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(Et_4N)_2[O_2MoS_2Fe(SPh)_2],M= 726. 77,orthorhombic, space group P212121,with a=12. 434(2),b=10. 162(3),c=28. 285(2) A,V=3573. 8(14) A3,Z = 4,Dc=1. 351gcnr-3,D0=1. 36gcm-3(flotation)λ(MoKa) = 0. 71069A ,μ=10. 0cm-1, F(000) = 1520,T=298K. The structure was solved by heavy-atom method and refined by full-matrix least squares techniques to final R=0. 071 and Rw = 0. 074 for 1992 reflections (I≥3σ(I)). The title complex is a hetero dimetallic cluster containing a planar Mo(μ-S)2Fe rhomboidal core with the Mo-Fe distance of 2. 765(2) A.