SYNTHESIS AND CHARACTERIZATION OF NI2SB4(OET)16 AND ITS HYDROLYSIS PRODUCTS

The hydrolysis pathways of Ni2Sb4(OEt)16 in toluene, ethanol and toluene-ethanol mixtures have been studied. Five intermediate compounds have been isolated from solutions having different H2O/Ni2Sb4(OEt)16 ratios (h values) with h<6. A detailed description of the routes used in connection with the preparation of Ni2Sb4(OEt)16 and of the five intermediates, Ni5Sb3O2(OEt)15(HOEt)4, Ni7Sb4O4(OEt)18, Ni6Sb4O4(OEt)16(HOEt)4, NiSb3O3(OEt)5 and Ni6Sb14O18(OEt)18(HOEt)2 are given. The composition of three of the intermediates compounds have been established from single-crystal structural studies. The suggested compositions of the two others, Ni7Sb4O4(OEt)18 and NiSb3O3(OEt)5, are based on elemental analysis. The chemical compositions of the sol and of the gel formed for h greater-than-or-equal-to 6, NiSb2O3(OEt)2, are estimated from chemical considerations. A brief investigation of the hydrolysis pathways of Sb(OEt)3 in the same solvents is also included.