The crystal and molecular structure of potassium pentachloronitrosylruthenate(II), K<sub>2</sub>[Ru(NO)Cl<sub>5</sub>]

Veal, Jack T.; Hodgson, Derek J.

doi:10.1107/s0567740872008295

Cited by 43 publications

(6 citation statements)

References 8 publications

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“…The crystal structure of the [Ru(NO)Cl 5 ] 2- anion closely resembles the structure reported earlier for the corresponding potassium salt, with no significant structural effects due to different cations. Therefore the structural data are provided only as Supporting Information, as well as the complete structural data for compound 4 ·HCl.…”

Section: Resultssupporting

confidence: 77%

Formation of Ruthenium Nitrosyl Complexes: Reactions of Ru(bpy)(CO)₂Cl₂and Its Methyl-Substituted Analogues Ru(4,4‘-dmbpy)(CO)₂Cl₂and Ru(6,6‘-dmbpy)(CO)₂Cl₂in Oxidizing Acidic Solutions

et al. 1997

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Experimental SectionMaterials. [Ru(CO)3Cl2]2 was purchased from Johnson & Matthey, and 2,2′-bipyridine and 4,4′-dimethyl-2,2′-bipyridine from were purchased Aldrich Chemicals. 6,6′-Dimethyl-2,2′-bipyridine was obtained from the University of Oulu, where it was synthesized according to the literature method. 16 Ru(bpy)(CO)2Cl2 and its dimethyl-substituted analogues were synthesized from [Ru(CO) 3Cl2]2 and 2,2′-bipyridine reagents by refluxing in THF as described earlier. 17,18 HNO3 (65%, J. T. Baker) and HCl (37%, Merck) were of analytical grade and were used as received. Ligand substitution reactions were carried out in a Berghof 60 mL digestive pressure bomb with a PTFE liner. 19 All manipulations were performed in air.Characterization of the Products. Infrared spectra were measured with a Nicolet Magna FTIR spectrometer 750. X-ray diffraction data were collected with a Nicolet R3m or Syntex P21 diffractometer using graphite-monochromatized Mo KR radiation (λ ) 0.710 73 Å). Cell parameters were obtained from 25 automatically centered reflections. Intensities were corrected for background, polarization, and Lorentz effects. Data collection, data reduction, and cell refinement were carried out with the P3/P4-Diffractometer Program V 4.27. 20 The structures were solved by direct methods. The structure solution was carried out with the SHELXS 86 program and the structure refinement with the SHELXL 93 program. 21,22 All non-hydrogen atoms, except one of the NO 3 -oxygens in 3, were refined anisotropically. The NO3 -oxygen was disordered in two positions with an equal occupation factor (0.5) and refined isotropically. All hydrogens in 1, 2, and 4 were located from the difference Fourier map and refined isotropically with a fixed isotropic displacement parameter (U ) 0.08 Å 2 for uncoordinated H2O hydrogens in 2 and U ) 0.05 Å 2 for all other hydrogens). The hydrogens of the H 2O ligand in 3 and those of the H3O + ions in (H3O)2-[Ru(NO)Cl 5] could not be located from the difference Fourier map and were therefore omitted. Both oxygens of the H 3O + ions in (H3O)2-[Ru(NO)Cl 5] were surrounded by nine chlorines of the [RuCl5(NO)]2anions in the range 3.32-3.65 Å, allowing weak interactions and several orientations of the H 3O + ions. The crystallographic data are collected in Table 1. Formation of Ru(dcbpy)Cl 3(NO) (1) (dcbpy ) 4,4′-Dicarboxy-2,2′-bipyridine).A 50 mg sample of Ru(4,4′-dmbpy)(CO) 2Cl2, 4 mL of hydrochloric acid (37%), and 50 µL of nitric acid (65%) were introduced into a 60 mL Berghof pressure vessel. The reaction mixture was heated to 240°C (temperature was maintained at 240°C for 2.5 h) and cooled slowly to room temperature (cooling rate about 16°C/ h). Dark red crystals (15.4 mg) formed during the cooling period were separated from the red solution by filtration and dried in air. The solid product was analyzed by X-ray diffraction and IR spectroscopic measurements as well as by elemental analysis. Anal. Calcd for 1: C, 29.95; N, 8.74; H, 1.68. Found: C, 30.05; N, 8.46; H, 1.59. IR (in KBr): ν(NO) 1912 ...

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Section: Resultssupporting

confidence: 77%

Formation of Ruthenium Nitrosyl Complexes: Reactions of Ru(bpy)(CO)₂Cl₂and Its Methyl-Substituted Analogues Ru(4,4‘-dmbpy)(CO)₂Cl₂and Ru(6,6‘-dmbpy)(CO)₂Cl₂in Oxidizing Acidic Solutions

et al. 1997

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“…To synthesize the Au x Ru 1Àx solid-solution NPs, we controlled the reduction speed of the precursors by choosing appropriate coordinating ligands of the metal precursors because the ligands can profoundly affect the ions' stability and reduction potential, and thus their reduction kinetics can be desirably tuned. 25 Potassium pentachloronitrosylruthenate(II) (K 2 Ru(NO)Cl 5 ) 39 and hydrogen tetrabromoaurate(III) hydrate (HAuBr 4 $nH 2 O) were chosen as metal precursors to form the solid-solution alloy NPs. Au x Ru 1Àx solid-solution NPs were synthesized using a polyol reduction method.…”

Section: Synthesis and Characterizationmentioning

confidence: 99%

Solid-solution alloy nanoparticles of a combination of immiscible Au and Ru with a large gap of reduction potential and their enhanced oxygen evolution reaction performance

Zhang

Kusada

et al. 2019

Chem. Sci.

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“…The AuRu 3 solid-solution NPs were synthesized using a polyol reduction method. For the synthesis of the fcc alloy NPs, hydrogen tetrabromoaurate (III) hydrate (HAuBr 4 ·nH 2 O) and potassium pentachloronitrosylruthenate (II) (K 2 Ru(NO)Cl 5 ) 12 were dissolved in diethylene glycol (DEG) with a 1:3 molar ratio. Then, the metal precursor solution was slowly dropped into an ethylene glycol (EG) solution containing polyvinylpyrrolidone (PVP) at 190 °C.…”

Section: Resultsmentioning

confidence: 99%

Selective control of fcc and hcp crystal structures in Au–Ru solid-solution alloy nanoparticles

et al. 2018

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Binary solid-solution alloys generally adopt one of three principal crystal lattices—body-centred cubic (bcc), hexagonal close-packed (hcp) or face-centred cubic (fcc) structures—in which the structure is dominated by constituent elements and compositions. Therefore, it is a significant challenge to selectively control the crystal structure in alloys with a certain composition. Here, we propose an approach for the selective control of the crystal structure in solid-solution alloys by using a chemical reduction method. By precisely tuning the reduction speed of the metal precursors, we selectively control the crystal structure of alloy nanoparticles, and are able to selectively synthesize fcc and hcp AuRu3 alloy nanoparticles at ambient conditions. This approach enables us to design alloy nanomaterials with the desired crystal structures to create innovative chemical and physical properties.

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The crystal and molecular structure of potassium pentachloronitrosylruthenate(II), K₂[Ru(NO)Cl₅]

Cited by 43 publications

References 8 publications

Formation of Ruthenium Nitrosyl Complexes: Reactions of Ru(bpy)(CO)₂Cl₂and Its Methyl-Substituted Analogues Ru(4,4‘-dmbpy)(CO)₂Cl₂and Ru(6,6‘-dmbpy)(CO)₂Cl₂in Oxidizing Acidic Solutions

Formation of Ruthenium Nitrosyl Complexes: Reactions of Ru(bpy)(CO)₂Cl₂and Its Methyl-Substituted Analogues Ru(4,4‘-dmbpy)(CO)₂Cl₂and Ru(6,6‘-dmbpy)(CO)₂Cl₂in Oxidizing Acidic Solutions

Solid-solution alloy nanoparticles of a combination of immiscible Au and Ru with a large gap of reduction potential and their enhanced oxygen evolution reaction performance

Selective control of fcc and hcp crystal structures in Au–Ru solid-solution alloy nanoparticles

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The crystal and molecular structure of potassium pentachloronitrosylruthenate(II), K2[Ru(NO)Cl5]

Cited by 43 publications

References 8 publications

Formation of Ruthenium Nitrosyl Complexes: Reactions of Ru(bpy)(CO)2Cl2and Its Methyl-Substituted Analogues Ru(4,4‘-dmbpy)(CO)2Cl2and Ru(6,6‘-dmbpy)(CO)2Cl2in Oxidizing Acidic Solutions

Formation of Ruthenium Nitrosyl Complexes: Reactions of Ru(bpy)(CO)2Cl2and Its Methyl-Substituted Analogues Ru(4,4‘-dmbpy)(CO)2Cl2and Ru(6,6‘-dmbpy)(CO)2Cl2in Oxidizing Acidic Solutions

Solid-solution alloy nanoparticles of a combination of immiscible Au and Ru with a large gap of reduction potential and their enhanced oxygen evolution reaction performance

Selective control of fcc and hcp crystal structures in Au–Ru solid-solution alloy nanoparticles

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The crystal and molecular structure of potassium pentachloronitrosylruthenate(II), K₂[Ru(NO)Cl₅]

Formation of Ruthenium Nitrosyl Complexes: Reactions of Ru(bpy)(CO)₂Cl₂and Its Methyl-Substituted Analogues Ru(4,4‘-dmbpy)(CO)₂Cl₂and Ru(6,6‘-dmbpy)(CO)₂Cl₂in Oxidizing Acidic Solutions

Formation of Ruthenium Nitrosyl Complexes: Reactions of Ru(bpy)(CO)₂Cl₂and Its Methyl-Substituted Analogues Ru(4,4‘-dmbpy)(CO)₂Cl₂and Ru(6,6‘-dmbpy)(CO)₂Cl₂in Oxidizing Acidic Solutions