The complexes Fe(NO)(CO)2(Ph3P)2X (X = Cl, Br, or NO3) have been prepared by the reaction of Fe(CO)3(Ph3P)2 with the corresponding nitrosyl halides. NOX (X = Cl or Br), or dinitrogen tetroxide, N2O4, in methyl cyanide or benzene. Metathetical reactions of the chloro- or bromo-complexes with NH4PF6, NaBF4, or Lil have led to the isolation of the analogous derivatives Fe(NO)(CO)2(Ph3P)2Y (Y = PF6–, BF4–, or I–). On the basis of molecular weight, infrared, and conductivity data these complexes are best formulated as 1 : 1 electrolytes, [Fe(NO)(CO)2(Ph3P)2]X and [Fe(NO)(CO)2(Ph2P)2]Y. Infrared data in the region 1700–2200 cm.–1 are consistent with a trigonal bipyramidal structure with apical triphenylphosphine groups and with an equatorial NO group for the cation [Fe(NO)(CO)2(Ph3P)2]+.