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This communication describes a new tandem metathesis reaction for which an RC-ROM mechanism was experimentally supported. This process was successfully applied to the synthesis of cis-fused polyhydroquinolines enabling a short stereoselective total synthesis of ent-lepadin B. Copyright

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

9/27 News What Unique Challenges Do Researchers Face in Benzylidenebis(tricyclohexylphosphine)dichlororuthenium

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Alternating ring-opening olefin metathesis polymerization of trans-RuCl2(Py)2((R,R)-Norphos) and COE using trans-RuCl2(=CHPh)(PCy3)(NHC) (NHC = 1,3-bis(2,4,6-trimethylphenyl)-4,5-dihydroimidazol-2-ylidene) as catalyst, followed by cross-linking of the ends of the living polymer with dicyclopentadiene, reaction with (1R,2R)-1,2-diphenylethylenediamine to displace the pyridine ligands, and finally deposition on BaSO4 produced a heterogeneous catalyst that was reused 10 times for hydrogenation of 1?-acetonaphthone in 85% ee.

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

09/27/21 News Get Up To Speed Quickly On Emerging Topics: Dichloro(benzene)ruthenium(II) dimer

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The bond-assisted cyclometalation and phosphorus-carbon bond cleavage in (Arene)ruthenium(II) complexes are discussed. The complexes contain functionalized iminophosphorane-phosphine ligands Ph2PCH 2P{=NP(=X)(OR)2}Ph2 (X = O, S; R = Et, Ph). It is found that the functionalized iminophosphorane-phosphines act as versatile ligands upon coordination to a (eta6-arene)-ruthenium(II) fragment. The results show that the ligands are used as templates for the construction and stabilization of unusual organometallic ruthenium(II) complexes.

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

27-Sep-21 News Extended knowledge of (1,3-Bis(2,4,6-trimethylphenyl)-2-imidazolidinylidene)dichloro(phenylmethylene)(tricyclohexylphosphine)ruthenium

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Four cyclic pentapeptides and two cyclic heptapeptides modelled on the 310 helical Pro138-Gly144 segment of the water channel aquaporin-4 (AQP4) postulated to mediate adhesive interactions between AQP4 tetramers were synthesised by olefin metathesis. Three related acyclic pentapeptides Boc-Ser(All)-Xaa1-Val-Ser(All)-Gly-OMe (Xaa1 = Val, Aib; Boc = tert-butoxycarbonyl; All = allyl) and Boc-Ser(Bn)-Val-Val-Gly-Gly-OMe (Bn = benzyl) and two acyclic heptapeptides Boc-Pro-Pro-Ser(All)-Val-Val-Ser(All)-Gly- OMe and Boc-Pro-Pro-Ser(Bn)-Val-Val-Gly-Gly-OMe were also prepared. NMR, CD and IR data provided evidence that the peptides can access a 310 helical structure in apolar solvents and pointed to a significant stabilising effect of the olefinic bridge on helicity in an aqueous environment. Thus we could demonstrate the viability of using ring closing olefin metathesis to stabilise short protein segments in the helical conformation that they adopt in their native protein environment. Our approach provides access to a set of peptides with potential binding affinity for AQP4.

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

9/27/21 News Extended knowledge of Dichloro(benzene)ruthenium(II) dimer

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Condensation of 1,4-dichloropyridazine with pyrazole, 3,5-dimethylpyrazole and 3-methylpyrazole yielded two types of pyrazolyl-pyridazine ligands, viz., (i) products of substitution on one side of the pyridazine as 3-chloro-6-(pyrazolyl)pyridazine (Cl-L1), 3-chloro-6-(3,5-dimethylpyrazolyl)pyridazine (Cl-L2) and 3-chloro-6-(3-methylpyrazolyl)pyridazine (Cl-L3), and (ii) products of substitution on both sides such as 3,6-bis(pyrazolyl)pyridazine (L1), 3,6-bis(3,5-dimethylpyrazolyl)pyridazine (L2) and tautomers of 3,6-bis(3-methylpyrazolyl)pyridazine (L3). The reactions of eta6-areneruthenium complexes in methanol with the above mentioned pyrazolyl-pyridazine ligands form mononuclear complexes of the type [(eta6-arene)Ru(Cl-L)(Cl)]+ and [(eta6-arene)Ru(L)(Cl)]+; (arene = benzene and p-cymene; Cl-L = Cl-L1, Cl-L2, Cl-L3; L = L1, L2, L3). All these complexes are characterized by IR, NMR, mass spectrometry and UV-vis spectroscopy. The structures of some representative complexes are established by single crystal X-ray diffraction studies.

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

27-Sep-21 News Extracurricular laboratory:new discovery of (1,3-Bis(2,4,6-trimethylphenyl)-2-imidazolidinylidene)dichloro(phenylmethylene)(tricyclohexylphosphine)ruthenium

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A method for producing at least one compound selected from the group consisting of a compound represented by the following formula (10), a compound represented by the following formula (11), a compound represented by the following formula (12), and a compound represented by the following formula (13), which the method containing reacting a compound represented by the following formula (2) with a compound represented by the following formula (7), in the presence of at least one compound selected from the group consisting of a compound represented by the following formula (1), a compound represented by the following formula (3), a compound represented by the following formula (4), a compound represented by the following formula (8), and a compound represented by the following formula (9).

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

9/27/21 News The important role of Chlorocyclopentadienylbis(triphenylphosphine)ruthenium(II)

Because a catalyst decreases the height of the energy barrier, its presence increases the reaction rates of both the forward and the reverse reactions by the same amount.Read on for other articles about C41H35ClP2Ru. name: Chlorocyclopentadienylbis(triphenylphosphine)ruthenium(II)

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Addition of cationic Lewis acids [M?Ln]+ (M?Ln = [Fe(CO)2Cp]+, [Fe(CO)(PPh3)Cp]+, [Ru(PPh3) 2Cp]+, [Re(CO)5]+, [1/2 Pt(PPh 3)2]+, [W(CO)3Cp]+ and the anionic thiocarbonyl complexes [HB(pz)3(OC)2M(CS)] – (M = Mo, W) have been prepared. Their spectroscopic data indicate that the addition of the cations occurs at the sulphur atom to give end-to-end thiocarbonyl bridged complexes [HB(pz)3(OC)2MCSM? Ln].

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

27-Sep News Properties and Exciting Facts 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

9/27 News Let’s Talk About Compound: Dichloro(benzene)ruthenium(II) dimer

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The reaction of [RuCl2(eta6-benzene)]2 with aroylthiourea resulted in the formation of Ru(ii) complexes of the type [RuCl2(eta6-benzene)L] (L = monodentate aroylthiourea ligand). The complexes were well characterized using UV-Visible, FT-IR, NMR and mass spectroscopic techniques. Single crystal X-ray diffraction confirmed the monodentate coordination of the ligand through a sulfur atom. The interaction of the Ru(ii) complexes with calf thymus DNA (CT DNA) was investigated using UV-Visible and fluorescence spectroscopic methods, and viscosity measurements. The binding ability of the complexes with bovine serum albumin (BSA) was explored using UV-Visible and fluorescence experiments. The results showed that the complexes interact with the biomolecules with appreciable binding constants. The gel electrophoresis technique was used to demonstrate the unwinding of the supercoiled DNA to its nicked form. The cytotoxicity of the Ru(ii) complexes was screened for a panel of cancer cell lines like HepG2, A549, MCF7 and SKOV3. Complexes 1, 2 and 3 showed modest activity at the concentration of 31.25 mug mL?1 against HepG2 cells. Complexes 1 and 3 displayed moderate cytotoxicity at the concentration of 62.5 mug mL?1 against A549 and SKOV3 respectively. Low cytotoxicity was observed for all the complexes against MCF7. Advantageously, complexes exhibited only less toxicity against Vero normal cells. Further DNA fragmentation, flow cytometry and fluorescence staining [DAPI (blue), FITC (green) and PI (red)] for the detection of apoptosis in HepG2 cells were carried out. The above methods demonstrated that the complexes have a significant ability to induce cell death by apoptosis.

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

Sep-21 News Get Up To Speed Quickly On Emerging Topics: Chlorocyclopentadienylbis(triphenylphosphine)ruthenium(II)

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The coordination chemistry of bis(di-ortho-tolylphosphino)methane (dotpm) has been studied. It is an excellent chelating ligand and a range of low-valent mononuclear complexes have been prepared; cis-[M(CO)4(eta 2-dotpm)] (M = Cr, Mo, W; 1-3), [CpRuCl(eta2-dotpm)] (4), and cis-[MX2(eta2-dotpm)] (M = Pt, X = Cl, Br, I; 5a-5c, M = Pd, X = Cl; 6). The backbone protons are relatively acidic and can be deprotonated using n-BuLi or LiN(SiMe3)2. Subsequent alkylation by RX (X = halogen; R = Me, Et, CH2Ph) affords cis-[M(CO)4(eta2-Rdotpm)] (M = Cr, Mo, W, R = Me; 7-9, M = Mo, W, R = Et, CH2Ph; 12-15), [CpRuCl(eta2-Medotpm)] (10), and cis-[PtI2(eta2-Medotpm)] (11). Thermolysis of cis-[Mo(CO)4(eta2-Medotpm)] (8) yields what is believed to be the coordinately and electronically unsaturated complex [Mo(CO) 3(eta2-Medotpm)] (16), suggesting that derivatives of dotpm (cone angle 194) are bulky enough to stabilize a 16-electron complex. Crystal structures of 2, 3, 7-9, 13, and 14 have been determined (diphosphine bite angles ranging from 66.58(3) to 70.96(5).

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