Synthesis and characterization of Ni2Sb4(OEt)16 and its hydrolysis products

Abstract

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 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.