新颖五核Mo/Cu/S簇合物[MoOS3Cu4(α-MePy)6Br2]的合成及晶体结构

杂核金属含硫簇合物具有丰富的结构,在生物化学、催化和非线性光学等方面显示了诱人的应用前景.近年来,我们主要从事用MS4 ]2 - 和Cp* MS3]- ( M=Mo,W)和Cu( ) ,Ag( )反应合成Mo( W) /Cu( Ag) /S簇合物并研究其非线性光学性质1,2 ] .鉴于用硫代金属酸盐作前驱体合成M- Cu- Ag- S杂三核金属簇合物的工作鲜有报道3] ,我们尝试用( NH4 ) 2 Mo OS3和Cu Br,Ag Br在α- Me Py中反应,希望得到Mo- Cu- Ag- S杂三核金属簇合物.但上述反应却形成了1个仅含Mo和Cu( )的五核簇合物Mo OS3Cu4 (α- Me Py) 6 Br2 ],其所含的Mo S3…

Synthesis and Crystal Structure of a Novel Pentanuclear Mo/Cu/S Cluster Compound [MoOS3Cu4(α-MePy)6Br2]

Reaction of(NH4)2MoOS3 with CuBr and AgBr(molar ratio=1∶4∶1) in α-MePy produced dark red crystals of MoOS3Cu4(α-MePy)6Br2]. The product was characterized by elemental analysis, IR and X-ray diffraction. It crystallizes in a triclinic system with space group P1 and unit cell parameters a=0.950 9(3) nm, b=1.066 8(2) nm, c=2.153 6(3) nm, α=94.846(9)°, β=92.054(7)°, γ=99.299(8)°, V=2.145 5(8) nm3, Z=2, D c=1.828 g·cm-3, F(000)=1 168, μ=42.79 cm-1, R=0.049 and Rw=0.051. The compound consists of a nido-shaped MoS3Cu3 cluster unit and a four-membered CuBrCuS ring by sharing the same Cu3—S3 bond. The Mo atom and the four Cu atoms adopt a distorted tetrahedral geometry coordination. The Mo…Cu1, Mo…Cu2 and Mo…Cu3 distances are 0.271 1(3), 0 269 8(2), and 0.268 1(1) nm, respectively.