The monoanions derived from μ-S2Fe2(CO)6 and RMgX (R = CH3, C2H5) react with o-, m-, or p-BrCH2C6H4CH2Br in THF to give the bridged double FeS cluster complexes of [(μ-RS)Fe2(CO)6]2[μ-S-(o, m, or p-CH2C6H4CH2)-S-μ] in 44-87% yield. These products were characterized by IR, proton NMR and elemental analysis. A single crystal X-ray diffraction study of [(μ-CH3S)Fe2(CO)6]2[μ-S-(m-CH2C6H4CH2)-S-μ] has shown that it crystallizes in the space group P1 with a 7.831(2), b 14.423(3), c 14.928(2)Å; α 68.29(1), β 87.76(2), γ 83.19(2)°; V 1555.4 Å3; Dc 1.755g cm-3. Intensity data of 4154 independent reflections were collected in the range of 2 < θ < 23°, with 3184 reflections (I > 3σ(I)) being used in the structure refinement. The final R value was 0.052. © 1990.