32025-94-8Relevant academic research and scientific papers
One step conversion of perrhenate into an Re(IV) complex: Synthesis and molecular structure of trans-[ReCl4(PMePh2)2]
Hahn, F. Ekkehardt,Imhof, Lutz,Luegger, Thomas
, p. 109 - 112 (1997)
KReO4 reacts in a one-pot reaction with 4 mole of diphenylmethylphosphine and aqueous hydrochloric acid in boiling ethanol to yield trans-tetrachloro-bis(diphenylmethylphosphine) rhenium (1) in high yield. The almost quantitative, direct reduction of perrhenate to Re(IV) by PPh2Me/HCl has been observed for the first time. Bright red 1 can be crystallized from chloroform/hexane to give bright red plates. Crystals of 1 are triclinic with a=8.898(6), b=9.543(4), c=9.713(3) A, α=66.68(2), β=88.54(4), γ=63.10(3)°, Z=1 and Dobs=1.83 g cm-3. The structure was solved from 2327 diffraction data (Fo2≥3σ(Fo2)) collected at 20(2)° and refined to R=0.029 (Rw=0.039).
Oxygen and chlorine atom transfer between tungsten, molybdenum, and rhenium complexes. Competition between one- and two-electron pathways
Over, Diana E.,Critchlow, Susan C.,Mayer, James M.
, p. 4643 - 4648 (2008/10/08)
Inter-metal oxygen atom transfer reactions between molybdenum, tungsten, and rhenium complexes are described. With only chloride and PMePh2 as supporting ligands, oxygen atom transfer is observed from rhenium to molybdenum and tungsten and from
Dinuclear Elimination from Rhenium Hydrides and AlMe3: Rhenium/Aluminum Polyhydrides
Skupinski, Wincenty A.,Huffman, John C.,Bruno, Joseph W.,Caulton, Kenneth G.
, p. 8128 - 8136 (2007/10/02)
Reaction of Al2Me6 with ReH7P2 and with ReH5P3 (P = PMe2Ph and PMePh2) in benzene occurs with methane elimination to give ReH6AlMe2P2 and ReH4AlMe2P3, respectively.Each bimetallic compound is fluxional and shows evidence for both bridging and terminal hydride ligands.The X-ray crystal structure of ReH6AlMe2(PMePh2)2 shows it to be based on a ReH6P2 dodecahedron with AlMe2 bound to two hydride ligands, forming a η2-H2AlMe2 unit.Crystallographic data (-162 deg C): triclinic, P with Z = 2 and a = 17.815(8) Angstroem, b = 10.386(4) Angstroem, c = 11.094(4) Angstroem, α = 111.47(2) deg, β = 86.08(2) deg, γ = 95.78(2) deg.The X-ray crystal structure of ReH4AlMe2(PMePh2)3 shows a ReH4P3 pentagonal bipyramid (one P axial and two equatorial) with AlMe2 attached through three hydride ligands, one axial and two equatorial on Re, forming a H3AlMe22- unit.Crystallographic data (-164 deg C): monoclinic, P21/a with Z = 4 and a = 15.053(4) Angstroem, b = 15.900(4) Angstroem, c = 11.705(2) Angstroem, and β = 92.59(1) deg.Evidence for the mechanism of these reactions is presented, and the trend for aluminum to achieve a coordination number greater than 4 is surveyed.
Stabilization of RN=NN=PR3. Preparation and structural characterization of stable tetraarylphosphazide complexes containing molybdenum and tungsten
Hillhouse, Gregory L.,Goeden, Gary V.,Haymore, Barry L.
, p. 2064 - 2071 (2008/10/08)
The reaction of aromatic azides (R′N3) with MBr2(CO)3(PPh3)2 (M = Mo, W; Ph = C6H5; tol = p-CH3C6H4) in dry methylene chloride at 20°C affords MBr2(CO)3(R′N3PPh3), N2, and R′N =PPh3 (R′ = Ph, tol). The phosphazide complexes exhibit remarkable stability with respect to N2 loss. In contrast to the Mo(II) and W(II) complexes, ReCl3(CH3CN)(PPh3)2 and ReCl3(PPh2Me)3 yield ReCl4(PR3)2 upon treatment with the same aryl azides. Triclinic needles of WBr2(CO)3(tolN3PPh3) were grown from chloroform - ether and crystallized in space group C11-P1 with Z = 2, a = 13.715 (6) A?, b = 9.904 (5) A?, c = 10.397 (5) A?, α = 100.98 (2)°, β = 83.11 (2)°, and γ = 85.80 (1)°. An X-ray diffraction study at -145 (5)°C showed the complex to be monomeric and seven-coordinate. The tolyl azide had inserted into the W-P bond, forming a phosphazide ligand (tolN3PPh3) which is bound to W in a chelating fashion through the α and γ nitrogen atoms; the N3W metallacycle is nearly planar. Salient metrical parameters of the structure include the following: W-N(1) = 2.163 (4) A?, W-N(3) = 2.220 (5) A?, N(1)-N(2) = 1.279 (6) A?, N(2)-N(3) = 1.364 (6) A?, N(3)-P = 1.672 (5) A?, N(1)-C(41) = 1.423 (7) A?; N(1)-W-N(3) = 56.7 (2)°, W-N(1)-N(2) = 102.4 (3)°, W-N(3)-N(2) = 96.8 (3)°, N(1)-N(2)-N(3) = 103.8 (4)°. The full-matrix, least-squares refinement converged to R(F) = 0.028 and Rw(F) = 0.037 for 4066 unique data with Fo2 > 3σ(Fo2).
