Chemistry of the metal carbonyls. Part LV. Synthesis of polynuclear carbonyl(iron–ruthenium) complexes

Yawney, D. B. W.; Stone, F. G. A.

doi:10.1039/j19690000502

Cited by 71 publications

(14 citation statements)

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“…Preparation of H2FeRu3(CO)i3. Reaction of Ru3(CO) 12 with Na2[Fe(CO)4] leads to formation of the known12•13 H2Fe-Ru3(CO)i3. The product was identified by its infrared and mass spectrum, and a 49% yield was obtained when the THF solution of Ru3(CO)i2 and Na2[Fe(CO)4] was refluxed for 75 min.…”

Section: Resultsmentioning

confidence: 99%

Synthesis of tetrahedral mixed-metal clusters of the iron triad. Preparation and characterization of tridecacarbonyldihydroironosmiumdiruthenium and tridecacarbonyldihydroirondiosmiumruthenium

Geoffroy

Gladfelter

1977

J. Am. Chem. Soc.

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Several new mixed-metal clusters of the Fe-Ru-Os triad have been prepared through the addition of carbonylmetalates to closed metal trimers. Addition of Na2[Fe(CO)4] to Ru2Üs(CO)i2 and RuOs2(CO)i2, followed by acidification, yielded Fl2FeRu20s(C0)i3 and H2FeRuOs2(CO)i3, the first examples of clusters comprised of three different transition metals. F)2Fe2Ru2(CO)i3 was prepared by allowing Na2[Fe(CO)4] to react with Fe2Ru(CO)i2 or by addition of [Ru(CO)4]2-to Fe3(CO)i2-Addition of [Ru(CO)4]2_ to Os3(CO)i2 or [Os(CO)4]2~t o Ru3(CO)¡2 gave an inseparable mixture of H4Ru4(CO)i2, H4Ru3Os(CO)12, H4Ru20s2(C0)12, H4RuOs3(CO)i2, and H4Os4(CO)i2. An improved synthesis of FFFe-Ru3(CO)i3 is reported and an alternative route to Fl2FeOs3(CO)i3 is described. The new clusters have been characterized by their NMR, infrared, electronic absorption, and mass spectra and the spectral evidence suggests tetrahedral structures similar to the known structures of H2FeRu3(CO)i3 and FI2Ru4(CO)i3.

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Section: Resultsmentioning

confidence: 99%

Synthesis of tetrahedral mixed-metal clusters of the iron triad. Preparation and characterization of tridecacarbonyldihydroironosmiumdiruthenium and tridecacarbonyldihydroirondiosmiumruthenium

Geoffroy

Gladfelter

1977

J. Am. Chem. Soc.

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“…Samples of Fe 2 Ru(CO) 12 , FeRu 2 (CO) 12 and Fe 3 (CO) 12 were prepared by literature methods, and recrystallized from dichloromethane/hexane solutions to give crystals suitable for the single-crystal studies.…”

Section: Methodsmentioning

confidence: 99%

Dynamic Disorder and Fluxionality in M₃(CO)₁₂Clusters: Variable-Temperature X-ray Diffraction Studies on Fe_nRu₃_-_n(CO)₁₂(n= 1, 2) and the Low-Temperature Phase of Fe₃(CO)₁₂

et al. 1999

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The metal atom disorder in the crystalline clusters Fe2Ru(CO)12 (1) and FeRu2(CO)12 (2) has been shown to be dynamic in origin. At and below 313 K, 1 crystallizes in the noncentrosymmetric space group Pn with two independent molecules in the asymmetric unit, both molecules having approximate C 2 v symmetry with small C 2 distortions. Above 313 K, crystals of 1 undergo a phase transition to the centrosymmetric space group P21/n, becoming isomorphous and isostructural with the room-temperature phase of Fe3(CO)12 (3). These reversible changes are accompanied by an increase in the metal atom disorder, from a completely ordered structure at 223 K to a statistically disordered (1:1) “Star of David” structure at 323 K. Crystals of 2 show similar behavior, belonging to the noncentrosymmetric space group C2cb below 228 K and undergoing a phase transition to the centrosymmetric space group Ccmb above this temperature. An increase in the extent of disorder is observed in 2, from an ordered structure at 173 K to the extended Star of David disorder above the phase transition temperature. Compound 2 has an all-terminal carbonyl arrangement, with a strong D 3 distortion, and provides the first example of the D 3 structural type for a homoleptic M3(CO)12 cluster. In contradiction to our earlier studies, Fe3(CO)12 (3) has now been shown to undergo a phase transition at ∼210 K to a second monoclinic phase with a partial ordering of the metal atom triangles. The asymmetric unit comprises four complete and one half-molecule of 3, and one of these molecules (3a) is completely ordered. The thermal motion in 1 and the structures of 1−3 have been examined in the context of the various proposed fluxional mechanisms in M3(CO)12 clusters.

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“…The structure of [FeRu 2 (CO) 12 ] 7 proved surprisingly interesting. 65 Earlier IR 53, 68 and Mössbauer 69 studies had indicated an all-terminal structure, possibly with a D 3 distortion. Venäläinen and Pakkanen 70 reported a room-temperature unit cell, but could not resolve the disorder.…”

Section: Fluxionality In [M 3 (Co) 12 ] (M = Fe Ru or Os)mentioning

confidence: 98%

Dynamics and fluxionality in metal carbonyl clusters: some old and new problems

Farrugia¹

1997

J. Chem. Soc., Dalton Trans.

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Chemistry of the metal carbonyls. Part LV. Synthesis of polynuclear carbonyl(iron–ruthenium) complexes

Cited by 71 publications

References 0 publications

Synthesis of tetrahedral mixed-metal clusters of the iron triad. Preparation and characterization of tridecacarbonyldihydroironosmiumdiruthenium and tridecacarbonyldihydroirondiosmiumruthenium

Synthesis of tetrahedral mixed-metal clusters of the iron triad. Preparation and characterization of tridecacarbonyldihydroironosmiumdiruthenium and tridecacarbonyldihydroirondiosmiumruthenium

Dynamic Disorder and Fluxionality in M₃(CO)₁₂Clusters: Variable-Temperature X-ray Diffraction Studies on Fe_nRu₃_-_n(CO)₁₂(n= 1, 2) and the Low-Temperature Phase of Fe₃(CO)₁₂

Dynamics and fluxionality in metal carbonyl clusters: some old and new problems

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Chemistry of the metal carbonyls. Part LV. Synthesis of polynuclear carbonyl(iron–ruthenium) complexes

Cited by 71 publications

References 0 publications

Synthesis of tetrahedral mixed-metal clusters of the iron triad. Preparation and characterization of tridecacarbonyldihydroironosmiumdiruthenium and tridecacarbonyldihydroirondiosmiumruthenium

Synthesis of tetrahedral mixed-metal clusters of the iron triad. Preparation and characterization of tridecacarbonyldihydroironosmiumdiruthenium and tridecacarbonyldihydroirondiosmiumruthenium

Dynamic Disorder and Fluxionality in M3(CO)12Clusters: Variable-Temperature X-ray Diffraction Studies on FenRu3-n(CO)12(n= 1, 2) and the Low-Temperature Phase of Fe3(CO)12

Dynamics and fluxionality in metal carbonyl clusters: some old and new problems

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Dynamic Disorder and Fluxionality in M₃(CO)₁₂Clusters: Variable-Temperature X-ray Diffraction Studies on Fe_nRu₃_-_n(CO)₁₂(n= 1, 2) and the Low-Temperature Phase of Fe₃(CO)₁₂