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Bridged silsesquioxane nanocomposites with tunable morphologies incorporating o-nitrophenylene–ammonium bridges are described. The systematic screening of the sol–gel parameters allowed the material to reach the nanoscale with controlled dense and hollow structures of 100–200 nm. The hybrid composition of silsesquioxanes with 50% organic content homogeneously distributed in the nanomaterials endowed them with photoresponsive properties. Light irradiation was performed to reverse the surface charge of nanoparticles from +46 to −39 mV via a photoreaction of the organic fragments within the particles, as confirmed by spectroscopic monitorings. Furthermore, such nanoparticles were applied for the first time for the on-demand delivery of plasmid DNA in HeLa cancer cells via light actuation.

Predetermining the physico‐chemical properties, biosafety, and stimuli‐responsiveness of nanomaterials in biological environments is essential for safe and effective biomedical applications. At the forefront of biomedical research, mesoporous silica nanoparticles and mesoporous organosilica nanoparticles are increasingly investigated to predict their biological outcome by materials design. In this review, it is first chronicled that how the nanomaterial design of pure silica, partially hybridized organosilica, and fully hybridized organosilica (periodic mesoporous organosilicas) governs not only the physico‐chemical properties but also the biosafety of the nanoparticles. The impact of the hybridization on the biocompatibility, protein corona, biodistribution, biodegradability, and clearance of the silica‐based particles is described. Then, the influence of the surface engineering, the framework hybridization, as well as the morphology of the particles, on the ability to load and controllably deliver drugs under internal biological stimuli (e.g., pH, redox, enzymes) and external noninvasive stimuli (e.g., light, magnetic, ultrasound) are presented. To conclude, trends in the biomedical applications of silica and organosilica nanovectors are delineated, such as unconventional bioimaging techniques, large cargo delivery, combination therapy, gaseous molecule delivery, antimicrobial protection, and Alzheimer's disease therapy. Predetermining the biological outcome of nanomaterials by designis essential for safe and effective biomedical applications. In this Review, it is chronicled that how the nanomaterial design of pure silica, partially hybridized organosilica, and fully hybridized organosilica governs not only their physico‐chemical properties but also their biocompatibility, protein corona, biodistribution, biodegradability, and clearance. Cargo loading/delivery strategies and trending biomedical applications are also discussed.