Br) (Me,pt = 3,5-dimethylpyrazolyI) have been prepared and characterised spectroscopically. Electrochemical studies (cyclic voltammetry, coulometry) of these complexes in acetonitrile established that all underwent at least one one-electron reduction process, some of which were reversible. The €& values for the reductionwere dependent on the nature of the metal, the halide, and the N H R' or OR group. The structure of [ Mo{H B( Me,pz),}( NO) I (OCH,CH,CH,Br)] was determined crystallographically. The six-co-ordinate nature of the complex was confirmed and the Mo-0 bond distance was 1.89 A, comparable to that in other related compounds.The compounds reported in this paper were prepared for two reasons: (a) to probe the nature of the co-ordination site when [M(HB(Me,pz),}(NO)X,] (X = halide, Me,pz = 3 3dimethylpyrazolyl) underwent substitution by Yto give [M{ HB(Me,pz),)(NO)XY], and (b) to establish that species of the type [M{HB(Me,pz),}(NO)XY] [X = halide, Y = OR or NHR' (R,R' = alkyl or aryl)] would undergo one-electron reduction as observed previously for [M{ HB(Me,pz))(NO)-