The Shuikoushan deposit is an economic 'skarn-type' polymetallic Pb-Zn deposit in South China. The deposit is located at the southern margin of the Hengyang basin in the northern part of the Nanling Range. Recently, economic Fe-Cu mineralization that occurs spatially connected to skarns along the contact zone between the granodiorite and limestones was discovered in the lower part of this deposit. Detailed zircon U-Pb geochronological data indicate that the granodiorite was emplaced at 153.7 +/- 0.58 Ma (Mean Square of Weighted Deviates (MSWD) = 2.4). However, the pyrite Re-Os isochron age reveals that Fe-Cu mineralization formed at 140 +/- 11 Ma (MSWD) = 8.1), which post-dates the emplacement of the granodiorite, as well as the previously determined timing of Pb-Zn mineralization (157.8 +/- 1.4 Ma) in this deposit. Considering that Fe-Cu mineralization was connected with the contact zone and also faults, and that sulfide minerals commonly occur together with quartz and calcite veins that crosscut skarns, we interpret this mineralization type as being related to injection of post-magmatic hydrothermal fluids. The timing of Fe-Cu mineralization (140 +/- 11 Ma) is inconsistent with a long-held viewpoint that the time interval of 145 to 130 Ma (e.g., Early Cretaceous) in the Nanling Range is a period of magmatic quiescence with insignificant mineralization, the age of 140 Ma may represent a new mineralization event in the Nanling Range.