Fabrication of multifunctional catalysts has always been the pursuit of synthetic chemists due to their efficiency, cost-effectiveness, and environmental friendliness. However, it is difficult to control multi-step reactions in one-pot, especially the spatial compartmentalization of incompatible active sites. Herein, we constructed metal-organic framework (MOF) composites which regulate the location distribution of metal nanoparticles according to the reaction path and coupled with the diffusion of substrates to achieve tandem reaction. The designed UiO-66-Pt-Au catalyst showed good activity and selectivity in hydrosilylation- hydrogenation tandem reaction, because the uniform microporous structures can control the diffusion path of reactants and intermediates, and Pt and Au nanoparticles were arranged in core-shell spatial distribution in UiO-66. By contrast, the low selectivity of catalysts with random deposition and physical mixture demonstrated the significance of artificial control to the spatial compartmentalization of active sites in tandem catalytic reactions, which provides a powerful approach for designing high- performance and multifunctional heterogeneous catalysts.