Reactions of molybdenum and chromium hexacarbonyls with isatin-3-oxime (H2L) in THF were carried out under sun light or according to the traditional thermal reflux synthetic routes. Di-l-oxo bimolybdenum complex, [Mo(H2L)(THF)(O)2]2 was successfully synthesized under the reflux conditions. However, the dichromium oxo complex, [Cr(H2L)(O)2]2 was prepared using the sun light route. The prepared complexes were characterized using elemental analysis, IR, mass spectrometry, UV–Vis spectra, thermal analysis, and magnetic measurements.