- Unexpected participation of nucleophiles in the reaction of palladium(II) acetate with divalent 3d metals
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The kinetics of reactions of palladium(II) acetate with cobalt(II), nickel(II), and copper(II) acetates were studied by spectrophotometry. These reactions produce heterobimetallic complexes PdII(μ-OOCMe) 4MII(OH2/sub
- Akhmadullina,Cherkashina,Kozitsyna,Gekhman,Vargaftik
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- First crystalline palladium(II) carboxylate complex with divalent 3d metal, PdCo(μ-OOCMe)4(NCMe): Synthesis and structure
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The first heterometallic palladium(II) acetate complex with divalent 3d metal, PdCo(μ-OOCMe)4(NCMe)·3 MeCN, was synthesized and structurally characterized.
- Kozitsyna,Nefedov,Cherkashina,Ikorskii,Vargaftik,Moiseev
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- The role of water molecules in formation of heterometallic palladium acetate complexes with cerium and neodymium
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The reactions of palladium(II) acetate with neodymium(III) and cerium(III) acetates in acetic acid containing a specified amount of water have been studied. The following homo- and heterometallic com- plexes have been synthesized and characterized by X-ray diffraction: Nd2(μ-OOCMe) 2(μ,η 2-OOCMe)2(η 2- OOCMe)2(HOOCMe)2(OH2)2 · 4HOOCMe, [Pd(μ-OOCMe)4Ce(OH2)2(μ,η 2-OOCMe)]2 · 2HOOCMe · 6H2O, [Pd(μ-OOCMe)4Ce(OH2)2(μ,η 2-OOCMe)]2 · 14H2O, [Pd(μ-OOCMe) 4M(HOOCMe)2(OH2)2]+ [Pd(μ-OOCMe)4M(μ- OOCMe)4Pd]- · 2MeCOOH · 1.5H2O (M = Nd, Ce), and {[Pd(μ- OOCMe)4Ce(OOCMe)4]2 [Pd4(μ-OOCMe)4]2(μ4-O) 8CePd4}(OH)3 · 27H2O. From kinetic and structural data and optical spectra of reaction solutions, the conclusion was drawn that hydrolytic processes play a decisive role in complexation reactions. Pleiades Publishing, Ltd., 2011.
- Nefedov,Kozitsyna,Akhmadullina,Cherkashina,Vargaftik,Moiseev
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- Heterodimetallic PdII-based carboxylate-bridged complexes: Synthesis and structure of single-crystalline PdII-M (M = MnII, CoII, NiII, CuII, ZnII, NdIII, EuIII, CeIV) acetates
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A series of crystalline PdII-based heterodimetallic acetate-bridged complexes containing the transition (MnII, CoII, NiII, CuII), post-transition (ZnII) and rare-earth (CeIV, NdIII, EuIII) metals were synthesized starting from Pd3(OOCMe)6 and the complementary metal(II, III) acetates. The crystal and molecular structures of the binuclear PdIIMII(μ-OOCMe)4L (M = Mn, Co, Ni, Zn; L = H2O, MeCN), trinuclear multiscripts(Pd, 2, mml:none(), mml:none(), II) CuII ( μ - OOCMe )6 and tetranuclear {Mathematical expression} (M = Nd, Eu) and {Mathematical expression} complexes were established by X-ray diffraction.
- Kozitsyna, Natalia Yu.,Nefedov, Sergei E.,Dolgushin, Fedor M.,Cherkashina, Natalia V.,Vargaftik, Michael N.,Moiseev, Ilya I.
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- Synthesis and solution behavior of the trinuclear palladium(II) unsaturated carboxylate complexes triangle-Pd3[μ-O2CC(R′) = CHMe]6 (R′ = Me, H): X-ray structure of palladium(II) tiglate (R′ = Me)
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The first examples of binary palladium(II) derivatives of unsaturated carboxylic acids are reported. It was found that the interaction of Pd3(μ-OAc)6 with the α,β-unsaturated 1-methylcrotonic (tiglic) and crotonic acids leads to the corresponding carboxylates of composition Pd3[μ-O2CC(R′) = CHMe]6, where R′ = Me (1) or H (2). The new compounds have been characterized by elemental analysis, solid and solution IR, 1H and 13C NMR, and ESI mass spectrometry. The crystal structure of 1 has been determined. This molecule displays a central Pd3 cyclic core with Pd-Pd distances of 3.093-3.171 A?. Each Pd-Pd bond is bridged by a pair of carboxylate ligands, one above and the other below the Pd3 plane, providing a square planar coordination for each Pd atom in an approximate D3h overall symmetry arrangement. Solution spectroscopic data show that the bridging η1:η1:μ2 interaction of the carboxylates of 1 and 2 is readily displaced, with a change of the ligand to the terminal (η1) coordination mode.
- Stromnova, Tatiana A.,Monakhov, Kirill Yu.,Cámpora, Juan,Palma, Pilar,Carmona, Ernesto,Alvarez, Eleuterio
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- On the nature of the chemical bond in heterobimetallic palladium(II) complexes with divalent 3d metals
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The complex Pd(μ-OOCMe)4Cu(OH2) ? 2Pd 3(μ-OOCMe)6 was synthesized and characterized by X-ray crystallography. In the heterometallic moiety of this complex, the Pd II and CuII atoms are at a
- Markov,Klyagina,Dolin,Akhmadullina,Kozitsyna,Cherkashina,Nefedov,Vargaftik,Moiseev
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- Non-trivial behavior of palladium(II) acetate
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Reaction of activated palladium metal with a HNO3/acetic acid mixture produces both orange Pd3(OAc)6, 1, and purple Pd3(OAc)5(NO2), 2. Compound 2 has a trinuclear structure derived from that of the well-known triangular complex 1 in which one acetate group has been replaced by a nitrite group which is bonded to one palladium atom by the nitrogen atom and to another Pd atom using one of the oxygen atoms. Highly pure 1 can be made by continuous removal of the nitric oxides from the reaction mixture using a flow of N2. 1H NMR spectra of solutions of 1 in CDCl3 and C6D6 show several signals of various intensities when a small amount of water is present in the deuterated solvents but only one signal when the solvents are thoroughly dried. These results are consistent with the occurrence of one or more hydrolysis processes when the solvents contain water and suggest that hypotheses about various [Pd(OAc)2]n aggregates that have previously been brought forward in the literature to explain the complexity of the spectrum of 1 are unnecessary, especially for nonpolar solvents. Compound 2 does not hydrolyze, and in wet or dried solvents shows a 1H NMR spectrum that consists of five equal-intensity signals due to the five nonequivalent acetate groups. The Royal Society of Chemistry 2005.
- Bakhmutov, Vladimir I.,Berry, John F.,Cotton, F. Albert,Ibragimov, Sergey,Murillo, Carlos A.
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- Method for producing ester compound and palladium catalyst used in the method
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A method for producing an ester compound includes reacting a compound having at least one cyclic structure of a norbornene ring and a norbornadiene ring with an alcohol and carbon monoxide by using a palladium catalyst and an oxidizing agent, to thereby introduce ester groups to carbon atoms forming a double bond in the cyclic structure and obtaining the ester compound, wherein the palladium catalyst includes a palladium acetate having a nitrite ligand in an amount of 10% by mole or more in terms of metal, and the palladium acetate having a nitrite ligand is represented by the general formula (1): Pd3(CH3COO)5(NO2).
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- METHOD FOR PRODUCING ESTER COMPOUND AND PALLADIUM CATALYST USED IN THE METHOD
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A method for producing an ester compound includes reacting a compound having at least one cyclic structure of a norbornene ring and a norbornadiene ring with an alcohol and carbon monoxide by using a palladium catalyst and an oxidizing agent, to thereby introduce ester groups to carbon atoms forming a double bond in the cyclic structure and obtaining the ester compound, wherein the palladium catalyst includes a palladium acetate having a nitrite ligand in an amount of 10% by mole or more in terms of metal, and the palladium acetate having a nitrite ligand is represented by the general formula (1): Pd3(CH3COO)5(NO2).
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- Can Palladium Acetate Lose Its "saltiness"? Catalytic Activities of the Impurities in Palladium Acetate
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Commercially available palladium acetate often contains two major impurities, whose presence can impact the overall catalytic efficacy. This systematic study provides a comparison of the differences in catalytic activity of pure palladium acetate, Pd3(OAc)6, with the two impurities: Pd3(OAc)5(NO2) and polymeric [Pd(OAc)2]n in a variety of cross-coupling reactions. The solid state 13C NMR spectra of all three compounds in conjunction with DFT calculations confirm their reported geometries.
- Carole, William A.,Bradley, Jonathan,Sarwar, Misbah,Colacot, Thomas J.
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supporting information
p. 5472 - 5475
(2015/11/18)
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- Palladium(II) acetates: Synthesis and molecular transformation scheme
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Known methods for synthesis of a trinuclear molecular form of palladium(II) acetate, [Pd3(CH3COO)6], are analyzed and a number of new techniques that enable reliable control over the type of the product obtained and provide its high yield are suggested. A molecular transformation scheme is suggested. This scheme takes into account the formation of both forms of palladium acetate and also the formation of the structurally similar [Pd3(CH3COO)3NO2].
- Mulagaleev,Kirik
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p. 2065 - 2075
(2011/05/07)
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- Synthesis and Reactivity of Palladium Complexes with Chiral Acido Ligands: Crystal Structure of Hexakis-[S(+)-2-Methylbutyrato]Tripalladium(II)
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Palladium(II) S(+)-2-methylbutyrate is obtained by the interaction of Pd3(OAc)6 with S(+)-2-methylbutyric acid. A single-crystal X-ray structure determination shows that a complex molecule contains the Pd3 triangular metal framework with nonbonding distances Pd-Pd (3.153-3.125 ?) and six bridging ligands 5(+)-2-EtC*H(Me)COO-, three of which are located above and three others below the plane of this Pd3 metal triangle. Using the Pd3[S(+)-2-EtC*H(Me)COO]6 complex and its analogues containing racemic ((±)-2-EtC*H(Me)COO-) and achiral (Me2CHCH2COO-) ligands as an example, the reduction of Pd(II) to Pd(0) with cyclohexene in aprotic media is studied. This reduction leads to the formation of esters of 2- and 3-cyclohexanol. Effects of chirality of the acido ligand and of a solvent on the mechanism of reduction of Pd(II) with alkenes are considered.
- Kozitsyna,Martens,Stolyarov,Nefedov,Vargaftik,Eremenko,Moiseev
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p. 1823 - 1829
(2008/10/08)
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