14489-09-9Relevant academic research and scientific papers
-bis Complexes of the Group 6B Elements: Synthesis and Spectroscopic Study
Oezer, Zahide,Oezkar, Saim,Pamuk, H. Oe.
, p. 37 - 43 (2007/10/02)
-bis complexes (CO)5MR2P(CH2)nPR2M(CO)5, (M: Cr, Mo, W; n: 1,2,3; R: CH3, C2H5, C6H5) were synthesized from the reaction of M(CO)5(CH3CN) with the appropriate ligand and characterized by means of IR and NMR (1H, 13C, 31P) spectroscopy.Spectral data indicate that the complexes contain two identical M(CO)5 moieties linked to each other by the R2P(CH2)nPR2 ligand.Each metal atom has a pseudo-octahedral arrangement of the five CO ligands and one phosphorus atom.Keywords: Chromium, Molybdenum, Tungsten, Dinuclear Complexes, Diphosphine
Substituted metal carbonyls. XXIII. Syntheses of unicoordinated diphosphine complexes of Cr and Mo and their entry into heterobimetallics MM'(CO)10(μ-P-P) as metalloligands
Gan, Kim-Suan,Lee, Hian Kee,Hor, T.S. Andy
, p. 197 - 202 (2007/10/02)
A series of pentacarbonyl complexes of chromium and molybdenum with unicoordinated-diphosphines, M(CO)5(η1-P-P) (P-P=dppe, dppp, dppb) has been prepared by amine oxide-induced phosphine substitution of the binary carbonyls.The basicity of the pendant phosphine groups was demonstrated by their ready conversion to the diphosphine-bridged heterobimetallic complexes (OC)5M(μ-P-P)M'(CO)5 (M,M'=Cr, Mo, W; M M') in the presence of M'(CO)5(CH3CN).The complexes were characterized by IR and NMR (1H and 31P-) spectroscopy.
SUBSTITUTED METAL CARBONYLS - I. MOLYBDENUM CARBONYL COMPLEXES CONTAINING UNIDENTATE AND BRIDGING DIPHOSPHINES: ONE-POT SYNTHESIS
Hor, T. S. Andy
, p. 213 - 218 (2007/10/02)
Trimethylamine N-oxide (TMNO)-initiated decarbonylations of Mo(CO)6 followed by phosphine additions yield the complexes Mo(CO)5(Ph2PCH2PPh2), which consists of a unidentate diphosphine, and the dinuclear phosphine-bridged complexes Mo2(CO)10(μ-Ph2P(CH2)nPPh2) (where n = 2,3) at ambient temperatures.The IR and NMR (1H and 31P) spectroscopic and structural properties of these complexes are presented and discussed.Some thermal analytical data are summarised.
Binuclear Molybdenum Carbonyls Bridged Both by Hydride and by Bidentate Phosphine Ligands. Crystal and Molecular Structures of Salts of (μ-H)(μ-Ph2P(CH2)nPPh2)Mo2(CO)8- (n=1-4) and Their Reactions with Acids
Darensbourg, Marcetta Y.,Mehdawi, Ramadan El,Delord, Terry J.,Fronczek, Frank R.,Watkins, Steven F.
, p. 2583 - 2591 (2007/10/02)
Reaction of Et4N+ and Ph4P+ salts of μ-HMo2(CO)10- with bidentate phosphine ligands in refluxing THF yielded salts of μ-HMo2(CO)8(Ph2P(CH2)nPPh2)-, n=1-4, designated as anions 1-, 2-, 3-, and 4-.X-ray crystal structure analyses for two of the new compounds were carried out, and the following parameters were obtained.Ph4P+1-: P21/c, Z=4, a=13.886(6) Angstroem, b=18.545(9) Angstroem, c=20.156(6) Angstroem, β=91.03(4) deg, V=5190(4) Angstroem3, R=0.0413 for 4402 reflections with /F0/>=3?/F0/.Et4N+4-: P1, Z=2, a=8.760(2) Angstroem, b=13.940(4) Angstroem, c=19.686(4) Angstroem, α=105.75(2) deg, β=93.59(2) deg, γ=97.38(2) deg, V=2282(1) Angstroem3, R=0.0471 for 4720 reflections with /F0/>=3?/F0/.Anions 1- and 4- are bridged by both H- and the bidentate ligands and show overall bent, staggered configurations with P1-Mo1-Mo2-P2 torsion angles of 21 deg for 1- and 42 deg for 4-.Similar framework bends (the intersection angle of (OC)ax-Mo vectors) of ca. 160 deg and similar Mo1-H-Mo2 angles of ca. 131 deg are observed for 1- and 4-.The Mo...Mo separation in 1- is 3.4028(8) Angstroem and in 4- it is 3.4995(8) Angstroem.The distance between the P-donor atoms in 1- is 3.19 Angstroem and in 4- it is 5.08 Angstroem.In 4- the hydride bridge is directed into the area underneath the ligand bridge (the (CH2)4 unit), whereas in 1- the plane of the hydride bridge is roughly perpendicular to the P-CH2-P bridge.The observed ligand substitution site selection was rationalized on the basis of the best match of bridge ligand donor site separation and intermetal ligand coordination site separation in the bent, staggered form of the parent μ-HMo2(CO)10-.A specific synthesis of the dibridged neutral bimetallics (μ-Ph2P(CH2)nPPh2)(μ-Ph2P(CH2)2PPh2)Mo2(CO)8 (n=1,2) and (μh2As(CH2)2AsPPh2)(μ-Ph2P(CH2)2PPh2)Mo2(CO)8 has been based on low-temperature protonation of 2- in the presence of other bidentate ligands.
