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将MoCl_3·3H_2O溶于无水乙醇中,加入适量的P_2S_5,产物用乙腈重结晶,获得四核钼原子簇化合物{Mo_4(μ_3-S)_3(μ_3-O)[S_2P(OEt)_2]_6}·3CH_3~CN。晶体属三方晶系,空间群为R3;晶胞系数:a=b=c=12.852(3) ;α=β=γ=108.37(2)°;V=1697.3 ~3;Z=1;D_c=1.693g·cm~(-3)。用Patterson法解出结构,并经全矩阵最小二乘法修正,偏离因子为0.072。结构分析表明,由四个钼原子组成的四面体及三个μ_3-S原子,一个μ_3-O原子形成类立方烷型的簇骼,结构中存在六个表观的键序平均为5/6的Mo—Mo键,键长分别为2.700(1)和2.831(1) 。
MoCl_3 · 3H_2O was dissolved in absolute ethanol, and the appropriate amount of P_2S_5 was added. The product was recrystallized from acetonitrile to obtain the tetranuclear molybdenum cluster {Mo_4 (μ_3-S) _3 (μ_3-O) [S_2P (OEt) _2] _6 } · 3CH_3 ~ CN. The crystal belongs to the trigonal system with a space group of R3. The unit cell coefficient is: a = b = c = 12.852 (3); α = β = γ = 108.37 (2) °; V = 1697.3-3; Z = 1; 1.693g · cm ~ (-3). The structure was solved by the method of Patterson method, and corrected by full matrix least square method, the deviation factor was 0.072. The structural analysis shows that the tetragonal and three μ_3-S atoms consist of four molybdenum atoms and one μ_3-O atom forms a carbanion-like cluster. There are six apparent bond sequences in the structure with an average of 5/6 Of the Mo-Mo bond length of 2.700 (1) and 2.831 (1).