AbstractA new tsumcorite-group mineral, nickeltsumcorite, Pb(Ni,Fe³⁺)₂(AsO₄)₂(H₂O,OH)₂, the Ni-dominant analogue of tsumcorite and cobalttsumcorite, was found in the oxidation zone of a hydrothermal orebody containing gersdorffite and galena at the Km-3 mine, Lavrion, Attikí Prefecture, Greece. It is associated with annabergite, nickellotharmeyerite, nickelaustinite, gaspéite, calcite, dolomite, aragonite, quartz, goethite, cerussite, arseniosiderite, mimetite, oxyplumboroméite and Mn oxides/hydroxides. Nickeltsumcorite occurs as open-work aggregates and interrupted crusts up to 3 mm × 5 mm in area and up to 0.2 mm thick. They typically consist of coarse radial spherulites or dense concentric nodules up to 0.15 mm in diameter. Bunches or hemispherical clusters of crude individuals and separate imperfect, elongated crystals (up to 0.02 mm long) are also observed. Nickeltsumcorite is yellow, brownish-yellow, light brown or brown, with a yellow streak and a vitreous lustre. The Mohs hardness is ∼4. The mineral is brittle; one direction of distinct cleavage is observed under the microscope. D(calc.) = 5.02 g cm^–3. Nickeltsumcorite is optically biaxial (–), α = 1.82(2), β = 1.87(1), γ = 1.90(1), 2V(obs.) is large. The chemical composition (wt.%, electron-microprobe data, H₂O by difference) is CaO 2.79, PbO 28.12, MgO 0.30, CoO 0.15, NiO 17.39, ZnO 0.76, Mn₂O₃ 0.57, Fe₂O₃ 6.83, As₂O₅ 38.17, H₂O 4.92, total 100.00. The empirical formula, calculated based on 10 O apfu, is (Pb_0.76Ca_0.30)_∑1.06(Ni_1.39Fe³⁺_0.51Zn_0.06Mn³⁺_0.04 Mg_0.04Co_0.01)_∑2.05As_1.99O_7.97[(H₂O)_1.25(OH)_0.78]. The strongest reflections in the powder X-ray diffraction pattern [d,Å(I)(hkl)] are 4.64 (100) (1̄11), 4.47 (41)(2̄01), 3.238 (82)(1̄12), 3.008(60)(201), 2.859(41)(021), 2.545(79)(3̄12, 112), 2.545 (79)(3̄12, 112) and 2.505 (61)(220, 2̄03). The cation composition, powder Xray diffraction data and IR spectrum show that nickeltsumcorite belongs to the tsumcorite structure type. The new mineral is monoclinic, space group C2/m, a = 9.124(8), b = 6.339(3), c = 7.567(7) Å, β = 115.19(6)°, V = 396.0(7) Å3 and Z = 2. Nickeltsumcorite forms a solid-solution series with nickellotharmeyerite.