Selenidoantimonate[Fe（en）3（Hen）]SbSe4（en=ethylenediamine） was solvothermally synthesized by a reaction on FeCl2·4H2O,Sb and Se in en at 140℃.It crystallizes in triclinic crystal system space group Pī,with a=8.8755（15）,b=9.6315（18）,c=14.251（3）,α=104.756（3）°,β=92.65（3）°,γ=109.587（4）°,V=1098.2（3）3,Z=2,Mr=734.86 g.mol-1,Dc.=2.222 g.cm-3,μ=8.526 mm-1,F（000）=700,R1=0.0236,wRw=0.0522.The crystal structure consists of tetrahedral 3- anion,octahedral [Fe（en）3]2+complex cation and protonated + cation.A three-dimensional supramolecular network is formed by the intermolecular N-H...Se and N-H...N hydrogen bonds between anions and cations.The crystal band gap is at 2.52 eV.On heating,the compound losses organic components in two steps under N2 atmospere.
