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Synthesis and Structural Characterization of a Dimolybdenum Complex Bridged by the Hydroxymethylphenylphosphinate Ligand

Journal of Chemical Crystallography volume 41, pages 1317–1322 (2011)Cite this article

Abstract

Hydroxymethylphenylphosphinic acid, 1 was synthesized and structurally characterized by single crystal X-ray diffraction. Ligand 1 crystallized in the monoclinic P21 space group with two molecules comprising the unit cell and cell dimensions a = 7.5587(13) Å, b = 5.9019(8) Å, c = 8.808(3) Å and β = 90.90(2)°. Molecules were linked up by hydrogen bonding involving all three oxygen atoms of 1 resulting in 2-dimensional sheets. Reacting 1 with MoO2Cl2 in a mixture of ethanol and dichloromethane afforded the dinuclear molybdenum complex Mo2O4Cl2[(HOCH2)PhPOO]2, 2 where the two molybdenum atoms were bridged by the phosphinate ligand. Complex 2 crystallized in the P21/C space group as a dietherate with a = 9.208(3) Å, b = 14.353(4) Å, c = 12.805(4) Å and β = 98.64(3)° and contained terminal O and Cl atom disorder. The two crystallographically identical molybdenum centers are in distorted octahedral environments. Complexes were analyzed by IR, 31P NMR and X-ray crystallography.

Graphical Abstract

The reaction of hydroxymethylphenylphosphinic acid with MoO2Cl2 in a mixture of ethanol and dichloromethane afforded the dinuclear molybdenum complex Mo2O4Cl2[(HOCH2)PhPOO]2, 2 where the two molybdenum atoms were bridged by the phosphinate ligand.

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Acknowledgement

We thank Michigan Technological University for financial support.

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Authors and Affiliations

  1. Department of Chemistry, Michigan Technological University, 1400 Townsend Drive, Houghton, MI, 49931, USA

    Linsheng Feng & Rudy L. Luck

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  1. Linsheng Feng
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  2. Rudy L. Luck
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Correspondence to Rudy L. Luck.

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Feng, L., Luck, R.L. Synthesis and Structural Characterization of a Dimolybdenum Complex Bridged by the Hydroxymethylphenylphosphinate Ligand. J Chem Crystallogr 41, 1317–1322 (2011). https://doi.org/10.1007/s10870-011-0096-5

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  • DOI: https://doi.org/10.1007/s10870-011-0096-5

Keywords

  • Hydroxymethylphenylphosphinic acid
  • Dioxomolybdenum
  • Molybdenum dimers
  • Hydrogen bonding

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