Interaction of potassium antimony(III) tartrate hydrate K2(SbC4H2O6)2·3H2O with the trilacunary Keggin derivatives [A-α-XW9O34]10− (X = SiIV, GeIV) and [A-α-PW9O34]9− in aqueous acidic medium (pH 4.8) resulted in three novel polyanions, [Sb3(A-α-XW9O34)2]11− (X = SiIV (1), GeIV (2)) and [Sb6O2(A-PW6O26)(A-α-PW9O34)2]15− (3), which were isolated as the hydrated potassium salts K11[Sb3(A-α-XW9O34)2]·31H2O (X = SiIV (K-1), GeIV (K-2)) and the mixed potassium–sodium salt K14Na[Sb6O2(A-PW6O26)(A-α-PW9O34)2]·61H2O (KNa-3) salts, respectively, and characterized by single-crystal X-ray diffraction, IR spectroscopy, as well as elemental and thermogravimetric analyses. The SbIII-containing polyanions 1–3 possess unique structural features, as they represent the first examples of sandwich-type POMs with trigonal-pyramidal SbIIIO3 linkers. The stability of 1–3 in aqueous media was investigated by multinuclear (183W, 31P) NMR and UV-Vis spectroscopy.
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