[η^5-Bz~5C~5(CO)~nM]~2的合成

本文通过η^5-Bz~5C~5MNa与氧化偶联试剂Fe~2(SO~4)~3/HOAC/H~2O的反应合成了含η^5-五苄基环戊二烯基配体的两个金属-金属单键化合物η^5-Bz~5C~5(CO)~3M]~2 (1: M=Mo; 2: M=W) , 产率分别为45%和19% . 1 在沸腾的甲苯中可进一步脱碳而以98%的产率生成金属-金属叁键化合物η^5-Bz~5C~5(CO)~2Mo]~2 (3).1～3的结构均经碳氢分析, IR, ^1H NMR 和MS鉴定. 3的结构尚被单晶X射线衍射分析确证 .

Syntheses and structures of dinuclear molybdenum and tungsten compounds containing η^5-pentabenzylcyclopentadienyl ligand [η^5-Bz~5C~5(CO)~nM]~2 (M=Mo, n=2,3; M=W, n=3)

Two metal-metal singly bonded compounds containing η^5-pentabenzlcyclopen tadienyl ligand η^5-Bz~5C~5(CO)~3M]~2 (1 M=Mo , 2 M=W) were synthesized in 45% and 19% yield through the reaction of η^5Bz~5C~5(CO)~3 M Na with a combined oxidative reagent Fe~2(SO~4)~3/HOAc/H~2O . Further decarbonylation of 1 in refluxing toluene gave the metal-metal triply bonded compound η^5-Bz~5C~5(CO)~2Mo]~2 (3) in 98% yield. The structures of 1～3 were characterized by C/H analysis IR, ^1H NMR and MS spectroscopies. The structure of 3 were characterized by C/H analysis IR,^1H NMR and MS spectroscopies. The structure of 3 was further confirmed by single-crystal X-ray diffraction analysis.