Decarbonylation of Mo and W hexacarbonyls in the presence of dimethylglyoxime was carried out under the control of trimethylamine N-oxide (TMNO). The two DMG substituted carbonyl complexes were prepared in a one pot synthesis using manipulated Schlenk techniques under dinitrogen in tetrahydrofuran. The Mo complex system was successfully carried out by stirring the mixture of the molybdenum hexacarbonyl and DMG in tetrahydrofuran at room temperature for 18hrs. A similar procedure afforded the starting ligand material for the W complex analogue. However, further refluxing for 6 h gave the desired W complex. The complexes were characterized using 1H NMR, IR, and CHN analyses. Results showed that the reactions produced analytically pure, mono-product dicarbonyl species; Mo(CO)2(DMG)2 I and W(CO)2(DMG)2 II where two DMG moieties were coordinated to the central metal atom through one N and O atoms respectively of each of the oxime groups.Keywords: Bioorganometallic, Metal carbonyl, CO-RMs, Decarbonylation, Trimethylamine N-oxid