An anionic binuclear complex of tungsten(II), [(μ-Cl)3{W(SnCl3)(CO)3}2]−, and its reactivity towards norbornene

An anionic binuclear complex of tungsten(II), [(μ-Cl)3{W(SnCl3)(CO)3}2]− (1−), containing the protonated piperidine molecule [Hpip]+ as the counter ion, has been obtained during crystallization of the product from reaction between [W(CO)4(pip)2] and SnCl4 in dichloromethane solution, and its molecular structure has been elucidated by single-crystal X-ray diffraction studies. The chemical properties of complex 1 were investigated by IR and NMR spectroscopy in solution and its catalytic activity was checked in reaction with norbornene (NBE). In the presence of complex 1, NBE transformed to a new olefin, 2,2′-binorbornylidene with ca. 50% yield in dichloromethane solution. The spectroscopic characteristics of complex 1− were compared with those of the reinvestigated analogue compound [(μ-Cl)3W2(SnCl3)(CO)7] (2). The 119Sn and 13C NMR data indicated that in dichloromethane solution complex 2 transformed to the ionic complex 1−.An anionic binuclear complex of tungsten(II), [(μ-Cl)3{W(SnCl3)(CO)3}2]− (1−), containing the protonated piperidine molecule [Hpip]+ as the counter ion, has been obtained during crystallization of the product from reaction between [W(CO)4(pip)2] and SnCl4 in dichloromethane solution, and its molecular structure has been elucidated by single-crystal X-ray diffraction studies. The chemical properties of complex 1 were investigated by IR and NMR spectroscopy in solution and its catalytic activity was checked in reaction with norbornene (NBE). In the presence of complex 1, NBE transformed to a new olefin, 2,2′-binorbornylidene with ca. 50% yield in dichloromethane solution. The spectroscopic characteristics of complex 1− were compared with those of the reinvestigated analogue compound [(μ-Cl)3W2(SnCl3)(CO)7] (2). The 119Sn and 13C NMR data indicated that in dichloromethane solution complex 2 transformed to the ionic complex 1−.