The AAAc(1 ~ 1) was synthesized in water by As2Os and Sb203 with molar ratio of 1 ' 1. AAAc(1 ." 1) was characterized by Raman, IR, TG/DTG, DSC, XPS and XRD. The results show that there are four peaks to vs of As--OH, As--O--Sb, Sb--OH and Sb--O--Sb in Raman spectra of AAAc(1 : 1) at 100 -1 000 em -1. The solution of AAAc(1 ~ 1) was also titrated with KOH solution. The titration results show that AAAc(1 : 1) is a hexabasic acid with dissociation constants of kl = 3.62 × 10 -2 , k2 = 3.05 )< 10 -3 , k3 = 6.43 × l0 -s , k4 = 9.78 ;< 10 -s , ks = 1.32 × 10 -n , ks = 3.87 )< 10 -12. AAAc(1 : 1) has a good solubility and stability in water, its solid obtained by free volatilizing water from its solution under air at ambient temperature is amorphous. Chemical and thermal analysis show that the composition of AAAc(1 ." 1) is As3Os • Sb2Os • 8H30 in air at 25 °C. AAAc(1 , 1) has the structure of AsO (OH)2--OH--Sb (OH)~--O--Sb (OH)4--OH--AsO (OH)3 or As (OH)3--O--Sb(OH)4--O--Sb(OH)4--O--As(OH)3 (isomerism) through experimental determination and geometry optimization.