无机-有机杂化层状锑硫化合物的溶剂热合成与结构

Solvothermal synthesis and structure of an inorganic-organic hybrid thioantimonate with layered structure

用溶剂热法合成了有机杂化层状锑硫化合物[C3H7NH3]2Sb4S7,并利用单晶X-射线衍射测定了其晶体结构。该化合物为三斜晶系,Pī空间群。晶胞参数:a=7.0098(10),b=11.9710(14),c=13.6685(17),α=115.244(6)°,β=98.671(9)°,γ=92.413(13),°V=1018.3(2)3,Z=2,Mr=831.71 g.mol-1,(=5.984 mm-1,F(000)=772,偏差因子R1=0.0334,wR2=0.0766。该化合物由质子化正丙胺离子[C3H7NH3]+和二维阴离子[Sb4S7]n2n-组成,[Sb4S7]n2n-二维离子由3个SbS3三角锥和1个SbS4变形四面体单元连接而成,[C3H7NH3]+离子位于无机阴离子层之间,形成三明治夹心式结构,[C3H7NH3]+的-NH3+基团与无机阴离子层的S原子形成N-H…S氢键作用。

An novel inorganic-organic hybrid thioantimonate（Ⅲ） [C3H7NH3]2Sb4S7 was synthesized solvothermally and characterized by X-ray single-crystal diffraction.It crystallizes in triclinic crystal system space group Pī,with a=7.0098（10）,b=11.9710（14）,c=13.6685（17）,α=115.244（6）°,β=98.671（9）°,γ=92.413（13）°,V =1018.3（2）3,Z=2,Mr=831.71 g.mol^-1,μ=5.984 mm^-1,F（000）=772,R1=0.0334,wR2=0.0766.It consists of [C3H7NH3]^＋ cations and two-dimensional inorganic [Sb4S7]n^2n-anion,which is composed of three SbS3 trigonal pyramids and one SbS4 tetrahedron.The protonated n-propylamine cations interdigitate in a bilayer and reside in the 2D channels leading to a sandwich-like arrangement of the thioantimonate anion and the cations.The-NH＋3 group of [C3H7NH3]^＋ contacts with inorganic layers by the intermolecular N-H… S hydrogen bonds.