Molecular oxo-hydroxo clusters have been synthesized by reactions of arylstibonic acids with organophosphonic acid and phenylseleninic acid. Single crystal X-ray structural elucidation revealed the formation of [(p-i-PrC6H4Sb)4(OH)4(t-BuPO3)6] (1), [(p-t-BuC6H4Sb)4(O)2(PhPO3)4(PhPO3H)4] (2), [(p-i-PrC6H4Sb)4(O)3(OH)(PhSeO2)2(t-BuPO3)4(t-BuPO3H2)2] (3), [(p-MeC6H4Sb)4(O)3(OH)(PhSeO2)2(t-BuPO3)4(t-BuPO3H2)2] (4) and [(p-t-BuC6H4Sb)2(O) (PhSeO2)2(t-BuPO3H)4] (5) respectively. Mass spectral studies reveal that the clusters maintain their structural integrity in solution as well. Solution NMR studies (1H, 31P and 77Se) show spectral patterns which correlate well with the observed solid state structures of 1–5.
