簇合物〔WOS_3 Ag_3 Br(PPh_3)_3〕·(OPPh_3)的合成和晶体结构

Synthesis and Crystal Structure of 〔WOS_3Ag_3Br(PPh_3)_3〕·(OPPh_3)

报道了〔WOS3Ag3Br(PPh3) 3〕·(OPPh3)簇合物 (C72 H6 0 Ag3BrO2 S3P4W ,Mr=176 4.6 1)单晶的合成和结构。该晶体属于三方晶系 ,空间群为R3 ,晶胞参数 :a =16 .14 0 (3) ,c =2 3 .0 0 3(4) ,V =5 189.4(15 ) 3,μ(MoKα) =3 .2 98mm- 1 ,Z =3 ,F(0 0 0 ) =2 5 98,Dc=1.6 94g/cm3。独立衍射点 2 181,可观察衍射点 195 2 (I≥ 2σ(I) ) ,R =0 .0 496 ,wR =0 .12 48。该晶体由簇合物分子〔WOS3Ag3Br(PPh3) 3〕和以P为中心的扭曲四面体结构的中性分子OPPh3 构成 ,其中的簇合物分子的骨架为由1个W原子、3个S原子、3个Ag原子和 1个Br原子构成的立方烷状。W、O(1)和Br原子位于C3轴上。

The title compound 〔WOS 3Ag 3Br(PPh 3) 3〕·(OPPh 3)was synthesized and the structure was determined by X ray diffraction. The crystal belongs to the trigonal system with space group R3. The cell parameters are a=16.140(3), c=23.003(4) , V=5189.4(15)  3 , μ (Mo Kα )=3.298mm -1 , Z=3, F(000)=2598, D c =1.694g/cm 3。 Final R and wR are 0.0496 and 0\^1248 respectively for 1952 ( I≥2σ(I )) observed reflections. The crystal molecule consists of 〔WOS 3Ag 3Br(PPh 3) 3〕 and OPPh 3, where 〔WOS 3Ag 3Br(PPh 3) 3〕 is cubane like skeletoned by one W atom , three S atoms , three Ag atoms and one Br, and OPPh 3 is of a distorted tetrahedron structure with P at the center. The W, O(1) and Br atoms are located on the c 3 axis.