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. 2021 Jun 4;60(12):8917–8923. doi: 10.1021/acs.inorgchem.1c00810

Scheme 1. Schematic Representation Showing the Synthesis of {X3W43} (X = SbIII and BiIII) and {Co3Sb3W42}.

Scheme 1

Taking the elevated potassium and acetate content as well as the use of a carboxylic acid and a X/W = 1:11 ratio as key parameters for the one-pot synthesis of {Bi3W43} into account, the step-by-step protocol for the synthesis of {Sb3W43} was designed. By using the nonlacunary {Sb2W22} Krebs archetype, which was prepared in a first step as a precursor together with l-malic acid in a KOAc/NaOAc (5% v/v) mixture, {Sb3W43} is obtained. Addition of {Sb3W43} to a CoCl2 solution in KOAc/NaOAc (5% v/v) leads to the formation of {Co3Sb3W42} in a consecutive reaction step. Black, turquoise, and red spheres represent the X = SbIII and BiIII, K+, and oxygen ions, respectively. Magenta and green transparent polyhedra represent {WVIO6} and {CoIIO6}.