Metal–organic frameworks (MOFs) based on transition metal elements are an important family of materials as they provide an opportunity to correlate their structure and magnetism, in addition to their adsorption and related properties arising from the porous structure. Among the broad family of transition metals, vanadium is particularly challenging due to its appearance in different oxidation states ranging from 2+ to 5+, which consequently exhibits an exceptionally rich variety of electronic ground states and magnetic properties. A new vanadium oxobenzoate [VO(C₆H₅COO)₂] has been synthesized under solvothermal conditions by reacting VO(OiPr)₃, benzoic acid and toluene. The resulting powder was thoroughly investigated by a number of complementary methods like XPS, electron microscopy techniques, synchrotron X-ray powder diffraction, thermal analysis, bulk density, and magnetic DC susceptibility measurement. The compound crystallizes in the monoclinic system with a = 20.661(2), b = 6.791(1), c = 9.959(1) Å, b = 92.08°, space group C2, and Z = 4. The crystal structure has been solved from synchrotron X-ray powder diffraction data using a direct space global optimization technique (program FOX) and refined by the constrained Rietveld method. The V atoms are in 4+ oxidation state as revealed by XPS. In the complex they have 5-fold coordination with respect to the oxygens, with the metal cation center in distorted squared pyramid coordination. Vanadium atoms are mutually linked via oxygen atoms forming helical zig-zag chains along the crystal b-axis as illustrated in Figure 1. The VO₅ inorganic layers lie at the distance of 10 Å, and are separated from each other by the organic part composed of benzoate moieties.

Figure 1. Molecular packing of vanadium oxobenzoate viewed along the [001] direction. The projection of unit cell is marked as a gray rectangle.

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