2,2 -Sulfinyl-bis(4-methyl phenol) 3 and it's thio derivative have been synthesized in this work. The reduction process of sulfoxide 3 to its thio derivative 5 was accomplished in the presence of Zn/AcOH/SiO 2 , under microwave irradiation. The structures have been confirmed by spectroscopic (IR, 1 HNMR, 13 CNMR) and single crystal x-ray diffraction methods. 2,2 -Sulfinyl-bis(4-methyl phenol) 3 crystallizes in the space group Cc of the monoclinic system with four molecules in the unit cell of dimensions a = 11.425(2)Å, b = 13.530(2)Å, c = 9.5215(17)Å, β = 117.289(4)Å, and 2,2 -thio-bis(4-methyl phenol) 5 crystallizes in the space group P 2 1 2 1 2 1 of the orthorhombic system with four molecules in the unit cell of dimensions a = 9.021(1)Å, b = 10.523(2)Å, c = 13.607(2)Å, α = 90. The structures have been refined to final values for the crystallographic R factor of 0.0189(3) and 0.0248(5) based on 2999 and 3720 observed independent reflections respectively.