Transition metal ions with polydentate Schiff base ligands is a well studied area of research in coordination chemistry [1,2]. A new vanadium(IV) coordination compound with Schiff-base 2,6-diacetylpyridine-bis(nicotinoylhydrazone) (H2L) [V(=O)(H2L)(SO4)].4.75H2O (I) was synthesized by solution refluxing, which contains VOSO4, 2,6-diacetylpyridine and nicotinic hydrazide with 1:1:2 molar ratio, during 3 hours. Obtained red-ruby colored prismatic monocrystals were characterized by single-crystal X-ray method. Compound I crystallizes in the monoclinic space group P21/n, a 10.7647(4), b 9.9740(5), c 25.4131(9) Å, β 91.485(3)°, V 2727.6(2) Å3, Z 4, D(calc) 1.583 g/cm3, C21H28.50N7O11.75S1V1, R 0.0708. Vanadium polyhedron represents a distorted pentagonal bipyramid. In the molecular complex V(IV) each metalic cation binds three N and two O atoms of neutral ligand H2L that reside in the equatorial plane of the coordination pentahedron of metal and two O atoms in axial positions V=O and V–O (SO4 2-) (Fig. 1). The V–N distances in the equatorial plane of the coordination core range within 2.125(4) – 2.130(4) Å and V–O distances are 1.969(3) and 1.983(3) Å. The H2L ligand is pentacoordinated to metal via O2N3 set of donor atoms and form four five-membered pentametallocycles. The O2N3 equatorial atoms are almost planar and the deviation of the vanadium atom from this plane is 0.138 Å to O(3). The axial distances V=O and V–O(anion) are 1.592(3) and 2.093(3) Å.