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Issue 14, 2012
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A general synthesis approach in action: preparation and characterization of polyoxomolybdenum(vi) organophosphonates through oxidative Mo–Mo bond cleavage in {MoV2O4}

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Abstract

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.

Graphical abstract: A general synthesis approach in action: preparation and characterization of polyoxomolybdenum(vi) organophosphonates through oxidative Mo–Mo bond cleavage in {MoV2O4}

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Article information


Submitted
18 Jan 2012
Accepted
25 Apr 2012
First published
26 Apr 2012

CrystEngComm, 2012,14, 4826-4833
Article type
Paper

A general synthesis approach in action: preparation and characterization of polyoxomolybdenum(VI) organophosphonates through oxidative Mo–Mo bond cleavage in {MoV2O4}

L. Zhang, J. Sun, Y. Zhou, S. ul Hassan, E. Wang and Z. Shi, CrystEngComm, 2012, 14, 4826
DOI: 10.1039/C2CE25093D

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