of dimethylamine. When [Zr(NMe2)4] reacted with 2 equivalents of 3,5-Me2PzH, the bis(dimethylamido)-bis(3,5-dimethylpyrazolato)zirconium(IV) compound [Zr(3,5-Me2Pz)2(NMe2)2]2 2 is obtained. Hydrolysis of [Zr(3,5-Me2Pz)3(NMe2)]2 in wet toluene affords the tetranuclear oxo compound [Zr4(eta2-3,5-Me2Pz)4(NMe2)2(mu3-O)2(mu2-3,5-Me2Pz)4(mu2-NMe2)2] . All synthesised compounds are characterised by NMR spectroscopic and analytical methods. Single crystal X-ray diffraction analysis has established the molecular structures of 1 and 4.

摘要

通过用3当量的3,5 - 二甲基吡唑（3,5 - Me₂PzH）处理[Zr(NMe₂)₄]并消除二甲胺，制备了双核二甲基氨基 - 三（3,5 - 二甲基吡唑基） - 锆（IV）配合物[Zr(3,5 - Me₂Pz)₃(NMe₂)]₂ 1。当[Zr(NMe₂)₄]与2当量的3,5 - Me₂PzH反应时，得到双（二甲基氨基） - 双（3,5 - 二甲基吡唑基）锆（IV）化合物[Zr(3,5 - Me₂Pz)₂(NMe₂)₂]₂ 2。在湿甲苯中[Zr(3,5 - Me₂Pz)₃(NMe₂)]₂水解得到四核氧代化合物[Zr₄(η² - 3,5 - Me₂Pz)₄(NMe₂)₂(μ₃ - O)₂(μ₂ - 3,5 - Me₂Pz)₄(μ₂ - NMe₂)₂] 。所有合成的化合物都通过核磁共振光谱和分析方法进行了表征。单晶X射线衍射分析确定了1和4的分子结构。