Reactions involving Fe(NO)(2)(CO)(2) and the bis(phosphine) ligands bis(diphenylphosphino)methane (DPPM), bis(diphenylphosphino)acetylene (DPPA), 1,6-bis(diphenylphosphino)hexane (DPPH), and 1,4-bis(diphenylphosphino)benzene (DPPB) have been examined. From these reactions, the mononuclear complex, Fe(kappa(1)-DPPM)(NO)(2)(CO) 3, linear dinuclear species of the type Fe-2(mu-L)(NO)(4)(CO)(2) (L = Ph2PCH2PPh2 4, Ph(2)pCequivalent toCPPh(2) 5, Ph2PCH2(CH3)(4)CH2PPh2 6, and Ph2P(p-C6H4)PPh2 7), and macrocyclic dinuclear species of the type Fe-2(mu-L)(2)(NO)(4) (L = Ph2PCH2PPh2 8 and Ph(2)PCequivalent toCPPh(2) 9) were isolated and spectroscopically characterized. For 4, 5, 8, and 9, the solid-state molecular structures of the products were determined by use of single-crystal X-ray diffraction techniques.