摘要
用新方法合成并测定了含W(O)的双核化合物(Et_4N)_2[(CO)_4W(μ—S)_2MoS_2](Ⅰ)和(Et_4N)_2[(CO)_4W(μ—S)_2WS_2)(Ⅱ)的晶体结构。Ⅰ和Ⅱ均属正交晶系,其空间群分别为PbCm和Pbam。Ⅰ的a=18.334(5),b=11.946(3),c=13.448(6),Z=4,R=0.057;Ⅱ的a=12.007(2),b=13.523(3),c=18.414(4),Z=4,R=0.058。Ⅰ和Ⅱ的阴离子均为以W(O)为中心的八面体和以Mo(Ⅵ)或(W)为中心的四面体共边且以μ—S连接,W(μ—S)_2M(M=Mo,W)共平面。其中W—Mo键距为2.964(3),W—W键距为3.0103(8),并发现其IR中M(O)—S_b键的ν在424.3～437.8cm^(-1)范围。
W ( O ) binuclear complexes (Et4N)2[(CO)4W(μ-S)2MoS2] ( Ⅰ ) and (Et4N)2[(CO)4W(μ-S)2WS2]D(Ⅱ) were synthesized with a new method, and their crystal structures were determined by X - ray crystallography. Ⅰ and Ⅱ Crystallize in the orthogonal system and the space group is Pbcm and Pbam, Ⅰ with a = 18. 334,b=11. 946,c = 13. 448A.Z = 4,R = 0. 057; Ⅱ with a = 12. 007,b = 13. 523,c = 18. 414A ,Z = 4,R = 0. 058. The structure of the anion of Ⅰ and Ⅱ is composed of an octahedron aroud the W(O) atom and a tetrahedron with the Mo( Ⅵ) or W(Ⅵ) atom in the center sharing an edge which is the line between the two bridged sulfur atoms. The bond distance of W-Mo is 2. 964(3) A and W -W is 3. 0103(8) A ,and the bimetallic center W (μ- S)2M (M = Mo. W) is planar. It was found in the IR spectrum of the complex Ⅱ that the absorption band of M(O)-Sb is v=424. 3-437. 8cm-1.
出处
《甘肃科学学报》
1992年第4期1-5,共5页
Journal of Gansu Sciences
关键词
合成
晶体结构
簇状化合物
钨
W(O)binuclear crusters,Synthesis,Crystal structure.
