Targeted synthesis of a polypyridyl polyoxometalate coordination complex using microwave-assisted reaction conditions

Jingjing Xu, Robert W. Gable, Chris Ritchie

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Abstract

In this article, we build upon our recent efforts that have focused on demonstrating the value of microwave-assisted synthesis in polyoxometalate (POM) chemistry. Herein, we report for the first time a microwave-assisted approach that enabled the facile preparation and crystallization of a large POM-containing coordination complex. The judicious selection and reaction of a sparingly water-soluble transition-metal-substituted polyanion (TMSP) salt with the tritopic ligand 2,4,6-tris(4-pyridyl)-1,3,5-triazine (TPT) in a mixed solvent system under moderately forcing conditions yields Ba9[(BIIIWVI 11O39CoIII)3(C18H12N6)]·38H2O in moderate yield. Crystallographic analysis reveals significant intermolecular interactions between the organic ligand and neighbouring polyanions, predominantly C—H…O(water) in nature; meanwhile, the solvated regions of the crystal show significant disorder. To supplement the crystallographic study, combustion analysis, and IR and 1H NMR spectroscopic analyses were conducted, revealing good bulk purity and the stability of the complex in aqueous media.

Original languageEnglish
Pages (from-to)1384-1389
Number of pages6
JournalActa Crystallographica Section C: Structural Chemistry
Volume74
Issue number11
DOIs
Publication statusPublished - 1 Nov 2018
Externally publishedYes

Keywords

  • crystal structure
  • microwave-assisted synthesis
  • polydentate ligand
  • polyoxometalate
  • POM
  • pyridyl
  • spectroscopy
  • transition metal

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