含SR桥的双核钼(Ⅰ)配合物Mo_2(CO)_(8-n)(SR)_2L_n的新合成途径和Mo_2(CO)_6(SPh)_2(MeCN)_2的结构研究  

New Route to Synthesize Dinuclear Mo (I) Complexes, Mo_2 (CO)_8-n(μ-SR)_2L_n and Structure of Mo_2 (CO)_6 (μ-SPh)_2 (CH_3CN)_2

作　　者：庄伯涛[1] 黄梁仁[1] 何玲洁[1] 杨瑜[1] 卢嘉锡[1] 

机构地区：[1]中国科学院福建物质结构研究所

出　　处：《化学学报》1989年第1期25-30,共6页Acta Chimica Sinica

基　　金：国家自然科学基金;中国科学院基金

摘　　要：经由零价双核钼含SR桥的配合物的氧化反应合成了一系列含各种SR桥的双核钼(Ⅰ)配合物Mo_2-(CO)_(8-n)(μ-SR)_2L_n[R=Bu^t,Ph,Bz(C_6H_5CH_2),CH_2CO_2Et;L=MeCN,PPh_3;n=0,2]。并应用红外光谱、元素分析等进行表征,讨论了新的合成途径。[含MeCN配位体配位到Mo(Ⅰ)上的配合物,Mo_2(CO)_6(SPh)_2(MeCN)_2经X射线结构测定,系属单斜晶系,空间群P2_1/c,a=9.241(2),b=9.330(3),c=15.458(4)A:β=105.77(2)°;V=1283(1)A^3;Z=2;R=0.033。Mo—Mo距离为2.978A,表明其Mo-Mo键的形成,Mo-S键长为2.469A。比较同系物Mo_2(CO)_8(μ-SCH_2CO_2-Et)_2,Mo_2(CO)_6(μ-SCH_2CO_2Et)_2(MeCN)_2和Mo_2(CO)_8(μ-SBu^t)_2的结构,并讨论其结构与化学。A series of dinuclear Mo (I) complexes containing SR bridges, Mo_2(CO)_(8-n) (μ-SR)_2- L_n[R=Ph, Bu^t, Bz (C_6H_5CH_2), CH_2CO_2Et; L= MeCN, PPh_3; n=0, 2], have been synthesized by oxidation of dinuclear Mo(0) complexes containing SR bridges with iodine and characterized by elemental analysis, infrared spectroscopy and X-ray crystallography. New route to synthesize these Mo (I) complexes has been discussed. The crystal and molecular structure of the complex, Mo_2(CO)_6(μ-SPh)_2(MeCN)_2 was determined from three-dimensional X-ray data. It crystallizes in tho monoclinic, space group P2_1/c, a=9.241(2), b=9.330(3) c=15.458(4)A; β=105.77(2)°; V=1283(1)A^3; Z=2; R=0.033 for 1628 reflections with I>3σ (I). The distance of Mo —— Mo is 2.978A indicating formation of Mo--Mo bond, and the distance of Mo--S bond is 2.469A. In comparison with its analogs Mo_2 (CO)_8 (μ-SCH_2CO_2Et)_2, Mo_2(CO)_3 (μ-SBu^t)_2 and Mo_2(CO)_6(μ-SCH_2CO_2Et)_2(MeCN)_2, the structure relevant to its chemistry was discussed.

关 键 词：SR桥基 双核钼配合物 X线检查 

分 类 号：O611.662[理学—无机化学]