Syntheses and Structures of Molybdenum(IV) Complexes with 3,5-Dimethyl- and 3,5-Di-<i>tert</i>-butylpyrazolato Ligands. Variable Coordination Modes and C−H Bond Activation
作者:Kerstin Most、Nadia C. Mösch-Zanetti、Denis Vidović、Jörg Magull
DOI:10.1021/om034076q
日期:2003.12.1
Treatment of tetrakis(dimethylamido)molybdenum(IV) (Mo(NMe2)4) with 4 equiv of 3,5-dimethylpyrazole (Me2pzH) in pentane yields Mo(Me2pzH)(Me2pz)3(η2-CH2NHCH3) (1), whereby the reaction with 3,5-di-tert-butylpyrazole (t-Bu2pzH) leads to Mo(t-Bu2pz)3(NMe2) (2), independent of the molar ratio. The homoleptic Mo(t-Bu2pz)4 (3) was synthesized from tetrachlorobis(tetrahydrofurano)molybdenum(IV) (MoCl4(thf)2)
四处理(二甲氨基)钼(IV)(钼(NME 2)4)与4当量3,5-二甲基的(ME 2的戊烷PZH)得到的Mo(ME 2 PZH)(ME 2 PZ)3(η 2 -CH 2 NHCH 3)(1),由此与3,5-二-反应叔-butylpyrazole(吨-Bu 2 PZH)导致的Mo(吨-Bu 2 PZ)3(NME 2)(2),独立摩尔比。均相Mo(t -Bu 2 pz)由四氯双(四氢呋喃)钼(IV)(MoCl 4(thf)2)与4当量的3,5-二叔丁基吡唑并钾(t- Bu 2 pzK)合成4(3)。磁性测量显示三个络合物是顺磁性的两个未成对电子(1,3.0; 2,2.8;和3,2.8 μ乙,分别地)。报告了通过X射线衍射分析确定的所有化合物的分子结构。复杂1揭示了η 2 -协调CH 2 NHCH 3配体以氮杂金属环的方式排列,通过较小的Mo-C-N角和典型的CN单键长度进行验证。所述配体pyr