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In an attempt to prepare a supramolecular assembly consisting of two, three, or four diosmium carbonyl sawhorse units linked together by dicarboxylato ligands, the reaction of [Os 3 (CO) 12 ] with ferrocene-1,1′-dicarboxylic acid, Fe(C 5 H 4 COOH) 2 , was carried out with microwave heating. Instead of an assembly, the lone diosmium product was the single sawhorse complex [Os 2 (μ-ferrocene-1,1′-dicarboxylato)(CO) 6 ] ( 1 ) with a tetradentate doubly bridging Fe(C 5 H 4 CO 2– ) 2  ligand, a metal–metal single bond, four equatorial carbonyl ligands, and two axial carbonyl ligands. Two additional sawhorse complexes, [Os 2 (μ-ferrocene-1,1′-dicarboxylato)(CO) 4 (tri- p -tolylphosphine) 2 ] ( 2 ) and [Os 2 (μ-ferrocene-1,1′-dicarboxylato)(CO) 4 ( N , N -dimethylaminomethylferrocene) 2 ] ( 3 ), were prepared by substituting the axial CO ligands in  1  with P- or N-donor ligands, respectively. Clusters  1 ,  2,  and  3  represent the first examples of carbonyl sawhorse complexes with ferrocenedicarboxylato ligands, and all three were characterized with single-crystal X-ray diffraction studies.

Diosmium carbonyl sawhorse complexes containing a ferrocenedicarboxylato ligand