Discovery of (1,3-Dimesitylimidazolidin-2-ylidene)(2-isopropoxybenzylidene)ruthenium(VI) chloride

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Solid-phase synthetic strategies toward the generation of libraries of biologically relevant molecules were developed using olefin cross-metathesis as a key step. It is remarkably the formal alkane metathesis based on a one-pot, microwave-assisted, ruthenium-catalyzed cross-metathesis and reduction to obtain Csp3-Csp3 linkages.

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Reference:
Highly efficient and robust molecular ruthenium catalysts for water oxidation,
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Awesome and Easy Science Experiments about Chlorocyclopentadienylbis(triphenylphosphine)ruthenium(II)

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The conversion of CpRuCl(PPh3)2 in boiling ethylene glycol within 90 h of reflux has been investigated.New complex cations in the form of their tetraphenylborates, for which the formulae + and + are proposed, were isolated.The former cation is also formed at lower temperatures during the reflux of CpRuCl(PPh3)2 in methanol.The following process takes place: 2CpRuCl(PPh3)2 -> + + Cl- + 2PPh3.In the presence of dicyclopentadiene during the reflux of CpRuCl(PPh3)2 in high boiling polar solvents (ethylene glycol, dimethyl sulphoxide), ruthenocene is formed in a 90 percent yield.One of the cyclopentadienyl groups in ruthenocene originates from dicyclopentadiene.As a result of the reaction of CpRuCl(PPh3)2 and NaBPh4 in a mixture of diglyme and methanol, a colourless, crystalline compound, CpRu(eta-C6H5)BPh3, is obtained in a 50-60 percent yield.

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Reference:
Highly efficient and robust molecular ruthenium catalysts for water oxidation,
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

New explortion of Cis-Dichlorobis(2,2′-bipyridine)ruthenium(II)

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The unique ligands of [Ru(bipy)2(bpda)](PF6)2 (1, bpda = 1,1?-biphenyl-2,2?-diamine) and [Ru(bipy)2(dabipy)](PF6)2 (2, dabipy = 3,3?-diamino-2,2?-bipyridine) are atropisomeric (exhibit hindered rotation about the sigma bonds that connect the two aromatic groups), so the complexes are diasteromeric with conformation isomers possible for the atropisomeric ligands and configurational isomers possible at the metal centers. Only one diastereomer is observed in the solid-state in both cases. The seven-(1) and five-membered (2) chelate ring of dabipy and bpda (the ligand is bound through its pyridyl groups) ligands are delta when the configuration at the metal is Delta. No evidence for atropisomerization is found in solution. For 1, we conclude bpda binds stereospecifically; however, the atropisomerization barrier of dabipy may be sufficiently low for 2 to preclude the observation of diastereomers by low-temperature NMR spectroscopy.

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Reference:
Highly efficient and robust molecular ruthenium catalysts for water oxidation,
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Some scientific research about Cis-Dichlorobis(2,2′-bipyridine)ruthenium(II)

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The surface enhanced resonance Raman spectroscopy (SERRS) of a series of tris(2,2′-bipyridine)ruthenium(II) complexes on chemically produced silver films is reported.The SERR spectra of 2+, several tris complexes of Ru(II) containing substituted 2,2′-bipyridine (4,4′-dimethyl’, 4,4′-diphenyl-, 4,4′-diamino- and 4,4′-diethylcarboxylate-2,2′-bipyridine) ligands and the natural cis-bis complexes and show very high band intensities.The large enhancement arises from the combination of the inherent resonance Raman effect and the surface plasmon resonance (due to the rough nature of the silver film).The molecules are not chemisorbed on the silver surface and hence the enhancement occurs solely via the electromagnetic mechanism.The SERR spectra are virtually free of the fluorescence which dominates the corresponding RR spectra thus illustrating the use of SERRS in the vibrational spectroscopy of strongly luminescing species.The SERRS spectra of the substituted 2,2′-bipyridine complexes are discussed.

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Reference:
Highly efficient and robust molecular ruthenium catalysts for water oxidation,
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Awesome Chemistry Experiments For 32993-05-8

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32993-05-8, Name is Chlorocyclopentadienylbis(triphenylphosphine)ruthenium(II), molecular formula is C41H35ClP2Ru, belongs to ruthenium-catalysts compound, is a common compound. In a patnet, once mentioned the new application about 32993-05-8, Application In Synthesis of Chlorocyclopentadienylbis(triphenylphosphine)ruthenium(II)

A family of [CpRu(PP)(MeCN)]PF6 complexes (2 a?e and 4) were prepared in which the bis-phosphine ligand contains a pendent tertiary amine in the second-coordination sphere. 2 a?e contain PPh2NR?2 ligands with two amine groups as the pendent base. Complex 4 has the PPh2NPh1 ligand with only one pendent amine. The catalytic performance of 2 a?e and 4 were assessed in the cyclization of 2-ethynyl aniline and 2-ethynylbenzyl alcohol. It was revealed that the positioning of the pendent amine near the metal active site is essential for high catalyst performance. A comparison of PPh2NR?2 catalysts (2 a?e) showed minimal difference in performance as a function of pendent amine basicity. Rather, only a threshold basicity ? in which the pendent amine was more basic than the substrate ? was required for high performance.

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Reference:
Highly efficient and robust molecular ruthenium catalysts for water oxidation,
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Final Thoughts on Chemistry for Dichloro(benzene)ruthenium(II) dimer

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Ru(II) eta6-arene complexes containing p-cymene (p-cym), tetrahydronaphthalene (thn), benzene (bz), or biphenyl (bip), as the arene, phenylazopyridine derivatives (C5H4NN:NC6H 5R; R = H (azpy), OH (azpy-OH), NMe2 (azpy-NMe 2)) or a phenylazopyrazole derivative (NHC3H 2NN:NC6H5NMe2 (azpyz-NMe 2)) as N,N-chelating ligands and chloride as a ligand have been synthesized (1-16). The complexes are all intensely colored due to metal-to-ligand charge-transfer Ru 4d6-pi* and intraligand pi ? piz.ast; transitions (epsilon = 5000-63 700 M-3 cm -1) occurring in the visible region. In the crystal structures of [(eta6-p-cym)Ru(azpy)Cl]PF6 (1), [(eta6-p- cym)Ru(azpy-NMe2)Cl]PF6 (5), and [(eta6-bip) Ru(azpy)Cl]PF6 (4), the relatively long Ru-N(azo) and Ru-(arene-centroid) distances suggest that phenylazopyridine and arene ligands can act as competitive pi-acceptors toward Ru(II) 4d6 electrons. The pKa* values of the pyridine nitrogens of the ligands are low (azpy 2.47, azpy-OH 3.06 and azpy-NMe2 4.60), suggesting that they are weak pi-donors. This, together with their pi-acceptor behavior, serves to increase the positive charge on ruthenium, and together with the pi-acidic eta6-arene, partially accounts for the slow decomposition of the complexes via hydrolysis and/or arene loss (t1/2 = 9-21 h for azopyridine complexes, 310 K). The pKa* of the coordinated water in [(eta6-p-cym)Ru(azpyz-NMe2)OH 2]2+ (13A) is 4.60, consistent with the increased acidity of the ruthenium center upon coordination to the azo ligand. None of the azpy complexes were cytotoxic toward A2780 human ovarian or A549 human lung cancer cells, but several of the azpy-NMe2, azpy-OH, and azpyz-NMe 2 complexes were active (IC50 values 18-88 muM).

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Reference:
Highly efficient and robust molecular ruthenium catalysts for water oxidation,
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Archives for Chemistry Experiments of Cis-Dichlorobis(2,2′-bipyridine)ruthenium(II)

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The binuclear (2-) and trinuclear <(CN)5Cr-CN-Ru(bpy)2-NC-Cr(CN)5>(4-) bimetallic complexes have been synthesized and their photophysical behavior has been studied.Visible light absorption by the Ru(bpy)2(2+) chromophore leads to phosphorescence from the Cr(CN)6(3-) luminophore.The results demonstrate the occurrence of a fast (tau<10ns), efficient (eta=1) intramolecular exchange energy transfer process from the MLCT triplet of the Ru(II) fragment to the doublet state of the Cr(CN)6(3-) fragment.Distinctive features of these chromophore-luminophore complexes with respect to the behavior of the isolated luminophore are as follows: (i) large light-harvesting efficiency (antenna-effect); (ii) response to visible light (spectral sensitization); (iii) 100percent efficient population of the emitting state; (iv) photostability.The excited-state absorption (ESA) spectrum of both bimetallic complexes exhibits a peculiar visible band not shown by free Cr(CN)6(3-).This band corresponds to intervalence-transfer transitions from Ru(II) to excited Cr(III).Contrary to the behavior of free Cr(CN)6(3-), the bimetallic complexes also undergo a distinct bimolecular doublet-doublet annihilation process (rate constants k of the order of 1E7-1E8 M-1 s-1).The mechanism is thought to involve oxidation of Ru(II) and reduction of Cr(III).Intramolecular processes of the same type are probably responsible for the failure to observe doubly excited species upon two-photon excitation of the trinuclear complex. I hope this article can help some friends in scientific research. I am very proud of our efforts over the past few months and hope to 15746-57-3, help many people in the next few years., Synthetic Route of 15746-57-3

Reference:
Highly efficient and robust molecular ruthenium catalysts for water oxidation,
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

The Absolute Best Science Experiment for (1,3-Dimesitylimidazolidin-2-ylidene)(2-isopropoxybenzylidene)ruthenium(VI) chloride

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Phosphine-scavenging resins can significantly facilitate the synthesis of highly active Ru metathesis catalysts, including the second-generation Grubbs, Hoveyda, and indenylidene catalysts (GII, HII, InII). These catalysts are customarily prepared by ligand exchange of the corresponding first-generation catalysts with the N-heterocyclic carbene (NHC) H2IMes. The PCy3 coproduct is conventionally removed by pentane extraction, but the partial solubility of the desired Ru products can cause product losses of over 20%. Sequestration of the PCy3 coproduct with CuCl is more efficient, but is undesirable given the potential for non-innocent copper residues. Use of the arylsulfonic acid resin Amberlyst-15 delivers near-quantitative catalyst yields, but the high acidity of the resin leads to problems with reproducibility and decomposition. An alternative approach is described, in which a neutral Merrifield resin (crosslinked polystyrene with pendant p-C6H4CH2I groups; MF-I) is used to sequester PCy3 as the covalently-tethered benzylphosphonium salt. Addition of MF-I following complete ligand exchange effects quantitative uptake of free PCy3 (and any residual free NHC) within 45 min at RT: the clean products are isolated by filtration, in ca. 95% yield. These yields compare well with those obtained via the Amberlyst-15 route, without the challenges due to resin acidity. The efficacy of this methodology is demonstrated in the synthesis of isotopically-labelled derivatives of HII, in which the H2IMes ligand bears a 13C-label at the carbene carbon, or perdeuterated mesityl rings.

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Reference:
Highly efficient and robust molecular ruthenium catalysts for water oxidation,
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Discovery of Cis-Dichlorobis(2,2′-bipyridine)ruthenium(II)

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Reaction of hexa(hydroxybutenyl)benzene, 1a, and its FeCp+ complex, 1b, with halogeno-polypyridine in DMSO in the presence of KOH yields the hexapolypyridine ligands 2-4 and their iron-centered complexes 5-7. The hexaligands 3 and 4 were metallated using Ru(bipy)2Cl2 and Ru(terpy)Cl3, respectively, which gave correct yields of the hexaruthenium complexes 8 and 9. The iron-centered core 1b also reacted with [Ru(bipy)2(4-chloro-bipy)]2+(PF6 -)2 to give the hexaruthenated heptanuclear complex 11. Full characterizations including various mass spectrometry techniques verified the proposed structures. CNRS-Gauthier-Villars.

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Reference:
Highly efficient and robust molecular ruthenium catalysts for water oxidation,
Catalysts | Special Issue : Ruthenium Catalysts – MDPI

Final Thoughts on Chemistry for Ruthenium(III) chloride

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Trimethylsilyl iodide is shown to be an efficient metathetical reagent for preparing transition-metal iodides from the corresponding chlorides, though often complications can cause problems. These include reduction of the starting metal chloride when its oxidation state is high, due to the reaction of iodide, and even oxidation of low-oxidation-state compounds, presumably by incipient silyl cations. Finally, some very inert chlorides, such as of iridium(III), react too slowly with the iodide under the experimental conditions, and simple reaction with solvent becomes predominant.

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Reference:
Highly efficient and robust molecular ruthenium catalysts for water oxidation,
Catalysts | Special Issue : Ruthenium Catalysts – MDPI