Abstract
Synthesis was performed and physicochemical properties were studied for the M4V2O3(SO4)4 complexes, where M = K, Rb, or Cs. Their crystal structures were determined using the set of data from X-ray diffraction and neutron diffraction studies. All compounds crystallize in a triclinic lattice (space group \( P\bar 1 \) , Z = 2) with the parameters: a = 7.7688(2), 7.8487(1), 8.1234(1) A; b = 10.4918(3), 10.8750(2), 11.1065(1) A; c = 11.9783(4), 12.1336(2), and 11.8039(1) A; α = 76.600(2)°, 77.910(1)°, 79.589(1)°; β = 75.133(2)°, 75.718(1)°, 87.939(1)°; γ = 71.285(2)°, 72.189(1)°, 75.567(1)°; V = 881.78(5), 945.42(3), 1014.34(2) A3 for K, Rb, Cs, respectively. The structure of M4V2O3(SO4)4 was found to be formed by discrete complex anions V2O3(SO4)44− incorporating two oxygen-bridged vanadium atoms in a distorted octahedral oxygen environment. The sulfate groups are coordinated by the vanadium atoms in the chelating mode with a large scatter of S-O interatomic distances and OSO angles. Every VO6 octahedron has a short terminal vanadium-oxygen bond with a length of about 1.6A. The V2O3(SO4)44− complex anions in potassium and rubidium compounds differ from that in Cs4V2O3(SO4)4 in the type of symmetry and mutual spatial orientation. The vibrational spectra were presented and interpreted in line with the structural analysis data.
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