Hydrothermal synthesis and structure of [H4AsIII 2AsVMoV 8MoVI 4O40]-, a bicapped, reduced keggin species

M. Ishaque Khan, Qin Chen, Jon A Zubieta

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Abstract

The hydrothermal reaction of As2O3, MoO3, NaCl, and water in a mole ratio of 5:10:10:380 for 50 h at 150°C yielded a dark blue solution, which upon standing produced blue-black crystals of Na0.5H4.5[As3MO12O 40]·4H2O (1). The structure of the anion of 1 [H4As3MO12I40]- consists of an α-Keggin core {AsMO12O40} capped on opposite {Mo4O4} faces by As(III) groups. The anion is a mixed-valence species with eight Mo(V) and four MO(VI) centers. Crystal data for As3Mo12Na0.5O44H12.5: Triclinic space group P1, a = 13.609(3) Å, b = 14.177(3) Å, c = 10.584(2) A, α = 111.02(1)°, β = 98.95(2)°, γ = 90.15(1)°, V = 1879.2(9) Å3, Z = 2, Dcalc = 3.711 g cm-3; structure solution and refinement were based on 7301 reflections converging at R = 0.0518.

Original languageEnglish (US)
Pages (from-to)2924-2928
Number of pages5
JournalInorganic Chemistry
Volume32
Issue number13
StatePublished - 1993

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ASJC Scopus subject areas

  • Inorganic Chemistry

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