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The two heterodinuclear nickel-ruthenium complexes [Ni(xbSmS)RuCp(PPh3)]PF6 and [Ni(xbSmSe)RuCp(PPh3)]PF6 (H2xbSmS = 1,2-bis(4-mercapto-3,3-dimethyl-2-thiabutyl)benzene, H2xbSmSe = 1,2,-bis(2-thiabutyl-3,3-dimethyl-4-selenol)benzene, Cp = cyclopentadienyl) were synthesized as biomimetic models of [NiFe] and [NiFeSe] hydrogenases. The X-ray structural analyses of the complexes show that the two NiRu complexes are isomorphous; in both NiRu complexes the nickel(ii) centers are coordinated in a square-planar environment with two thioether donor atoms and two thiolate or selenolate donors that are bridging to the ruthenium(ii) center. The Ru(ii) ion is further coordinated to a eta5-cyclopentadienyl group and a triphenylphosphane ligand. These complexes catalyze hydrogen evolution in the presence of acetic acid in acetonitrile solution at around -2.20 V vs. Fc+/Fc with overpotentials of 810 and 830 mV, thus they can be regarded as functional models of the [NiFe] and [NiFeSe] hydrogenases.

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

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A quite general approach for the preparation of eta5-and eta6-cyclichydrocarbon platinum group metal complexes is reported. The dinuclear arene ruthenium complexes [(eta6-arene)Ru(mu-Cl)Cl]2 (arene = C6H6, C10H14 and C6Me6) and eta5-pentamethylcyclopentadienyl rhodium and iridium complexes [(eta6-C5Me5)M(mu-Cl)Cl]2 (M = Rh, Ir) react with 2 equiv. of 4-amino-3,5-di-pyridyltriazole (dpt-NH2) in presence of NH4PF6 to afford the corresponding mononuclear complexes of the type [(eta6-arene)Ru(dpt-NH2)Cl]PF6 {arene = C10H14 (1), C6H6 (2) and C6Me6 (3)} and [(eta6-C5Me5)M(dpt-NH2)Cl]PF6 {M = Rh (4), Ir (5)}. However, the mononuclear eta5-cyclopentadienyl analogues such as [(eta5-C5H5)Ru(PPh3)2Cl], [(eta5-C5H5)Os(PPh3)2Br], [(eta5-C5Me5)Ru(PPh3)2Cl] and [(eta5-C9H7)Ru(PPh3)2Cl] complexes react in presence of 1 equiv. of dpt-NH2 and 1 equiv. of NH4PF6 in methanol yielded mononuclear complexes [(eta5-C5H5)Ru(PPh3)(dpt-NH2)]PF6 (6), [(eta5-C5H5)Os(PPh3)(dpt-NH2)]PF6 (7), [(eta5-C5Me5)Ru(PPh3)(dpt-NH2)]PF6 (8) and [(eta5-C9H7)Ru(PPh3)(dpt-NH2)]PF6 (9), respectively. These compounds have been totally characterized by IR, NMR and mass spectrometry. The molecular structures of 4 and 6 have been established by single crystal X-ray diffraction and some of the representative complexes have also been studied by UV-Vis spectroscopy.

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

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Reaction of (M = Ru, X = Cl; M = Os, X = Br; R = Me or Ph) with HPF6 gives the metal(IV) complexes , and with Cl2- gives .Reaction with gives the dications )2+), which have unusually high nu(NO) frequencies (1 850 – 1 875 cm-1).The crystal structure of has been determined by single-crystal X-ray methods at 295 K and refined by least squares to a residual of 0.044 for 2 038 ‘observed’ reflections.Crystals are orthorhombic, space group Pbca, with a = 21.680(6), b = 16.606(4), c = 12.772(5) Angstroem, and Z = 8.The Os-N-O system is linear, Os-N 1.75(1), N-O 1.17(2) Angstroem being indicative of the Os=N+=O moiety; Os-P lengths are 2.364(4) Angstroem and Os-C 2.23(2)-2.29(2) Angstroem.

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

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Reaction of Cp(PPh3)2RuCl (1) with primary alkylmagnesium halides (alkyl = Et, Pr, n-Bu, i-Bu) leads to the corresponding alkylruthenium complexes 4 – 7.Above 50 deg C 4 – 7 lose a PPh3 molecule and form by Ru-beta-H-elimination the (eta2-alkene)hydridoruthenium complexes 9 – 12.With R = isobutyl the intermediately formed, coordinatively unsaturated Cp(PPh3)Ru – R commplex can be stabilized by complexation with ethylene (50 bar) as (eta2-ethylene)isobutylruthenium complex 15.Mechanistic investigations of the <2-D3>ethyl complex 16 indicate that the Ru-beta-H-elimination is reversible. – Rotation of the eta2-alkene ligand in 9 – 12 leads to temperature-dependent 1H NMR spectra.The 31P chemical shifts of 1,2,4 – 7 and 9 – 12, respectively, are characteristic for the corresponding type of complexes.

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

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This paper describes the successful preparation of new Ru(IV)-pi-allyl complexes having the general formula (C5R5)RuX2(eta3-allyl) (R = H, Me; X = Cl, Br) by the oxidative addition of allylic halides to Ru(II) complexes, (C5R5)Ru(L)2X (R = H, Me; L = CO, PPh3; X = Br, Cl). These new compounds were subjected to NMR analysis to determine the structure, which was confirmed by X-ray crystallographic analysis of a representative compound. During the course of this study, the authors found facile reductive elimination of allylic halides from the Ru(IV)-pi-allyl complexes to form Ru(II)-carbonyl or Ru(II)-arene complexes, induced by contact with CO or aromatic solvents, respectively.

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

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Diphenyl-2-phosphinopyridyl (dppy) and 1,1,1-tris(diphenylphosphinomethyl)ethane (triphos) react with RuCpCl(COD), ( COD = cycloocta-1,5-diene; Cp = eta5-C5H5) by the displacement of the COD ligand to give, respectively, RyCpCl(eta1-dppy)2 (I) and RuCpCl(eta2-triphos) (II). When RuCpCl(PPh3)2 was used as the starting material, substitution of PPh3 ligands by dppy ligands afforded a mixture of di-(I) and mono-substituted RuCpCl(dppy)(PPh3) (III) complexes. The structure of (I) has been determined by X-ray crystallography and has been refined to a final R value of 0.0516. Both dppy ligands are P-coordinated. Crystal structure analysis of (II) shows that two phosphorus atoms are coordinated to the ruthenium atom in a chelating mode, and that the third phosphorus atom is free. This structure was refined successfully to a conventional R value of 0.0495. Reaction of RuCpCl(eta2-tripod) (tripod = 1,1,1-tris(triphenylphosphino)methane) with an excess of NH4PF6 gives the first eta3-tripod ruthenium complex [RuCp(eta3-tripod)][PF6] (IV) in 94 percent yield. The analogous triflate complex [RuCp(eta3-tripod)][CF3SO3] (V) has also been prepared. Crystal structure analyses of complex (IV) shows that all three phosphorus atoms are coordinated to the ruthenium atom, and that all three P-C-P angles are less than 90 deg, leading to considerable strain in the tricyclic system. The structure was refined successfully to a conventional R value of 0.0538. Treatment of the triflate complex (V) with [(C4H9)N][Rh)CO)2Cl2] gave the known complex CpRu(mu-CO)2(mu-Ph2PCH2PPh2)RhCl2 via a P-C bond cleavage reaction.

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

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Complexes with the CpRu(PPh3) fragment bound by iminopyridine ligands functionalised by a Hantzsch dihydropyridine donor of hydride ion or by a Hantzsch pyridinium acceptor of hydride ion have been prepared, and their redox chemistry studied by cyclic voltammetry and EPR and UV-Vis spectroelectrochemical investigations. These Ru(II) complexes have a coordinatively saturated, electronically precise (18-electron) ruthenium(II) centre with a non-labile ligand donor set, which suppresses complicating metal-centred reactivity and, thereby, allows the baseline physicochemical properties of the Hantzsch dihydropyridine/pyridinium-functionalised ligands to be investigated. In Ru(II) complexes, the iminopyridine chelate is linked to the Hantzsch pyridine groups by either an ortho-phenyl bridge (electronically delocalized) or by a meta-phenyl bridge (electronically isolated), which leads to notable differences in spectroscopic properties, even for ruthenium centre, and differences in redox reactions. Of note, the primary electrochemical reduction of the Ru(II) complexes with a Hantzsch pyridinium substituent is centred on this group, but did not afford the corresponding Ru(II) complexes with a 1,4-dihydropyridine substituent. Rather it was found that the reduction products were identical to the 1:1 hydroxide adducts formed upon addition of hydroxide ion to the starting Hantzsch pyridinium-substituted Ru(II) complexes. Based on these results and comparisons with data from the literature, the reduction products and hydroxide adducts are tentatively assigned as the corresponding hydroxy-dihydropyridine substituted Ru(II) complexes (during reduction, hydroxide ion was likely formed from the residual water present in the acetonitrile solvent). Implications for the electrochemical cycling of transition metal catalysts with Hantzsch pyridinium/dihydropyridine functional substituents are considered.

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

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Tetramethylarsoles (R=Ph, Me, t-Bu) have been obtained from Cp2Zr(C4Me4) and RAsCl2.From these a number of complexes of the type M(CO)5 (arsole) (M=Cr, W), cis-W(CO)4L(arsole) (L=piperidine, i-Pr3P), PF6, PF6 ((PR3)2=(PPh3)2, dppm, dpme), and PF6 (L2=(PMe3)2, norbornadiene) have been prepared through ligand exchange reactions.For R=Me, Ph the complexes readily undergo Diels-Alder-addition with acetylenedicarboxylic acid dimethyl ester.The 7-arsanorbornadienes formed as intermediates are unstable and decompose into arene and arsinidene complex which in one case has been trapped through consecutive insertion reactions. Key words: Arsole, Zirconocene; Phosphorus; Manganese; Ruthenium; Group 6

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

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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)

(eta5-Cyclopentadienyl)(eta5-ligand)ruthenium(II) (ligand=1,2,3,4,5-eta6-exo-methoxy-d3-7-oxo-2,4-cycloheptadienyl-2d 3a, 1,2,3,4,5-eta6-exo-methoxy-7-oxo-2,4-cycloheptadienyl-2d, 1,2,3,4,5-eta6-exo-methoxy-7-oxo-2,4-cycloheptadienyl, and 1,2,3,4,5-eta6-exo-ethoxy-7-oxo-2,4-cycloheptadienyl) was isolated in fairly good yields by treatment of (eta5-C5H5)(eta6-tropone)ruthenium(II)BF4 with KOH in CD3OD, CH3OD, CH3OH, and ethanol, respectively. The selectively deuterated tropone-2d was readily removed by photolysis of 3a accompanied by demethoxylation with visible light in the presence of large excess of P(OCH3)3.

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

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A method for isomerizing a maleate, or a maleate containing a 2-propenyloxy group in the molecule at a high selectivity is provided which employs an isomerizing catalyst containing a Group VIII element. This method produces a fumarate, or a fumarate containing a 1-propenyloxy group in a high yield, which is useful in the fields of resin source materials and plasticizer. This method gives high-purity fumarates containing no catalyst residue by use of a heterogeneous catalyst which is readily separable and non-corrosive.

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