The hydrolysis-condensation pathways of Mn2Sb4(OEt)16 in various ethanol-toluene solvents have been studied for h < 1.5 (h = H2O/Mn2Sb4(OEt)16). The hydrolysis was performed by slow addition of H2O diluted with the ethanol-toluene solvent. Mn2Sb4(OEt)16 and its hydrolysis products were studied by FT-IR spectroscopy, SEM-EDS and single-crystal X-ray diffraction. The hydrolysis pathway for a given h-value was found to depend on the solvent composition. In ethanol-rich solvent mixtures, Mn7Sb4O4(OEt)18(HOEt)2 was obtained in maximum yield at h = 1.14, and in toluene-rich solvents, Mn8Sb4O4(OEt)20 was obtained in maximum yield at h = 1.0. In both cases, the remaining Sb was found as nonhydrolyzed Sb(OEt)3. The structures of the heterometallic ethoxides Mn2Sb4(OEt)16, Mn7Sb4O4(OEt)18(HOEt)2 and Mn8Sb4O4(OEt)20 have been determined earlier by single-crystal X-ray diffraction. According to FT-IR evidence the molecular structures of the latter two are retained almost intact in solution, whereas the first one changes appreciably. The hydrolysis products of Mn2Sb4(OEt)16 are compared with those of Ni2Sb4(OEt)16, and the structural and compositional changes in different solvents and at different h-values are discussed.