Hydrothermal synthesis and characterization of the tri-capped and mono-supported pseudo-Keggin-type tungstovanadophosphate: {l_brace}PW{sub 4}{sup VI}W{sub 5}{sup V}V{sub 3}{sup IV}O{sub 40}(V{sup IV}O){sub 3}[Cu(en){sub 2}]{r_brace}{sup 6-}
- College of Chemistry and State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, Jilin University, Jilin Province, Changchun 130021 (China)
A novel polyoxometalate [Cu(phen){sub 2}]{sub 3}{l_brace}PW{sub 4}{sup VI}W{sub 5}{sup V}V{sub 3}{sup IV}O{sub 40}(V{sup IV}O){sub 3}[Cu(en){sub 2}]{r_brace}.4H{sub 2}O 1 (en=ethylenediamine, phen=1,10-phenanthroline) has been synthesized hydrothermally and characterized by elemental analysis, IR, XPS, TG, EPR and single-crystal X-ray diffraction analysis. The crystal structure analysis shows that compound 1 contains a novel highly reduced tri-capped and mono-supported pseudo-Keggin-type heteropolyanion, {l_brace}PW{sub 4}{sup VI}W{sub 5}{sup V}V{sub 3}{sup IV}O{sub 40}(V{sup IV}O){sub 3}[Cu(en){sub 2}]{r_brace}{sup 6-}, three [Cu(phen){sub 2}]{sup 2+} cations and four lattice water molecules. They are further linked to form three-dimensional supramolecular networks through extensive hydrogen bonding and {pi}-{pi} stacking interactions. Interestingly, the water dimer and terminal oxygen of the cluster polyanion constitute a beautiful supramolecular helix chain. The heteropolyanion is the first example of tri-capped and mono-supported pseudo-Keggin-type tungstovanadophosphate and the pH value is crucial for obtaining compound 1 in synthetic procedure. - Graphical abstract: A novel complex [Cu(phen){sub 2}]{sub 3}{l_brace}PW{sub 4}{sup VI}W{sub 5}{sup V}V{sub 3}{sup IV}O{sub 40}(V{sup IV}O){sub 3}[Cu(en){sub 2}]{r_brace}.4H{sub 2}O, the first example of tri-capped and mono-supported highly reduced pseudo-Keggin-type tungstovanadophosphate was synthesized under hydrothermal condition. And the heteropolyanions are linked by water dimer and cation [Cu(phen){sub 2}]{sup 2+} through the hydrogen bond forming a three-dimensional (3D) supramolecular network. Interestingly, the water dimer and terminal oxygen of the polyanion cluster constitute a beautiful supramolecular helix chain.
- OSTI ID:
- 21043774
- Journal Information:
- Journal of Solid State Chemistry, Journal Name: Journal of Solid State Chemistry Journal Issue: 12 Vol. 180; ISSN 0022-4596; ISSN JSSCBI
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
COPPER COMPLEXES
CRYSTAL STRUCTURE
DIMERS
ELECTRON SPIN RESONANCE
HETEROPOLYANIONS
HYDROTHERMAL SYNTHESIS
MONOCRYSTALS
PH VALUE
PHENANTHROLINES
PHOSPHATES
POLYMERS
THREE-DIMENSIONAL CALCULATIONS
TUNGSTEN COMPOUNDS
VANADIUM COMPOUNDS
WATER
X-RAY DIFFRACTION
X-RAY PHOTOELECTRON SPECTROSCOPY