The high-grade metamorphic rocks of the Ashuanipi complex have been the subject of a microthermometric fluid-inclusion study. Four types of fluid inclusions were observed: CO2-rich fluids; low-temperature, high-salinity H2O fluids; CH4 ± N2-rich fluids; and high-temperature, low-salinity H2O fluids. The regionally distributed CO2-rich fluids are the earliest fluids, and their calculated isochores indicate a clockwise post-peak metamorphic P–T–t path for the Ashuanipi complex. The low-temperature, high-salinity aqueous fluid inclusions are also distributed regionally and can be interpreted as late brines, retrograde metamorphic fluids, or the wicked-off aqueous component of H2O–CO2 fluid inclusions. Both CH4 ± N2-rich fluids and the high-temperature, low-salinity aqueous fluid inclusions were found only locally in gold-bearing metamorphosed banded iron formations. Fluid-inclusion microthermometry, arsenopyrite thermometry, and metamorphic petrologic study at Lac Lilois, one of the principal gold showings, suggest that some gold deposition may have occurred during regional post-peak metamorphic exhumation and cooling at P–T conditions near the amphibolite–greenschist transition. However, it is possible that gold deposition began at higher near-peak metamorphic P–T conditions. Another major gold showing, Arsène, is characterized by CH4 ± N2-rich fluid inclusions, tentatively inferred to be either directly related to gold deposition or responsible for secondary gold enrichment. The association of CH4 ± N2-rich fluids with gold occurrences in the Ashuanipi complex is comparable to gold deposits of the Abitibi greenstone belt and of Wales, Finland, and Brazil.