Two gallium antimony sulfides, [Ni(en)(3)][Ga2Sb2S7] (1) and [(Me)(2)NH2](2)[Ga2Sb2S7] (2), have been prepared under mild solvothermal conditions. Both structures feature a two-dimensional network in which two GaS4 tetrahedra and two SbS3 trigonal pyramids are combined to form a heterometallic cluster of {Ga2Sb2S9} as a new secondary building unit. The thermal properties of 1 and 2 have been studied by thernogravimetric analysis, and the optical properties of 1 and 2 have been characterized by UV-vis spectra.