4,4'-Bis(3-N-methoxyformyl thioureido)-diphenyloxide was prepared via reaction of 4,4'-diaminodiphenyl alter with potassium sulfocyanate and ethyl chloroacetate in ethyl acetate. The single crystal of the title compound was cultured by slow evaporation method at room temperature. The crystal structure was determined with X-ray diffractometer. It is a monoclinic crystal, space group C2/c with a=0.95911 (19)
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