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用新方法合成并测定了含Mo(0)的双核化合物(Et_4N)_2[(CO)_4Mo(μ-S)_2MOS_2](Ⅰ)和(Et_4N)_2[(CO)_4Mo(μ-S)_2WS_2](Ⅱ)的晶体结构.Ⅰ和Ⅱ空间群均为Pbcm,Ⅰ的a=1.8403(2)nm,b=1.1963(1)nm,c=1.3482(1)nm,Z=4,R=0.042;Ⅱ的a=1.8453(2)nm,b=1.2004(2)nm,c=1.3494(3)nm,Z=4,R=0.032,Ⅰ和Ⅱ的阴离子均为以Mo(0)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,Mo(μ-S)2M(M=Mo,W)共平面.其中Mo—Mo键距为0.2992(2)nm,Mo—W为0.30330(8)nm,并发现其Fourier IR中Mo(0)-Sb键的v=424.3 cm~-1。
A new method was used to synthesize and measure the dinuclear compounds (Et_4N) _2 [(CO) _4Mo (μ-S) _2MOS_2] (I) and (Et_4N) _2 [(CO) _4Mo (μ-S) _2WS_2 ] (Ⅱ). The space group Ⅰ and Ⅱ are all Pbcm, with Ⅰ = 1.8403 (2) nm, b = 1.1963 (1) nm, c = 1.3482 (Ⅱ), a = 1.8453 (2) nm, b = 1.2004 (2) nm, c = 1.3494 (3) nm, Z = 4 and R = Octahedron and Mo (Ⅵ) (or W) centered tetrahedra and connected by μ-S, Mo (μ-S) 2M (M = Mo, W) 0.2992 (2) nm and Mo-W 0.30330 (8) nm. The v = 424.3 cm ~ (-1) of Mo (0) -Sb bond in Fourier IR was found.