NiFeMo alloy nanoparticles were synthesized by co-precipitation in the presence of organic additives. Nanoparticles thermal evolution shows that there is a significant increase in the average size (from 28 to 60 nm), consolidating a crystalline structure of the same type as the Ni3Fe phase but with lattice parameter a = 0.362 nm. Measurements of magnetic properties follow this morphological and structural evolution increasing saturation magnetization (Ms) by 578% and reducing remanence magnetization (Mr) by 29%. Cell viability assays on as-synthesized revealed that nanoparticles (NPs) are not cytotoxic up to a concentration of 0.4 μg/mL for both non-tumorigenic (fibroblasts and macrophages) and tumor cells (melanoma).