The Kibali gold district, located on the Congo Craton, comprises a Neoarchean gold resource exceeding 28.7 Moz. The district is located within a westerly-verging stacked fold-and-thrust belt associated with a compressional tectonic regime active from ca. 2.64–2.60 Ga. Deposits are hosted by a major fault zone that consists of a complex series of smaller thrust faults, shear zones, and folds, which extend over 60 km. Gold deposits are primarily hosted in BIF and clastic sedimentary rocks. The gold and associated sulfides are in veins and disseminated in NE-to NNE-trending ore shoots within the deformed and metamorphosed volcanosedimentary rocks. Pyrite is the dominant sulfide mineral and hosts both solid solution gold and free gold. Because of its strong association with the gold mineralization, our study focusses on unravelling the metallogeny of the area by considering pyrite textural analyses, in situ trace element analyses using Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS), and S isotopic composition (δ34S) analyses using Secondary Ion Mass Spectrometry (SIMS).Eight distinct pyrite types were identified, including microcrystalline sooty (py-0a), small grains (<40 μm) (py-0b), aggregate recrystallized (py-1), core-rich inclusion (py-2), vein-like (py-3), non-zoned (py-4a), oscillatory As-bands zoned (py-4b), and cubic euhedral (py-5) pyrite. The ore-forming processes occurred over a polyphase evolution. Syn-diagenetic pyrite py-0a in volcaniclastic layers of older basin sediments served as the primary repository of Au (15.6 ppm median) with a near-zero δ34S value. Late diagenetic or early metamorphic pyrite (py-0b) was found in younger basin sediments. Py-1 resulted from solid-state recrystallization of py-0a and py-0b. During the early ore stage, porous py-2 with high Au concentrations (3.1 ppm) and various trace element enrichments precipitated due to fluid-rock interaction. Metal precipitation occurred through sulfidation and carbonation of wall rock with a relatively reduced fluid undergoing 34S-depletion. However, py-3 displayed notable trace element depletion and a complex mineral association. In a second ore stage, py-4a and zoned py-4b deposition occurred, dominated by an over-pressured fluid fracturing brittle rock. Py-4b, rich in Au (5.5 ppm) concentrated in oscillatory zoned As-rich bands, resulted from interactions during pulsed fluid flow. This process involved fluid phase separation, non-equilibrium conditions, 32S-depletion, and precipitation of py-4b with a high δ34S value (6.4 ‰ mean). Subsequently, pyrite (0–4) generations underwent deformation during a later ductile deformation event, leading to the remobilization and concentration of invisible gold into adjacent gold grains within the high-grade shoot plunging NE. This process involved shearing, boudinaging, and folding ore minerals in tightly folded structures. Late-stage py-5 formed under gold-poor fluid conditions or inefficient gold depositional conditions. Brittle fracturing of these grains later provided local sites for remobilized gold. The study contributes insights into the origin and evolution of gold mineralization in the Kibali gold district, supporting a multistage ore-forming fluid system.