Abstract: | Single crystals of Ti1.6Os2.4B2 and the solid solution Ti1–xFexOs2RhB2 (0 < x < 0.5) were synthesized by arc‐melting the elements in a water‐cooled copper crucible under an argon atmosphere. The new silver‐like phases, structurally characterized by single‐crystal X‐ray and EDX analyses, crystallize in the hexagonal Ti1.6Os1.4RuB2 structure type (space group (Nr. 189), Z = 3) and contain trigonal‐planar B4‐units and one‐dimensional chains of titanium or mixed titanium/iron atoms, respectively. |