Reactions of Ph2SbCl3 with RSi(OH)3 [where R = tert-Bu, cyclo-C6H11] and Ph2Si(OH)2 in toluene in the presence of triethylamine as a base were performed. Single-crystal X-ray structural elucidation of the products revealed the formation of hexanuclear antimony(V) and mixed-valent antimony (III/V) oxo-hydroxo clusters built up of an incomplete cubane subunit. Interestingly, in all the reactions, at least one Sb-C bond cleavage has been observed, leading to the formation of novel cluster assemblies [(Ph2Sb)4(PhSb)2(C4H9SiO3)2(O)6(OH)2] (1), [(Ph2Sb)4(PhSb)2(C6H11SiO3)2(O)6(OH)2] (2), [(Ph2Sb)(PhSb)2(Ph2SiO2)2(O)3(OH)2](-)Et3NH(+) (3), and [(Ph2Sb)4(Sb)2(Ph2SiO2)2(O)6(OH)2] (4), respectively.
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