The stibnite mineralization at Rizana (Kilkis ore district; Serbo-Macedonian metallogenic province; northern Greece) occurs along a NE–SW-trending brittle shear-zone, which transects a two-mica and an augen-gneiss of the Vertiskos Unit. Barren Triassic A-type granites and satellite pegmatites and aplites, as well as Oligocene-Miocene plutonic, subvolcanic and volcanic rocks that are variably hydrothermally altered and mineralized, outcrop in the broader region. The mineralization appears as veins, discordant lodes and disseminations. Veins and discordant lodes exhibit massive and brecciated textures. Historic underground mining (1930s–1950s) produced 9000 t of stibnite ore, grading 40% Sb on average. The main ore mineral assemblage includes stibnite + berthierite + sphalerite + pyrite + chalcopyrite + native antimony and traces of wolframite, galena, tetrahedrite, marcasite, pyrrhotite, arsenopyrite, realgar, native arsenic and native gold. Quartz, minor barite and ankerite are the gangue minerals. Sericitization and silicification developed along the shear-zone, forming hydrothermal halos of moderate intensity in the two-mica gneiss. Locally, valentinite, goethite and claudetite are present due to the supergene oxidation of the stibnite mineralization. Bulk ore geochemistry shows enrichments in specific elements including As, Au, Cd, Se, Tl and W. Fluid inclusion microthermometry showed that the mineralization was formed under a limited range of temperatures and salinities. The fluids had low to slightly moderate salinities (6.6–8.1 wt% equiv. NaCl) with low homogenization temperatures (217–254 °C, with a maximum at 220 °C).