We present field, chemical and U–Pb age data for metamafic–ultramafic bodies of the Triassic rift-related Therma– Volvi–Gomati (TVG) complex of the Serbo-Macedonian Massif (SMM) in the northern Aegean region. The TVG rocks record igneous textures overprinted by Alpine metamorphism and deformation. The high-Ti Volvi body was transformed into amphibolites, which also rim the low-Ti Gomati and Nea Roda bodies. The compositions are compatible with normal (N-) and enriched (E-) mid-ocean ridge basalt (MORB) and weak ocean island basalt (OIB) signatures of the high-Ti rocks, whereas the low-Ti rocks are depleted with respect to MORB, suggesting melt extraction from a mantle source. U–Pb geochronology reveals Triassic crystallization of the Volvi body at 240 Ma. Ordovician to Carboniferous xenocrystic zircons were found in the Stratoni body of the TVG complex, which were sampled from the SMM basement. The Triassic Arnea rift-related metagranite intrudes the Volvi body. Comparison of the compositions of the Volvi body and the Arnea metagranite of the SMM with Triassic metagranite of the Rhodope Massif (RM) supports the presence of a regional bimodal rift suite. The location of the TVG complex at the SMM–RM margin of Eurasia confirms its origin as a Middle Triassic rift suite, and its nature as a continental margin ophiolite representing an ocean–continent transition of the propagating Neotethys.