Hydrothermal synthesis and characterization of (N(C2H 5)4)4VMo12v2O 44

Cevik S., Alkan Z., Poyraz M., SARI M., Büyükgüngör O.

Crystal Research and Technology, cilt.42, sa.10, ss.955-960, 2007 (SCI-Expanded) identifier

  • Yayın Türü: Makale / Tam Makale
  • Cilt numarası: 42 Sayı: 10
  • Basım Tarihi: 2007
  • Doi Numarası: 10.1002/crat.200710924
  • Dergi Adı: Crystal Research and Technology
  • Derginin Tarandığı İndeksler: Science Citation Index Expanded (SCI-EXPANDED), Scopus
  • Sayfa Sayıları: ss.955-960
  • Anahtar Kelimeler: Heteropolymolybdovanadate, Heteropolyoxometalate, Heteropolyoxomolybdate, Polyoxometalate, Polyoxomolybdate
  • Uşak Üniversitesi Adresli: Evet

Özet

The hydrothermal reaction of a mixture of Na2MoO 4·2H2O, V2O5, pyromellitic acid (1,2,4,5-C6H2(COOH)4), (C 2H5)4NCl and 0,1 M H2SO4 for 88 h at 180°C gives blue needle-like crystals of [VIV 2O2(H2O)2 (C6H 2(COO)4)] in 20% yield (based on V) and dark blue prismatic crystals of the title compound, mixed-valance (N(C2H 5)4)4VMo12V2O 44], 1, in 12% yield (based on Mo). 1 was investigated by means of elemental analysis, thermogravimetry, Fourier Transform Infrared Spectroscopy and Single Crystal X-ray Diffraction Methods. Crystal data for the compound: monoclinic space group P21/c (No:14), a=13.7815(12) b=13.0271(9) c= 21.189(2) Å, β= 113.909(7)°, Z=2. Although [XM14O 42]-n (X=P, Si, Ge, V and M=Mo and/or V) cores have been previously determined, this is the first time that [VMo12V 2O44]-4 core is synthesized and characterized. The structural difference between 1 and these HPOMs is the coordinational geometry of the central metal atoms. The central vanadium in 1 has an octahedral coordination geometry, whereas in literature, the central V, P, Si and Ge atoms in [V15O42]-9 / [SiM8V 6O42]-4 / [PM8V6O 42]-5 / [GeM8V6O42] -4 have tetrahedral coordinational geometry. © 2007 WILEY-VCH Verlag GmbH & Co. KGaA.