We report a high yield, two-step synthesis of fac-[Ru(bpy)(CH3CN)(3)NO2] PF6 from the known complex [(p-cym) Ru-bpy) Cl] PF6 (p-cym = eta(6)-p-cymene). [(p-cym) Ru(bpy) NO2] PF6 is prepared by reacting [(p-cymene) Ru(bpy) Cl] PF6 with AgNO3/KNO2 or AgNO2. The (NO2)-N-15 analogue is prepared using (KNO2)-N-15. Displacement of p-cymene from [(p-cym) Ru(bpy) NO2] PF6 by acetonitrile gives [Ru(bpy)(CH3CN)(3)NO2] PF6. The new complexes [(p-cym) Ru(bpy)NO2] PF6 and fac-[Ru(bpy)(CH3CN)(3)NO2] PF6 have been fully characterized by H-1 and N-15 NMR, IR, elemental analysis, and single-crystal structure determination. Reaction of [Ru(bpy)(CH3CN)(3)NO2] PF6 with the appropriate ligands gives the new complexes [Ru(bpy)(Tp) NO2] (Tp = HB(pz)(3)(-), pz) 1-pyrazolyl), [Ru(bpy)(Tpm) NO2] PF6 (Tpm = HC-pz)(3)), and the previously prepared [Ru(bpy)(trpy) NO2] PF6 (trpy) 2,2', 6', 2"-terpyridine). Reaction of the nitro complexes with HPF6 gives the new nitrosyl complexes [Ru(bpy) TpNO][PF6](2) and [Ru(bpy)(Tpm) NO][PF6](3). All complexes were prepared with N-15-labeled nitro or nitrosyl groups. The nitro and nitrosyl complexes were characterized by H-1 and N-15 NMR and IR spectroscopy, elemental analysis, cyclic voltammetry, and single-crystal structure determination for [Ru(bpy) TpNO][PF6](2). For the nitro complexes, a linear correlation is observed between the nitro N-15 NMR chemical shift and 1/v(asym), where v(asym) is the asymmetric stretching frequency of the nitro group.