New routes are described for the preparation of cuboidal complexes [Mo3InS4(H2O)(12)](5+), [Mo3GaS4(H2O)(12)](5+), and [Mo6InS8(H2O)(18)](8+) from the incomplete cuboidal [Mo3S4(H2O)(9)](4+). A comparison of the aqueous solution properties of the single cubes, [Mo3GaS4(H2O)(12)](5+) and [Mo3InS4(H2O)(12)](5+), and the double cubes, [MO6InS8(H2O)(18)](8+) and [Mo6TlS8(H2O)(18)](8+), the total listing of group 13 derivatives, is reported. The single cube [Mo3InS4(H2O)(12)](5+) can be quantitatively converted into the double cube by reductive (H3PO2 or BH4-) addition of [Mo3S4(H2O)(9)](4+). The double cubes are O-2 sensitive, much more so in HCl than Hpts (pts(-) = p-toluenesulfonate), and are oxidized by H+ in HCl solutions with the formation of H-2 (detected by gas chromatography). The single cubes are less reactive in air, and are only oxidized by H+ at higher (similar to 4 M) levels. Stoichiometry measurements with [Co(dipic)(2)](-) and [Fe(H2O)(6)](3+) as le(-) oxidants were used to confirm charges on the clusters. In the absence of reduction potentials, rate constants for outer-sphere [Co(dipic)(2)](-) oxidations give a measure of redox properties. Oxidation of [Mo6InS8(H2O)(18)](8+) with [Co(dipic)(2)](-) provides a route back to the single cube [Mo(3)TnS(4)(H2O)(12)](5+). Properties of [W3InS4(H2O)(12)](5+) and [Mo6InO2S6(H2O)(18)](8+) obtained from [W3S4(H2O)(9)](4+) and [Mo3OS3-(H2O)(9)](4+) are also considered. The single cube [W3InS4(H2O)(12)](5+) is >10(3) times more reactive with [Co(dipic)(2)](-) than [Mo3InS4(H2O)(12)](5+), consistent with reducing properties W > Mo. No evidence was obtained in these studies for [Mo3TlS4 (H2O)(12)](5+), [Mo6GaS8(H2O)(18)](8+), or the recently proposed 6+ analogue of [Mo3GaS4(H2O)(12)](5+).