The solid complex of HSb(SCH2COO)2 were synthesized through a reaction between antimony trioxide and thioglycollic acid in the aqueous solution . The complex was characterized with elemental analyses, infrared spectra, X-ray powder diffraction and X-ray crystal structure. The crystal structure of the compex belongs to monoclinic system, space group C2/c, with lattice parameters: a=1. 40005(8)nm, b=1.19121(8)nm, c=1.23588(8)nm, β=126.822(1)°, V=1.6499 (2)nm^3, Dc=2.439g·cm^-3, Z=8 and R1=0.0250. The antimony ion bonds directly to the sulfur atom of the thiohydroxy-group and the oxygen atom fo the carboxyl-group. There is not only the hydrogen bond of intermolecule, but also the coordination bonds of the antimony ion- sulfur or- oxygen atom of intermolecule. The results of indexes to the X-ray powder diffraction data for the complex are consistent with the results of single crystal.

Key words: ANTIMONY COMPLEX, MERCAPTO COMPOUNDS, CRYSTAL STRUCTURE, ELEMENTAL ANALYSIS, INFRARED SPECTROPHOTOMETRY, ANTIMONY OXIDE, MERCAPTOACETIC ACID