- Unusual reactivity of the {ReVO}3+ core: Syntheses and characterization of novel rhenium halide complexes with N-methyl-o- diaminobenzene
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The reactions of 1 or 2 equiv of N-methyl-o-diaminobenzene with trans-[ReOX3(PPh3)2] (X = Cl, Br) in refluxing chloroform gave oxo-free rhenium complexes [ReVIX4(NC 6H4NHCH3
- Wei, Lihui,Babich, John W.,Zubieta, Jon
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p. 6445 - 6454
(2008/10/09)
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- ReCl4(PPh3)2 - Reactions and Structure
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The compounds ReCl4(PPH3)2 and Re2OCl3(C2H5COO)2(PPh3)2 resulting from the reaction of ReOCl3(PPh3)2 with PPh3 in boiling propionic acid and HClatmosphere were characterized by their VIS-spectra and structural data. Ligand exchange reactions with acetylacetone gave ReCl2(acac)2 as well as ReCl2(acac)PPh3)2. Crystallographic data see "Inhaltsuebersicht".
- Kraudelt, H.,Schilde, U.,Uhlemann, E.
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- REACTION OF (PPh3)2ReH7 WITH DIENES: PREPARATION AND SOME PROPERTIES OF TRIHYDRO η4-DIENE COMPLEXES OF RHENIU
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L2ReH7 (L=PPh3) reacts smoothly with acyclic and cyclic dienes to give crystalline, air-stable, trihydrido-Η4-dienerhenium complexes L2(η4-diene)ReH3.The majority of these complexes are fluxional at room temperature; their NMR spectra suggest that at low temperature (-50 deg C) they are pentagonal bipyramidal, with the two phosphine ligands apical and the remaining ligands equatorial.Except for L2(η4-cyclopentadiene)ReH3, which readily loses dihydrogen to give L2(η5-C5H5)ReH, these diene trihydrides are thermally remarkably stable; L2(η4-cyclohexa-1,3-diene)ReH3 loses dihydrogen at >100 deg C to afford L2(η5-cyclohexadienyl)ReH2 and then L2(η6-C6H6)ReH, and L2(η4-butadiene)ReH3 and L2(η4-cycloocta-1,5-diene)ReH3 are stable in air up to 115 and 130 deg C, respectively.Protonation of the trihydrido-η4-diene complexes affords the corresponding saturated hydrocarbons and/or olefins.Hydrogenation of L2(η4-2,3-dimethylbutadiene)ReH3 regenerates the heptahydride L2ReH7.
- Baudry, Denise,Ephritikhine, Michael,Felkin, Hugh
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p. 363 - 376
(2007/10/02)
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- Stabilization of RN=NN=PR3. Preparation and structural characterization of stable tetraarylphosphazide complexes containing molybdenum and tungsten
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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).
- Hillhouse, Gregory L.,Goeden, Gary V.,Haymore, Barry L.
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p. 2064 - 2071
(2008/10/08)
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- Reaction of (PPh3)2ReH7 with Dienes: Preparation and Some Properties of Trihydrido η4-Diene and Dihydro η5-Dienyl Complexes of Rhenium
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The title compound reacts with dienes to give trihydrido η4-diene or dihydro η5-dienyl complexes; pyrolysis of the η5-cyclohexadienyl compound (6) gives the hydrido arene complex (7), and protonation of the η4-d
- Baudry, Denise,Ephritikhine, Michel
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p. 249 - 250
(2007/10/02)
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