59751-32-5Relevant academic research and scientific papers
ReOCl3(PPh3)2] as a substrate for the synthesis of the rhenium(I) carbonyl complexes [Re(CO)2(OAc)(PPh 3)2] and [ReCl(CO)3(PPh3) 2
Krawczyk, Monika K.,Krawczyk, Marta S.,Siczek, Mi?osz,Lis, Tadeusz
supporting information, p. 60 - 62 (2013/06/27)
New preparative methods have been developed for the synthesis of the rhenium(I) carbonyl complexes [Re(CO)2(OAc)(PPh3) 2] (1) and [ReCl(CO)3(PPh3)2] (2). Acetic anhydride was decarbonylated during the course of its reaction with [ReOCl3(PPh3)2], resulting in the formation of the rhenium(I) carbonyl complex [Re(CO)2(OAc)(PPh3) 2] (1), which was subsequently converted almost quantitatively to [ReCl(CO)3(PPh3)2] (2) via the decarbonylation of its acetate group under acidic conditions.
Synthesis and characterization of ruthenium, rhenium and titanium formate, acetate and trifluoroacetate complexes. Correlation of IR spectral properties and bonding types
Gibson, Dorothy H.,Ding, Yan,Miller, Rebecca L.,Sleadd, Bradley A.,Mashuta, Mark S.,Richardson, John F.
, p. 1189 - 1200 (2008/10/08)
New formate (1-3; 4b, 6 and 7), acetate (8, 9) and trifluoroacetate (12, 13 and 15) complexes have been synthesized and characterized by elemental analysis and by IR and 1H and 13C NMR spectroscopies. New data or new synthetic proced
A Re(I)-Re(VII) COMPLEX BY THE OXYGENATION REACTIONS OF Re(I) SPECIES. REACTIVITY AND X-RAY STRUCTURAL CHARACTERIZATION OF Re(CO)3(PPh3)2(OReO3)
Ardizzoia, G. Attilio,Cenini, Sergio,D'Alfonso, Giuseppe,Monica, Girolamo La,Masciocchi, Norberto,Moret, Massimo
, p. 515 - 520 (2007/10/02)
The hydrido complex HRe(CO)2(PPh3)3 reacts with tertiary amines, in the presence of O2 and H2O, to give Re(CO)2(PPh3)2(O2CR), containing a chelating carboxylato group originated by oxidation of the alkyl group of the amine.NEt3, N(n-Pr)3 and N(n-Bu)3 have been used, the acetato, propionato and butyrato derivatives being respectively obtained.In the absence of the amine, the reaction gives the Re(I)-Re(VII) complex Re(CO)3(PPh3)2(OReO3), 1, containing a coordinated perrhenate ion.The same species was obtained by reaction of Re(CO)2(PPh3)2(NHCOC6H4Me) with O2/H2O.Complex 1 has been alternatively prepared by reacting ReCl(CO)3(PPh3)2 with AgReO4.Crystals of 1 have been shown by single crystal X-ray analysis to be monoclinic, space group P21/n (No. 14) with a = 10.248(6), b = 27.487(5), c = 13.247(2) Angstroem, β = 97.55(2) deg and Z = 4.The refinement performed by full-matrix least-squares methods, for 4651 independent significant reflections, gave a final R value of 0.029.The crystals contain discrete dinuclear molecules with an octahedrally coordinated Re(I) atom bearing three carbonyls, two mutually trans triphenylphosphine ligands and a coordinated ReO4- moiety.Complex 1 was shown to be partially dissociated in acetone solution and the value of the dissociation constant has been estimated by means of the Ostwald relationship -5>.The addition of NEt3 to an acetone solution of 1 at room temperature causes its complete dissociation.Complete dissociation was also observed in acetonitrile, with formation of the ionic species , 2.Complex 1 reacts with NEt3, at 55 deg C under an inert atmosphere, to give the rhenium(I) acetato derivative Re(CO)2(PPh3)2(O2CCH3), showing that the perrhenate anion is able to perform the oxidation of alkyl groups of tertiary amines to carboxylato groups.
Reactions of the polyhydrides Re2H8(PPh3)4 and ReH7(PPh3)2 with acetic acid/acetic anhydride. Isolation and characterization of the rhenium(I) carbonyl complexes Re(O2CCH3)(CO)1+x(PPh3) 3-x (x = 0, 1) and the homoleptic dirhenium(III) ...
Cameron, Charles J.,Fanwick, Phillip E.,Leeaphon, Malee,Walton, Richard A.
, p. 1101 - 1104 (2008/10/08)
Full title: Reactions of the polyhydrides Re2H8(PPh3)4 and ReH7(PPh3)2 with acetic acid/acetic anhydride. Isolation and characterization of the rhenium(I) carbonyl complexes Re(O2CCH3)(CO)1+x(PPh3) 3-x (x = 0, 1) and the homoleptic dirhenium(III) carboxylate complex Re2(μ-O2CCH3)4(O 2CCH3)2. The dirhenium octahydride Re2H8(PPh3)4 reacts with acetic acid/acetic anhydride mixtures in dichlorobenzene to give the homoleptic acetate complex Re2(μ-O2CCH3)4(O 2CCH3)2 as the major product together with small quantities of the carbonyl complex Re(O2CCH3)(CO)2(PPh3)2. The related reaction with propionic acid/propionic anhydride gives only Re(O2CC2H5)-(CO)2(PPh 3)2 in very low yield. Treatment of ReH7(PPh3)2 with these same acid/anhydride mixtures in THF, in the presence of PPh3, affords yellow Re(O2CR)(CO)(PPh3)3 (R = CH3, C2H5) in high yield. Solutions of these complexes in 0.1 M n-Bu4NPF6/CH2Cl2 show a reversible couple in their cyclic voltammograms associated with a one-electron oxidation to their 17-electron cations. Chemical oxidation of Re(O2CR)(CO)(PPh3)3 to the paramagnetic, orange salts [Re(O2CR)(CO)(PPh3)3]PF6 has been accomplished by using [(η5-C5H5)2Fe]PF6 in acetone. The acetate complex [Re(O2CCH3)(CO)(PPh3)3]PF 6·THF has been characterized structurally by X-ray crystallography. Crystal data at 20°C: space group Pnma, a = 15.785 (4) A?, b = 22.577 (3) A?, c = 23.824 (3) A?, V = 5656 (5) A?3, and Z = 4. The structure was refined to R = 0.033 and Rw = 0.040 for 2600 data with F2 > 3.0σ(F2).
