We succeeded in synthesizing single crystals of a novel nickel sulfate Ni2-δSO5 by a hydrothermal method. A single-crystal X-ray diffraction revealed a tetragonal structure with lattice constants, a = 5.184 Å and c = 12.91 Å. In this structure, one-dimensional chains composed of face-shared NiO6 octahedra elongate along the a axis and the b axis alternately, constructing a ‘log-cabin’ type framework where neighbor chains lying orthogonally to each other are connected by SO4 tetrahedra. A detailed refinement of the structure suggested that the site occupancy of Ni is only 63%, corresponding to δ ≈ 2/3. Furthermore, X-ray oscillation photographs exhibit diffuse-scattering patterns probably arising from a short-range order of the Ni defects. Magnetic susceptibility revealed an antiferromagnetic transition accompanied by a weak ferromagnetism at 17 K.