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.
出处
《化学学报》
SCIE
CAS
CSCD
北大核心
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
