Synthesis and structural characterization of (C14H16N2)3(C14H17N2)2[β-Mo8O26

Abstract

A novel polyoxomolybdate (C14H16N2)3(C14H17N2)2[β-Mo8O26] (1) has been synthesized from hydrothermal reaction of tolidine and molybdenum trioxide in water and characterized by its IR and UV spectra, 1H NMR, cyclic voltammetry and single crystal X-ray diffraction. Compound 1 crystallizes in the triclinic crystal system, space group Pı̄, with the crystal cell parameters of a=11.5360 Å, b=11.6080 Å, c=15.2520 Å, α=72.50∘, β=79.46∘, γ=86.91∘, V=1915.00 Å3 and Z=1. The asymmetric unit of the crystal structure of (C14H16N2)3(C14H17N2)2[β-Mo8O26] contains β-octamolybdate [β-Mo8O26]4− anions, two tolidine molecules and shows the presence of monoprotonated tolidine cations. One tolidine molecule and a β-Mo8O26 polyanions species lie across crystallographic inversion centres while the two tolidine molecules occupy general sites. The structural characterization of the title compound namely (C14H16N2)3(C14H17N2)2 [β-Mo8O26] isolated from hydrothermal synthesis of a mixture of C14H16N2 and MoO3 in distilled water is reported. The compound is characterized by IR and UV spectra, 1H NMR, cyclic voltammetry and single crystal X-ray diffraction.