The aim of this study is to obtain organomercury compounds containing nitro group such as (10-nitroanthracen-2-yl)mercury(II) chloride and (9-nitroanthracen-2-yl)mercury(II) chloride by a mercuration reaction. The paper includes the preparation of a new organomercury compound based on nitroanthracene was prepared by mercuration reaction to 9-nitroanthracene by mercuric acetate then lithium chloride. m-C14H8ClHgNO2 (A) and o-C14H8ClHgNO2 (B). The prepared compounds were characterized by using FT- IR, 1H NMR, 13C NMR, XRD and MASS technique. The results of the chemical analysis to prepared compounds showed that it a good agreed with the proposed chemical structures. The purpose of this study to compare between meta and ortho organomercury derivatives for 9-nitroanthracene according to physical and chemical properties.