The complex of N′-methyl-N-piperazinly-carbodithioato-S,S′-antimony(III) was synthesized with the raw materials of carbon bisulfide, N-methyl-piperazinly and antimonous oxide in chloroform. The composition and structure of the complex was characterized by chemical and elemental analysis, Fourier transformed infrared spectra (FTIR), X-ray powder diffraction (XRD) and thermal analysis. The results show that the composition of the complex is [Sb(S2CNC4H8NCH3)3]?H2O, the ligand is coordinated simultaneity with Sb(III) via the sulphur atoms of dithiocarbamate to form bidentate chelates. The effects of reaction temperature, reaction time and different solvent on the yield were discussed respectively. The results showed that the yield of the complex was maximal when chloroform was used as the solvent at 25 ℃ for 1 hour, the mixed solvent of chloroform-methanol was chose in recrystallization, and the yield was 74%.