Monophasic Sn 1Àx Co x O 2 (x 5 0.05, 0.10, and 0.15) nanoparticles with tetragonal structure have been successfully synthesized by solvothermal method using oxalate precursor route. Powder x-ray diffraction and selected area electron diffraction studies confirmed highly crystalline cassiterite SnO 2 structure. The contraction of lattice constants confirmed the incorporation of Co 21 in SnO 2 host lattice. Hexagonal nanoparticles with average grain size of 8-13 nm have been formed. With the increasing Co content, the decreasing crystallite size of SnO 2 with increasing surface areas from 194 to 219 m 2 /g was found. The percentage reflectance increases on increasing the cobalt concentration, and a noticeable blue shift appeared. The band gap was found to be 3.85, 3.91, and 4.09 eV, respectively. Co-doped SnO 2 showed distinct magnetic behavior with different Co 21 concentration. For x 5 0.05 and 0.10, nanoparticles showed paramagnetism with antiferromagnetic interaction, however, on further increasing x 5 0.15, the nanoparticles showed canted antiferromagnetic coupling.