MCM-41 has been synthesized at two different pH using cetyl-trimethylammonium bromide (CTAB) surfactant as template and adding the silica precursor to aqueous solutions containing CTAB. The obtained solids were calcined at 600 ◦C for 4 h. Mn-MCM-41 powders with different Mn/Si molar ratios were prepared using the incipient wetness method, followed by calcination at 550 ◦C for 5 h. At the end of the impregnation process the powders colour changed from white to brown whose intensity depends on manganese quantity. The materials characterization was performed by X-ray diffraction, N2 adsorption, 29Si Cross Polarization–Magic Angle Spinning NMR, and X-ray Photoelectron Spectroscopy. The effects of the manganese quantity and of the structural characteristic of the MCM-41 support were studied. The catalytic activity of the prepared systems was evaluated in a complete n-hexane oxidation.