Three new tetramolybdenum organophosphonate compounds, (NH4)7{FeIII[MoVI2O6CH3C(O)(PO3)2]2}·10H2O 1, (NH4)4[Na(H2O)6]{CrIII[MoVI2O6CH3C(O)(PO3)2H]2}·7.67H2O 2 and (NH4)8{MnII[MoVI2O6CH3C(O)(PO3)2]2}·9H2O 3 have been successfully synthesized by reacting metal-containing oxidants Fe2(C2O4)3, MnO4− and CrO42− with a simple aqueous solution containing {MoV2O4(H2O)6}2+, respectively, in the presence of (hydroxylethylidene) diphosphonic acid. These compounds are characterized by elemental analyses, spectroscopic methods (IR, UV-Vis, XPS), TG-DTA, single-crystal X-ray diffraction analyses (including bond valence sum calculations) and powder X-ray diffraction analysis. Single crystal X-ray diffraction analyses have revealed that Mo–Mo bonds of {MoV2O4(H2O)6}2+ are cleavaged in the oxidation reaction to form {MoVI2O6} motifs, which are concomitantly stabilized by organophosphate and linked by the resulted metal ions coming from the metal-containing oxidants and bring on the formation of compounds 1–3, whose anions have a general formula {M[MoVI2O6CH3C(O)(PO3)2]2}n−(M = FeIII1; CrIII2; MnII3). It is important that the successful synthesis and characterization of the three new compounds induces a simple yet general strategy which can be utilized for the preparation of polyoxomolybdenum(VI) organophosphonates through oxidative Mo–Mo bond cleavage with various metal-containing oxidants like FeIII, MnVII and CrVI in the presence of various organophosphonates.
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