Abstract: | The redox-active doubly bridged species {Mo(NO)(TpMe2)Q}2] TpMe2 = tris(3,5-dimethylpyrazol-1-yl)hydroborate, Q = O(CH2)nO, n = 3, 5, or OCH2(CF2)n−2CH2O, n = 5, 6], and a chelate complex Mo(NO)-(TpMe2)O(CH2)5O] were prepared and characterised by elemental and mass analyses, 1H NMR and IR spectroscopy. The bimetallic species with C3, C5, and C5(F) bridges exhibit two well-resolved reduction processes in their cyclic voltammograms (ΔE1/2 values of 290, 170, and 170 mV, respectively). These results indicate that the presence of the second bridge increases the extent of electrochemical interactions (by ca. 90-130 mV) in comparison with their singly bridged analogues. All non-fluorinated and the chelate species were catalytically active in cathodic reduction of chloroform. |