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A series of gold nanoparticles (AuNPs) was prepared in situ with different cucurbit[<i>n</i>]urils (CB[<i>n</i>]s) in an alkaline aqueous solution. The nanoparticle sizes can be well controlled by CB[<i>n</i>]s (<i>n</i> = <i>5</i>, <i>6</i>, <i>7</i>, <i>8</i>) with different ring sizes. The packing densities of CB[<i>5</i>&#8315;<i>8</i>] and free surface area on AuNPs were determined. A direct relationship was found between the ring size and packing density of CB[<i>n</i>]s with respect to the AuNP-catalyzed reduction of 4-nitrophenol in the presence of NaBH₄. The larger particle size and higher surface coverage of bigger CB[<i>n</i>]-capped AuNPs significantly decreased the catalytic activity. Furthermore, this work could lead to new applications that utilize AuNPs under an overlayer of CB[<i>n</i>]s for catalysis, sensing, and drug delivery.