A novel polyoxomolybdate (C 14 H 16 N 2) 3 (C 14 H 17 N 2) 2 [β-Mo 8 O 26 ](1) has been synthesized from hydrothermal reaction of tolidine and molybdenum trioxide in water and characterized by its IR and UV spectra, 1 H NMR, cyclic voltammetry and single crystal X-ray diffraction. Compound 1 crystallizes in the triclinic crystal system, space group Pī, 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 Å 3 and Z=1. The asymmetric unit of the crystal structure of (C 14 H 16 N 2) 3 (C 14 H 17 N 2) 2 [β-Mo 8 O 26 ] contains β-octamolybdate [β-Mo 8 O 26 ] 4− anions, two tolidine molecules and shows the presence of monoprotonated tolidine cations. One tolidine molecule and a β-Mo 8 O 26 polyanions species lie across crystallographic inversion centres while the two tolidine molecules occupy general sites.
The asymmetric unit of the title compound, (C6H4S4)8[Mo6O19]2·CH3CN, contains two halves of two centrosymmetric [Mo6O19]2− hexamolybdate anions, which are each built up from six distorted MoO6 octahedra sharing common edges and one common vertex at the central O atom, six tetrathiafulvalene cations (three of which are located on mirror planes) to balance the charge and a half of an acetonitrile solvent molecule, likewise located on a mirror plane. The two central hexamolybdate O atoms occupy special positions 2a and 2d, respectively. The cations and anions are interlinked through C—H⋯O contacts.
The structure of the title compound, NH4(C8H20N)3[Mo8O26], is built up by discrete cations and anions, with two formula units in the asymmetric unit. The β-octamolybdate anions are linked to the ammonium cations via N—H⋯O hydrogen bonding involving terminal oxide groups and to the tetraethylammonium cations via weak C—H⋯O interactions.
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