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We report herein the preparation of mixed periodic mesoporous organosilica nanoparticles (<b>E-Pn 75/25</b> and <b>90/10 PMO NPs</b>) by sol-gel co-condensation of <i>E</i>-1,2-bis(triethoxysilyl)ethylene ((<i>E</i>)-BTSE or <b>E</b>) with previously synthesized disilylated <i>tert</i>-butyl 3,5-dialkoxybenzoates bearing either sulfide (precursor <b>P1</b>) or carbamate (precursor <b>P2</b>) functionalities in the linker. The syntheses were performed with cetyltrimethylammonium bromide (CTAB) as template in the presence of sodium hydroxide in water at 80 °C. The nanomaterials have been characterized by Transmission Electron Microscopy (TEM), nitrogen-sorption measurements (BET), Dynamic Light Scattering (DLS), zeta-potential, Thermogravimetric Analysis (TGA), FTIR, ¹³C CP MAS NMR and small angle X-ray diffraction (p-XRD). All the nanomaterials were obtained as mesoporous rodlike-shape nanoparticles. Remarkably, <b>E-Pn 90/10 PMO NPs</b> presented high specific surface areas ranging from 700 to 970 m²g⁻¹, comparable or even higher than pure <b>E PMO</b> nanorods. Moreover, XRD analyses showed an organized porosity for <b>E-P1 90/10 PMO NPs</b> typical for a hexagonal 2D symmetry. The other materials showed a worm-like mesoporosity.