Two novel thioindate-thioantimonate compounds [Ni(dien)(2)](2)In2Sb4S11 (1) and [Ni(dien)(2)](3)(In3Sb2S9)(2) center dot 2H(2)O (2) (dien = diethylenetriamine) have been solvothermally synthesized and structurally characterized. 1 contains heterometallic pseudosemicube [In2SbS8] clusters and bow-like trimeric [Sb3S7] units, which are linked to form a [In2Sb4S114-](n) chain, whereas 2 consists of chain-like [In6S18] units and pyramidal SbS3, which are interconnected to give a [In3Sb2S96-](n) layer with a large rectangle-like 12-ring. The optical properties of 1 and 2 have been investigated by UV-vis spectroscopy.