新型钼-氧簇化合物Ni(en)_3MoO_4的水热合成及表征

Hydrothermal syntheses and structure characterization of a new molybdenum-oxygen cluster Ni(en)_3MoO_4

采用水热方法合成一种新型钼-氧簇化合物Ni(en)3MoO4,并通过X射线单晶结构分析、红外光谱分析、元素分析、差热热重分析对该化合物进行了表征.结构分析数据表明:该化合物属三方晶系,P-31c空间群,晶胞参数a=0.9226(13)nm,b=0.9226(13)nm,c=0.9959(2)cm,α=90°,β=90°,γ=120°,V=0.7342(2)nm3,Z=2,Dc=1.805mg/m3,μ=2.153mm-1,F(000)=408,R=0 0553,Rw=0.1732;该化合物是分立结构,是由MoO4四面体簇和Ni(en)3八面体簇形成,其中MoO4四面体簇和Ni(en)3八面体簇交替排列,存在较强的氢键作用,结构中分立的手性配合物Ni(en)3的两种对映体构象以MoO4簇为中心对称排布.

A new molybdenum-oxygen cluster Ni(en)_3MoO_4 have been hydrothermally synthesized and characterized by the methods of X-ray single crystal structure analysis,ICP,IR,and TGA-DTA analysis.The results of structure analysis indicated that the title compound is trigonal system, P -31c group,with a =0.922 6(13) nm, b =0.922 6(13) nm,( c =0.995 9(2) cm,) α =90°, β =90°, γ =120°, V =0.734 2(2) nm^3, Z =2, D_c =1.805 (mg/m^3,) μ =2.153 mm^(-1),F(000)=408, R =0.055 3, R_w =0.173 2.The structure of the compound is consisted of MoO_4 tetrahedra cluster and Ni(en)_3 octahedra cluster,which these clusters are absolute and connected with hydrogen bonds.The enantiomers of the chiral metal complex Ni(en)_3 are separated symmetrically as two chiral configurations by MoO_4 clusters.