Hydrothermal synthesis and structural characterization of three inorganic-organic composite sandwich-type phosphotungstates

Journal Article · Sat Dec 15 04:00:00 EST 2007 · Journal of Solid State Chemistry

DOI:https://doi.org/10.1016/j.jssc.2007.09.029· OSTI ID:21043758

Junwei, Zhao; Shoutian, Zheng ^[1]

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1. State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Graduate School of the Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China)

Three inorganic-organic composite sandwich-type phosphotungstates [Ni(tepa)(H{sub 2}O)]{sub 4}H{sub 2}[Ni{sub 4}(H{sub 2}O){sub 2}({alpha}-B-PW{sub 9}O{sub 34}){sub 2}].8H{sub 2}O (1), (enH{sub 2}){sub 3}[Ni{sub 2}(H{sub 2}O){sub 10}][Ni{sub 4}(H{sub 2}O){sub 2}({alpha}-B-PW{sub 9}O{sub 34}){sub 2}].en.8H{sub 2}O (2) and (enH{sub 2}){sub 10}[Mn{sub 4}(H{sub 2}O){sub 2}({alpha}-B-PW{sub 9}O{sub 34}){sub 2}]{sub 2}.20H{sub 2}O (3) (tepa=tetraethylenepentamine and en=ethylenediamine) have been synthesized by the hydrothermal reaction of the trivacant Keggin polyoxoanion [{alpha}-A-PW{sub 9}O{sub 34}]{sup 9-} with Ni{sup 2+} or Mn{sup 2+} ions in the presence of tepa or en and structurally characterized by IR spectra, elemental analysis, thermogravimetric analysis and variable temperature magnetic susceptibility. X-ray crystallographic analyses indicate that they all contain the classical tetra-M sandwiched polyoxoanions [M{sub 4}(H{sub 2}O){sub 2}({alpha}-B-PW{sub 9}O{sub 34}){sub 2}]{sup 10-} (M=Ni{sup 2+} or Mn{sup 2+}) and nickel-organoamine cations or organoamine cations work as the charge balance ions. The tetra-M clusters in 1, 2 and 3 exhibit the familiar structural type of a {beta}-junction at the sites of metal incorporation. The study of magnetic property of 1 is indicative of a typical ferromagnetic coupling between Ni{sup 2+} cations. - Graphical abstract: Three inorganic-organic composite sandwich-type phosphotungstates [Ni(tepa)(H{sub 2}O)]{sub 4}H{sub 2}[Ni{sub 4}(H{sub 2}O){sub 2}({alpha}-B-PW{sub 9}O{sub 34}){sub 2}].8 H{sub 2}O (1), (enH{sub 2}){sub 3}[Ni{sub 2}(H{sub 2}O){sub 10}][Ni{sub 4}(H{sub 2}O){sub 2}({alpha}-B-PW{sub 9}O{sub 34}){sub 2}].en.8H{sub 2}O (2) and (enH{sub 2}){sub 10}[Mn{sub 4}(H{sub 2}O){sub 2}({alpha}-B-PW{sub 9}O{sub 34}){sub 2}]{sub 2}.20H{sub 2}O (3) have been hydrothermally synthesized and structurally characterized by IR spectra, elemental analysis, thermogravimetric analysis and magnetic susceptibility. They all contain tetra-M sandwiched polyoxoanions [M{sub 4}(H{sub 2}O){sub 2}({alpha}-B-PW{sub 9}O{sub 34}){sub 2}]{sup 10-} (M=Ni{sup 2+} or Mn{sup 2+}) and nickel-organoamine cations or organoamine cations work as the charge balance ions.

• OSTI ID: 21043758
• 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

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
BALANCES
CATIONS
COUPLING
CRYSTALLOGRAPHY
HYDROTHERMAL SYNTHESIS
INFRARED SPECTRA
MAGNETIC SUSCEPTIBILITY
MANGANESE COMPOUNDS
MANGANESE IONS
NICKEL COMPOUNDS
NICKEL IONS
THERMAL GRAVIMETRIC ANALYSIS
TUNGSTATES
WATER