新型含钒硒代锑酸盐化合物[V(1,2-dap)_2SbSe_3]的溶剂热合成与表征

Solvothermal synthesis and characterzation of novel selenidoantimonate compound containing vanadium[V(1,2-dap)_2SbSe_3]

利用溶剂热法成功合成了一种新型的硒代锑酸盐化合物[V(1,2-dap)2Sb Se3](1)(1,2-dap=1,2-丙二胺),并通过红外光谱、热重分析对该化合物进行了结构表征。单晶X-射线衍射结果显示:化合物属单斜晶系,P2(1)/c空间群,分子式为C6H20N4Sb Se3V,Mr=557.83,a=0.667 2(2)nm,b=1.745 9(6)nm,c=1.331 4(5)nm,β=98.898(7)°,V=1.532 4(10)nm3,Z=4,λ=0.071 073 nm,F(000)=1 040,Dc=2.418 mg/m3,μ=9.478 mm-1,R(F)=0.060 5,wR(F2)=0.127 0。该晶体是以过渡金属钒为中心,并由两个双齿1,2-丙二胺和一个双齿[Sb Se33-]共同配位得到的孤立零维结构。同时,晶体1又是首例由钒与硫属化物直接螯合的硒代锑酸盐。

A novel selenidoantimonate compound, [V（1,2-dap）2SbSe3] （1） （1,2-dap = 1,2-dianinopropane）, was solvothermally synthesized and characterized by IR and TGA. Single crystal X-ray diffraction revealed that the crystal structure was monoclinic in the space group P2 （ 1 ）/c. Crystallographic data was as follow： molecular formula=C6 H20 N4 SbSe3 V, Mr=557. 83, a=0. 667 2（2） nm, b=1. 745 9（6） nm, c=1. 331 4（5） nm,β=98. 898（7）o, V= 1. 532 4（10） nm^3,Z=4,λ=0. 071 073 nm, F（000）=104 0, Dc=2. 418 mg/m3, μ=9. 478 mm-1, R（F）=0. 060 5, wR（F2）=0. 127 0. The compound 1 was of isolated zero-dimensional（0D）structure, in which the existed V3＋ was chelated by two bidentate 1,2-dap molecules and one bidentate[SbSe33-]ligand. Meanwhlie, compound 1 was the first selenidoantimonate of vanadium with chalcogenide ligand.