Synthesis and Crystal Structure of a Molybdovanadate with a Keggin-Type Anion
Journal of Structural Chemistry
, E-ISSN: 1573-8779
Institute of Inorganic Chemistry, Academy of Sciences of the USSR, Siberian Branch
Institute of Chemical Sciences, Academy of Sciences of the Kazakh SSR
An x-ray structural investigation of single crystals of [(C2Hs)2NH2]4 NH4*H[V(V3Mo9)040], which were obtained from sodium molybdovanadate solutions, has been carried out [Syntex P21 autodiffractometer, Mo K~ radiation, 3151 values of F(khs R = 0.064, R w ~ 0 058~ The crystals are monoclinic, a = 13.217(2), b = 20.279(4), c 21.440(6) ~, ~ = ~.8(2) ~ V = 5679(3) ~3, dcal = 2.38 g/cm 3, Z = 4. The characteristic fragment in the structure is a Keggin-type heteropoly anion with metal atoms (3V + 9Mo) statistically located at 12 positions within deformed octahedrons and with a tetrahedrally coordinated central V atom. The bonding between the heteropoly anions is realized by means of contacts with diethylamine molecules, NH4 ammonium groups, and an acidic proton. The 51V N~R spectra have been investigated,
and they confirmed the composition and structure of the complex [V4MogO40] 6- and showed that it is mainly dissociated into mixed isopoly anions of the 6 series and an Mo-subsituted decavanadate in a DMFA solution.