TY - JOUR
T1 - Synthesis and Properties of Iron(II) Hydride Complexes Containing the Tripodal Tetraphosphine Ligand P(CH2CH2PMe2)3
AU - Field, Leslie D.
AU - Messerle, Barbara A.
AU - Smernik, Ronald J.
PY - 1997
Y1 - 1997
N2 - The preparation and characterization of iron(II) hydride complexes containing the tripodal tetraphosphine ligand tris[2-(dimethylphosphino)ethyl]phosphine, P(CH2CH2PMe2)3 (PP3), 1, are reported. Dissolution of the chloro hydride complex FeHCl(PP3), 2, in methanol affords an equilibrium mixture of 2 and the methoxy hydrido complex FeH(OMe)(PP3), 3. Reaction of a methanol solution containing 2 and 3 with anionic or neutral ligands affords the corresponding hydrido complexes: reaction with NaBr affords FeHBr(PP3), 4; reaction with NaI affords FeHI-(PP3), 5; reaction with NaN3 affords FeHN3(PP3), 6; reaction with CO affords [FeH(CO)(PP3)]+, 8; reaction with N2 affords [FeH(N2)(PP3)]+, 8; and reaction with PPh3 affords [FeHPPh3(PP3)]+, 9. In some cases, further reaction of the product iron hydride complexes is observed. Reaction of FeHN3(PP3), 6, with NaN3 for an extended period affords Fe(N3)2(PP3), 10. On standing in solution, [FeH(N2)(PP3)]+, 8, is converted to the dinitrogen-bridged complex [FeH(PP3)N≡NFeH(PP3)]2+, 11. The carbonyl hydride complex 7 and the dinitrogen hydride complex 8 can be deprotonated to give the neutral iron(O) complexes Fe(CO)(PP3), 12, and Fe(N2)(PP3), 13, respectively. The air-sensitive complexes 4-13 were characterized, by multinuclear NMR, IR, Raman, and mass spectroscopy and by elemental analysis.
AB - The preparation and characterization of iron(II) hydride complexes containing the tripodal tetraphosphine ligand tris[2-(dimethylphosphino)ethyl]phosphine, P(CH2CH2PMe2)3 (PP3), 1, are reported. Dissolution of the chloro hydride complex FeHCl(PP3), 2, in methanol affords an equilibrium mixture of 2 and the methoxy hydrido complex FeH(OMe)(PP3), 3. Reaction of a methanol solution containing 2 and 3 with anionic or neutral ligands affords the corresponding hydrido complexes: reaction with NaBr affords FeHBr(PP3), 4; reaction with NaI affords FeHI-(PP3), 5; reaction with NaN3 affords FeHN3(PP3), 6; reaction with CO affords [FeH(CO)(PP3)]+, 8; reaction with N2 affords [FeH(N2)(PP3)]+, 8; and reaction with PPh3 affords [FeHPPh3(PP3)]+, 9. In some cases, further reaction of the product iron hydride complexes is observed. Reaction of FeHN3(PP3), 6, with NaN3 for an extended period affords Fe(N3)2(PP3), 10. On standing in solution, [FeH(N2)(PP3)]+, 8, is converted to the dinitrogen-bridged complex [FeH(PP3)N≡NFeH(PP3)]2+, 11. The carbonyl hydride complex 7 and the dinitrogen hydride complex 8 can be deprotonated to give the neutral iron(O) complexes Fe(CO)(PP3), 12, and Fe(N2)(PP3), 13, respectively. The air-sensitive complexes 4-13 were characterized, by multinuclear NMR, IR, Raman, and mass spectroscopy and by elemental analysis.
UR - http://www.scopus.com/inward/record.url?scp=0001128461&partnerID=8YFLogxK
M3 - Article
C2 - 11670230
AN - SCOPUS:0001128461
SN - 0020-1669
VL - 36
SP - 5984
EP - 5990
JO - Inorganic Chemistry
JF - Inorganic Chemistry
IS - 26
ER -