A group of 5 new peroxomolybdates was synthesized and characterized. All the compounds belong to the group of oxidodiperoxidomolybdenum compounds, with a pyridine carboxylic acid N-oxide moiety coordinating the Mo atoms. They were investigated using single crystal or powder X-ray diffraction techniques. The obtained compounds were additionally characterized by IR spectroscopy and their thermal stability was studied by XRPD methods. The synthesized peroxomolybdates exhibit catalytic activity in the oxidation of cyclooctane with molecular oxygen.