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Organic functionalization and structural control of mesoporous materials are important for their applications. This study reports here that yolk–shell structured mesoporous nanoparticles with thioether-bridged organosilica frameworks can be successfully prepared by hydrothermal treatment of mesostructured organic–inorganic hybrid nanospheres. The thioether-bridged yolk–shell nanoparticles have ultrahigh condensation degree, i.e., (T³+Q⁴)/(Qⁿ+T^m) = 94%, large surface area (400 m² g^–1), accessible ordered mesochannels (2.0 nm), large pore volume (0.67 cm³ g^–1), and uniform diameter (290–90 nm), core size (180–40 nm), and shell thickness (19–8 nm). Thanks to the abundant thioether groups and the unique structure, the yolk–shell mesoporous nanoparticles can be used as nanoreactors to generate in situ polyhedral gold nanoparticles into their hollow spaces in a hot tetrachloride aurate aqueous …