Ruthenium(II) complexes containing both arene and functionalized phosphines. Synthesis and catalytic activity for the hydrogenation of styrene and phenylacetylene

Moldes, Isabel; Encarnación, Esther de la; Ros, Josep; Álvarez‐Larena, Ángel; Piniella, J. F.

doi:10.1016/s0022-328x(98)00647-0

Cited by 110 publications

(56 citation statements)

References 30 publications

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“…The η 1 -coordination mode is clearly evidenced by the presence of two doublets at δ = 15.1 and -30.6 ppm ( 3 J PP = 9.1 Hz) in the 31 P NMR spectrum, with the high-frequency resonance corresponding to the coordinated P centre. Selected NMR spectroscopic data 12.9 [b] -37.3 [b] dppa -32.0 0.4 [b] -34.2 [b] 3.6 [b] 10.1 [15] 3.2 [b] 5.8 [b] -37 To provide a possible explanation for the selective formation of these pendant phosphane complexes the solid-state structures of 2 and the oxide derivative of 1, [(η 6 -p-cymene)-RuCl 2 (η 1 -dppmO)] (3), obtained by slow oxidation of 1 in solution over a period of months, [16] were determined by X-ray diffraction analysis (see Figure 3 and Figure 4). The solid-state structure of 3 is much the same as that of 1, particular relevance to the reactivity of the pendant phosphane is the close proximity of the P centres in both 2 and 3 (and 1).…”

Section: Introductionmentioning

confidence: 99%

The Synthesis and Characterisation of Bis(phosphane)‐Linked (⁶‐p‐Cymene)ruthenium(II)–Borane Compounds

2005

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The reaction of [(η6‐p‐cymene)RuCl2]2 with some bis(phosphane) ligands (dppm, dppe, dppv, dppa, dpp14b, dppf) has been investigated. In general mixtures of products were obtained, although the pendant phosphane complexes [(η6‐p‐cymene)RuCl2(η1‐dppv)] and [(η6‐p‐cymene)RuCl2(η1‐dppa)] were isolated and characterized in the solid state by X‐ray diffraction. The later complex was obtained in lower yield and undergoes an equilibration reaction resulting in the formation of a dimeric species, where the dppa bridges two ruthenium centres, and uncoordinated phosphane; the bridging species was also structurally characterised in the solid state. In contrast, the reaction of [(η6‐p‐cymene)RuCl2(PPh3)] with dppa in the presence of [NH4]PF6 results in the formation of [(η6‐p‐cymene)RuCl(PPh3)(η1‐dppa)]PF6, which is stable in solution. A series of linked ruthenium–borane complexes, viz. [(η6‐p‐cymene)RuCl2(η1‐phosphane‐BH3)] (phosphane = dppm, dppe, dppv, dppa, dpp14b, dppf) and [(η6‐p‐cymene)RuCl(PPh3)(η1‐dppa‐BH3)]PF6 have been prepared from isolated pendant phosphane complexes, those generated in situ, or from a preformed phosphane–borane adduct. The solid‐state structures of [(η6‐p‐cymene)RuCl2(η1‐dppm‐BH3)], [(η6‐p‐cymene)RuCl2(η1‐dppe‐BH3)] and [(η6‐p‐cymene)RuCl2(η1‐dppv‐BH3)] have been determined by X‐ray diffraction analysis. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2005)

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Section: Introductionmentioning

confidence: 99%

The Synthesis and Characterisation of Bis(phosphane)‐Linked (⁶‐p‐Cymene)ruthenium(II)–Borane Compounds

2005

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“…2 and selected bond distances and angles are listed in Table 3. Although both the P-mono and P,N-bidentate coordination manners have been known for mononuclear systems, 5 the dppy ligand coordinates to the ruthenium center through only the phosphorus atom, as shown in Fig. 2.…”

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Crystal Structure of (2,2'-Bipyridine-N,N')(diphenyl-2-phosphinopyridine-P)-chloro(dicarbonyl)ruthenium(II) Hexafluorophosphate

Ooyama

Sato

2003

Anal. Sci. X

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The chemistry of polynuclear metal complexes including various bridging ligands has been widely developed for many years. 1 In particular, the diphenyl-2-phosphinopyridine (dppy) ligand has been used to construct hetero-binuclear metal complexes due to its possessing both the soft (P) and hard (N) donor atoms. 2In this work, an X-ray structural analysis of [Ru(bpy)(dppy)(CO)2Cl] + (bpy = 2,2′-bipyridine), which is a precursor for constructing new hetero-binuclear metal complex systems based on polypyridyl ruthenium complexes, was carried out.The title compound was prepared by the following procedure: [Ru(bpy)(CO)2Cl2] (0.1 g) 3 was added to H2O (10 cm 3 ), and an ethanolic solution (10 cm 3 ) of dppy (0.09 g) was added to the suspension. The mixture was refluxed with stirring for 2 h. The addition of a saturated aqueous solution of KPF6 to the solution resulted in a colorless precipitate. The recrystallized compound from ethanol-acetone was identified as a dppy coordination complex, [Ru(bpy)(dppy)(CO)2Cl]PF6. 4 A colorless crystal of the title compound, having approximate dimensions of 0.33 × 0.28 × 0.05 mm, was mounted on a glass fiber. Data collections were performed at 173 K with graphitemonochromated Mo Kα radiation (λ = 0.71070 Å) on a Rigaku/MSC Mercury CCD diffractometer. The data were corrected for Lorentz and polarization effects. The structure was solved by the Patterson method using DIRDIF94 PATTY.All of the non-hydrogen atoms were refined anisotoropically by full-matrix least-squares methods. All hydrogen atoms were located by a geometrical calculation, and were not refined. All calculations were performed using the teXsan crystallographic software package. The crystal and experimental data are given in Table 1. The atomic positional and thermal parameters are given in Table 2.The molecular structure of the cation is shown in Fig. 2 and selected bond distances and angles are listed in Table 3. Although both the P-mono and P,N-bidentate coordination manners have been known for mononuclear systems, 5 the dppy ligand coordinates to the ruthenium center through only the phosphorus atom, as shown in Fig. 2. The coordination sphere of the ruthenium atom consists of one dppy ligand, two mutually cis carbonyl ligands, a chelating bipyridine ligand, and one chloride ligand. The Ru-P bond is not significantly x39 ANALYTICAL SCIENCES 2003, VOL. 19 X-ray Structure Analysis Online Crystal Structure of (2,2′-Bipyridine-N,N′)(diphenyl-2-phosphinopyridine-P)-chloro(dicarbonyl)ruthenium(II) HexafluorophosphateDai OOYAMA † and Masahito SATO Faculty of Education, Fukushima University, Kanayagawa, Fukushima 960-1296, Japan The crystal structure of (2,2′-bipyridine-N,N′)(diphenyl-2-phosphinopyridine-P)-chloro(dicarbonyl)ruthenium(II) hexafluorophosphate ([Ru(bpy)(dppy)(CO)2Cl]PF6; bpy = 2,2′-bipyridine, dppy = diphenyl-2-phosphinopyridine) has been determined by X-ray diffraction. This compound crystallizes in a monoclinic system, space group P21/n, with the following unit cell parameters: a = 10.237 (1)

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“…X-ray crystallography in mononuclear systems, 7 the dppy ligands coordinate to the ruthenium center through only the phosphorus atom. The geometry about the ruthenium is slightly distorted octahedral.…”

Section: Resultsmentioning

confidence: 99%

Crystallographic report: A synthetic precursor for hetero‐binuclear metal complexes, [Ru(bpy)(dppy)₂(CO)₂](PF₆)₂ (bpy = 2,2′‐bipyridine, dppy = 2‐(diphenylphosphino)pyridine)

Ooyama

Sato

2004

Applied Organom Chemis

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In the title complex, [Ru(bpy)(dppy) 2 (CO) 2 ](PF 6 ) 2 (bpy = 2,2 -bipyridine, dppy = 2-(diphenylphosphino)pyridine), the ruthenium atom exhibits a slightly distorted octahedral coordination with the carbonyl ligands in cis positions. In addition, two dppy ligands coordinate to the ruthenium center through the phosphorus atoms in mutually trans positions and two pyridyl nitrogen atoms of the dppy direct toward two carbonyl ligands.

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Ruthenium(II) complexes containing both arene and functionalized phosphines. Synthesis and catalytic activity for the hydrogenation of styrene and phenylacetylene

Cited by 110 publications

References 30 publications

The Synthesis and Characterisation of Bis(phosphane)‐Linked (⁶‐p‐Cymene)ruthenium(II)–Borane Compounds

The Synthesis and Characterisation of Bis(phosphane)‐Linked (⁶‐p‐Cymene)ruthenium(II)–Borane Compounds

Crystal Structure of (2,2'-Bipyridine-N,N')(diphenyl-2-phosphinopyridine-P)-chloro(dicarbonyl)ruthenium(II) Hexafluorophosphate

Crystallographic report: A synthetic precursor for hetero‐binuclear metal complexes, [Ru(bpy)(dppy)₂(CO)₂](PF₆)₂ (bpy = 2,2′‐bipyridine, dppy = 2‐(diphenylphosphino)pyridine)

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Ruthenium(II) complexes containing both arene and functionalized phosphines. Synthesis and catalytic activity for the hydrogenation of styrene and phenylacetylene

Cited by 110 publications

References 30 publications

The Synthesis and Characterisation of Bis(phosphane)‐Linked (6‐p‐Cymene)ruthenium(II)–Borane Compounds

The Synthesis and Characterisation of Bis(phosphane)‐Linked (6‐p‐Cymene)ruthenium(II)–Borane Compounds

Crystal Structure of (2,2'-Bipyridine-N,N')(diphenyl-2-phosphinopyridine-P)-chloro(dicarbonyl)ruthenium(II) Hexafluorophosphate

Crystallographic report: A synthetic precursor for hetero‐binuclear metal complexes, [Ru(bpy)(dppy)2(CO)2](PF6)2 (bpy = 2,2′‐bipyridine, dppy = 2‐(diphenylphosphino)pyridine)

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The Synthesis and Characterisation of Bis(phosphane)‐Linked (⁶‐p‐Cymene)ruthenium(II)–Borane Compounds

The Synthesis and Characterisation of Bis(phosphane)‐Linked (⁶‐p‐Cymene)ruthenium(II)–Borane Compounds

Crystallographic report: A synthetic precursor for hetero‐binuclear metal complexes, [Ru(bpy)(dppy)₂(CO)₂](PF₆)₂ (bpy = 2,2′‐bipyridine, dppy = 2‐(diphenylphosphino)pyridine)