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Two new gallium antimony sulfides,[enH2][Ga2Sb2S7]·en (1) and [puH]2[Ga2Sb2S7](2)(en=ethylenediamine,pu=propyleneurea),have been solvothermally synthesized. In the preparation of compound 2,the protonated propyleneurea cation as eounterion and template was in situ synthesized by the reaction of 1,3-diaminopropane with CO2 in pyridine. Both structures contain a two-dimensional network composed of novel heterometallic clusters of {Ga2Sb2Sg} as the seconddary building unit. The thermal and optical properties of compounds 1 and 2 were characterized by TGA and UV-Vis,respectively.