Reactions of metalloalkynes 3. Facile synthesis of pentanuclear ruthenium clusters. X-ray structures of [Ru5(μ5-CC)(η-C5H4R)2(dppm)(μ2-CO)2(CO)7] (R=H, CH3)

Byrne, Lindsay T.; Griffith, Christopher S.; Hos, James P; Koutsantonis, George A.; Skelton, Brian W.; White, Allan H.

doi:10.1016/s0022-328x(98)00525-7

Cited by 20 publications

(5 citation statements)

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“…We have found that the CpRu(CO) 2 moiety is extremely flexible in its mode of coordination and has allowed us to investigate a number of unusual − bonding situations. Thus, we first decided to attempt the formation of mono-alkynyl complexes to provide suitable models for the formation of oligomeric complexes.…”

Section: Resultsmentioning

confidence: 99%

Coordinating Tectons: Bipyridyl-Terminated Group 8 Alkynyl Complexes

et al. 2009

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The pendant bipyridyl moiety of transition metal σ-acetylide complexes incorporating the 5-ethynyl-2,2′-bipyridine moiety provides a site of chelation for additional metal centers and facile access to multinuclear complexes as model systems for organometallic "molecular wires". The mononuclear complexes [CpRu(CO) 2 (C 2 bpy)] (Cp ) C 5 H 5 , C 5 Me 5 ) and [RuCl(P∩P) 2 (C 2 bpy)] (P∩P ) dppm, dppe) have been synthesized and characterized through spectroscopic means, providing context for the synthesis and spectroscopic characterization of the heterometallic coordination complex [RuCl(dppe) 2 (C 2 bpy-κ 2 -N,N′-PdCl 2 )]. A number of the complexes were further characterized by solid-state X-ray structural determinations. These studies were extended to other metal ligand systems, and the structures of the tris-bidentate ruthenium(II) complex [Ru(bpy) 2 (5-ethynyl-2,2′-bipyridine)](PF 6 ) 2 and gold(I) σ-alkynyl complexes [(PR 3 )Au(C 2 bpy)] (PR 3 ) PEt 3 , PPh 3 ) are reported.

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Section: Resultsmentioning

confidence: 99%

Coordinating Tectons: Bipyridyl-Terminated Group 8 Alkynyl Complexes

et al. 2009

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“…In this paper we present the results of the synthesis and structural characterization of some coinage metal (Cu and Ag) adducts of [{Ru(CO) 2 (η-C 5 H 4 R)} 2 (μ 2 -CC)] ( 1a , R = H; 1b , R = Me), continuing an investigation of ruthenium ethyne-1,2-diyl complexes. − The structures of the adducts were probed in solution and the solid state, resulting in the single-crystal X-ray structure determinations of [Ag 3 ({Ru(CO) 2 (η-C 5 H 4 Me)} 2 (μ 2 -η 1 :η 1 -CC)) 3 ](O 3 SCF 3 ) 3 ( 2b ), [Ag 3 ({Ru(CO) 2 (η-C 5 H 4 R)} 2 (μ 2 -η 1 :η 1 -CC))({Ru(CO) 2 (η-C 5 H 4 R)} 2 (μ 2 -η 1 :η 2 -CC)) 2 ](BF 4 ) 3 (R = H, 3a ; R = Me, 3b ), [Ag 4 ({Ru(CO) 2 (η-C 5 H 4 R)} 2 (μ 2 -η 2 -CC)) 2 ](μ 2 -O 2 CCF 3 ) 4 (R = H, 4a ; Me, 4b ), [Ag({Ru(CO) 2 (η-C 5 H 5 )} 2 (η 2 -CC)) 2 ](BF 4 ) ( 5 ), [Cu({Ru(CO) 2 (η-C 5 H 5 )} 2 (η 2 -CC)) 2 ](PF 6 ) ( 6 ), [Cu 3 ({Ru(CO) 2 (η-C 5 H 5 )} 2 (μ 2 -η 1 :η 2 -CC))({Ru(CO) 2 (η-C 5 H 5 )} 2 (μ 2 -η 2 -CC))](PF 6 ) 3 ( 7a ), [Cu 3 ({Ru(CO) 2 (η-C 5 H 4 Me)} 2 (μ 2 -η 1 :η 2 -CC)) 3 ](PF 6 ) 3 ( 7b ), [Cu 2 (μ-Cl) 2 ({Ru(CO) 2 (η-C 5 H 4 R)} 2 (η 2 -CC))] ∞/∞∞ (R = H, 8a ; R = Me, 8b ), [Cu 2 (μ-Br) 2 ({Ru(CO) 2 (η-C 5 H 4 Me)} 2 (η 2 -CC))] ( 9 ), and [{Ru(CO) 2 (η-C 5 H 5 )} 3 (η 1 : η 2 -CC))][BF 4 ] ( 10 ).…”

Section: Introductionmentioning

confidence: 99%

Anion-Directed Solid-State Structures of Copper(I) and Silver(I) Adducts of Ruthenium Ethyne-1,2-diyl Compounds

et al. 2015

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A number of group 11 salts, [MX] (M = Ag, X– = –O3SCF3, –O2CCF3, BF4 –; M = Cu; X = Cl, Br) and [Cu(MeCN)4][PF6], were found to react in varying stoichiometries with ethyne-1,2-diyl compounds, [{Ru(CO)2(η-C5H4R)}2(μ2-CC)] (R = H, Me), to give a number of complex cations. The trication salts [Ag3({Ru(CO)2(η-C5H4Me)}2(μ2-η1:η1-CC))3](O3SCF3)3, [Ag3({Ru(CO)2(η-C5H4R)}2(μ2-η1:η1-CC))({Ru(CO)2(η-C5H4R)}2(μ2-η1:η2-CC))2](BF4)3, and [Cu3({Ru(CO)2(η-C5H4R)}2(μ2-η1:η2-CC))({Ru(CO)2(η-C5H4R)}2(μ2-η2-CC))](PF6)3 result from the use of the respective anion salts in their syntheses. Coordination of Ag+ by the ethyne-1,2-diyl complexes in the presence of F3CCO2 – yields the tetranuclear complexes [Ag4({Ru(CO)2(η-C5H4R)}2(μ2-η2-CC))2](μ2-O2CCF3)4 (R = H, Me). The reaction of CuCl does not afford the discrete dimeric complexes normally observed for internal alkynes and metal alkynyl complexes but, rather, the 1-D polymer [Cu2(μ-Cl)2({Ru(CO)2(η-C5H4R)}2(η2-CC))](∞|∞), while CuBr gives the discrete dimer motif known in the literature. The solution structures at 1/2, 1/1, and 2/1 stoichiometries of Ag+/[{Ru(CO)2(η-C5H5)}2(μ2-CC)] have been probed spectroscopically, and the {Ru(CO)2(η-C5H4R)} environments appear to be equivalent and, likewise, the resonances attributable to their CC units. In a subsequent reaction of [{Ru(CO)2(η-C5H4R)}2(μ2-CC)] and AgBF4 use of a strict Ag+/ethyne-1,2-diyl ratio gave [Ag({Ru(CO)2(η-C5H5)}2(η2-CC))2](BF4). The analogous Cu+ adduct [Cu({Ru(CO)2(η-C5H5)}2(η2-CC))2](PF6) is observed, along with the tricopper(I) adduct from the reaction of [{Ru(CO)2(η-C5H4R)}2(μ2-CC)] and [Cu(NCMe)4](PF6). A combination of factors appears to control the solid-state structures of these coinage metal adducts, with the anion found to be that which influences the packing to the greatest extent.

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“…[10][11][12] We have for some considerable time explored the chemistry associated with the CpRu(CO) 2 moiety because of the conformational flexibility it exhibits, which has allowed the isolation of many interesting complexes. [13][14][15][16][17][18][19][20][21][22] In the course of preparing [CpRu(CO) 2 Br] using a minor modification of the published procedure 23 (using bromoform rather than CBr 4 ) we discovered that the reaction did not proceed according to our expectations, Scheme 1, giving not only the expected bromide complex but also gave appreciable contamination with hexabromoethane.…”

Section: Introductionmentioning

confidence: 99%