Abstract:Two compounds of antimony trichloride and bismuth trichloride with valine are synthesized by solid phase synthesis at room temperature. Their compositions, determined by element analysis, are Sb(C5H10O2N)3·2H2O and Bi(C5H10O2N)2Cl·0.5H2O . The crystal structure of antimony complex with valine belongs to triclinic system and its lattice parameters are: a= 0.959 9 nm,b=1.506 8 nm, c=1.985 1 nm,α=92.27°,β=95.05°,γ=104.27°. The crystal structure of bismuth complex with valine belongs to monoclinic system and its lattice parameters are: a=1.601 2 nm, b=1.894 1 nm, c=1.839 nm,β=99.73°. The far-infrared spectra and the infrared spectra show that the amino group and carboxyl of valine may be coordinated to antimony and bismuth, respectively, in two compounds. The TG-DSC results also reveal that the complexes are formed.