Synthesis of cluster compounds via nucleophilic metal complexes; X-ray crystal structures of [Os3Pt(µ-H)2(CO)10{(C6H11)3P}] and [Os2Pt2(µ-H)2(CO)8(Ph3P)2]

Farrugia, Louis J.; Howard, Judith A. K.; Mitrprachachon, P.; Spencer, John L.; Stone, F. Gordon A.; Woodward, Peter

doi:10.1039/c39780000260

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“…)-C(l1)-O(I1) 168.0(10) Ru(3)-C(33)-0(33) 171.2(14) though a detailed study has been carried out2 1 on [Ru3(p-H),-(p3-CMe)(C0)9] which differs only in the ligand on the triplybridging carbyne species. Surprisingly, in the light of the results for (2), comparison of (3) with [Ru3(p-H),(p-CMe)-(CO),] reveals differences which are only marginally significant except, of course, for the reduction of symmetry consequent upon replacement of one bridging hydrido-ligand by AuPPh,.…”

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confidence: 99%

Replacement of hydrido-ligands in triruthenium complexes by triphenylphosphinegold groups. Crystal structures of [AuRu₃(µ-COMe)(CO)₁₀(PPh₃)], [AuRu₃(µ-H)₂(µ₃-COMe)(CO)₉(PPh₃)], and [Au₃Ru₃(µ₃-COMe)(CO)₉(PPh₃)₃]

Batsman¹,

Green²,

Mead³

et al. 1983

J. Chem. Soc., Dalton Trans.

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The compound [AuMe( PPh3)] reacts under mild conditions (diethyl ether, ambient temperatures) with the compounds [M3(p-H) (p-COMe) (CO),o] and [ R u ~( ~-H ) ~( ~~-C O M ~) ( C O ) ~] to give the complexes [ A U M , ( ~-C O M ~) ( C O ) , ~( P P ~~) ~ [M = Fe ( 1 ) or Ru ( 2 ) L [ A ~R u ~( c L -H ) ~( c L ~-C O M ~) ( C O ) ~( P P ~~) ~ ( 3 ) , Spectroscopic properties of the new species are reported and discussed, and the structures of ( 2 ) , ( 3 ) , and (5) have been established by X-ray diffraction studies. The structure of [AuRu3(p-COMe) (CO),,( PPh3)] ( 2 ) can be regarded as a molecule of [ R u ~( ~-H ) ( ~-C O M ~) ( C ~) , ~]in which the bridging hydrido-ligand is replaced by a bridging AuPPh, group, thus producing a ' butterfly ' metal atom core (interplanar angle 1 17") with the gold atom occupying a ' wing-tip ' site. The COMe ligand bridges the body of the butterfly on the convex side. The Au-Ru bonds [2.760(2) and 2.762(2) A] are ca. 0.1 A shorter than the non-bridged Ru-Ru bonds [2.845(2) and 2.839(3) A] but the bridged Ru-Ru bond is significantly longer at 2.879(2) A. Crystals of ( 2 ) are triclinic, space group P i , and the asymmetric unit comprises two molecules of complex. The structure has been refined to R 0.075 for 4 868 intensities measured to 29 = 40" at 220 K. In [ A U R U , ( ~-H ) ~( ~~-C O M ~) ( C O ) ~( P P ~~) ] ( 3 ) the carbyne ligand triply bridges an equilateral triangle [Ru-Ru 2.865(2)-2.879(2) A] of ruthenium atoms, while on the opposite side of the triangle there are two edge-bridging hydrido-ligands and one edge-bridging AuPPh, group. Each ruthenium atom carries three terminal carbonyl ligands, giving octahedral co-ordination if the Ru-Ru bonds are ignored. The molecule has approximate C, symmetry, not required crystallographically. The structure is triclinic, space group P i , and has been refined to R 0.042 for 3 247 intensities measured to 28 = 45" at 293 K. The complex [ A U ~R U , ( ~~-C O M ~) ( C ~) ~( P P ~~) ~] (5) crystallises with half a molecule of CH2CI2 per molecule of (5) incorporated into the crystals. Again the carbyne ligand triply bridges a near-equilateral triangle of Ru atoms [Ru-Ru 2.895(3)-2.929(2) A], but on the opposite side of this triangle one gold atom is co-ordinated to form a tetrahedron [Au-Ru 2.818(2), 2.825(2), and 2.987(2) A]. The two faces of this tetrahedron adjacent to the long Au-Ru bond are each further

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confidence: 99%

Replacement of hydrido-ligands in triruthenium complexes by triphenylphosphinegold groups. Crystal structures of [AuRu₃(µ-COMe)(CO)₁₀(PPh₃)], [AuRu₃(µ-H)₂(µ₃-COMe)(CO)₉(PPh₃)], and [Au₃Ru₃(µ₃-COMe)(CO)₉(PPh₃)₃]

Batsman¹,

Green²,

Mead³

et al. 1983

J. Chem. Soc., Dalton Trans.

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“…The overall configuration is comparable with that of [AuRu,(p-COMe) (CO),o(PPh3)]11 in that the 'butterfly' configuration of the Ru( l)-Ru(3) 2.879(2), Ru(l)-Ru(2) 2.875(2), Ru(3)-Ru(2) 2.865(2), Au-P 2.308(3), Ru(l)-C(4) 2.11 5( 13), Ru(2)-C(4) 2.065(1 I), Phenyl rings omitted for clarity. Dimensions : Ru(1)-Ru(2) 2.979 (6), Ru( l)-Ru(4) 3.001(5), R u ( ~) -R u ( ~) 2.962 (8), Ru(3)-Ru(4) 2.803(5), Ru(l)-Ru(3) 2.81 5 (6), Ru(2)-Ru(3) 2.802(8), Au( 1)-Ru(1) 2.838(5), Au(2)-Ru(l) 2.844 (7), Au(3)-Ru(l) 2.839(5), Au(2)-Ru(2) 2.843(4), Au(3)-Ru(2) 3.012(4), Au(1)-Ru(4) 2.825(4), Au(3)-Ru(4) 2.956 (6), Au(l)-Au(3) 2.81 9(4), A u ( ~) -A u ( ~) 2.842(3), Au(1) -P(1) 2.27(2), A u ( ~) -P ( ~) 2.30(2), Au(3)-P(3) 2.30 (1). metal atom core is sitnilar, with the gold atom occupying one of the wing-tips.…”

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confidence: 99%

“…Molecular structure of [Au,Ru,( p-H)(CO),,(PPh,),] (4).Phenyl rings omitted for clarity. Dimensions : Ru(1)-Ru(2) 2.979(6), Ru( l)-Ru(4) 3.001(5), R u ( ~) -R u ( ~) 2.962(8), Ru(3)-Ru(4) 2.803(5), Ru(l)-Ru(3) 2.81 5(6), Ru(2)-Ru(3) 2.802(8), Au( 1)-Ru(1) 2.838(5), Au(2)-Ru(l) 2.844(7), Au(3)-Ru(l) 2.839(5), Au(2)-Ru(2) 2.843(4), Au(3)-Ru(2) 3.012(4), Au(1)-Ru(4) 2.825(4), Au(3)-Ru(4) 2.956(6), Au(l)-Au(3) 2.81 9(4), A u ( ~) -A u ( ~) 2.842(3), Au(1) -P(1) 2.27(2), A u ( ~) -P ( ~) 2.30(2), Au(3)-P(3) 2.30(1).…”

mentioning

confidence: 99%

Replacement of hydrido-ligands in [Ru₃(µ-H)₃(µ-H)₃(µ₃-COMe)(CO)₉] and [Ru₄(µ-H)₄(CO)₁₂] by triphenylphosphinegold groups: X-ray crystal structures of [AuRu₃(µ-H)₂(µ-COMe)(CO)₉(PPh₃)], [Au₃Ru₃(µ-COMe)(CO)₉(PPh₃)₃], and [Au₃Ru₄(µ-H)(CO)₁₂(PPh₃)₃]

Bateman¹,

Green²,

Howard³

et al. 1982

J. Chem. Soc., Chem. Commun.

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“…The structural relationship between 5 and 6c is of particular interest. The replacement of a μ -H group in a M( μ -H)M system by the isolobal μ -Au(PPh 3 ) group was first recognized 20 years ago, and the methodology was subsequently developed to prepare many heteronuclear metal clusters with μ -Au(PR 3 ) groups . Hence, treatment of 4b with [Au(PPh 3 )] + might have been anticipated to yield a molecule wherein the gold fragment bridges a Ru−Ru bond as does the bridging hydrido ligand H(23) of 5 (Figure ).…”

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confidence: 99%

Synthesis and Reactions of the Triruthenamonocarboncarborane Cluster Complex [NHMe₃][Ru₃(CO)₈(η⁵-7-CB₁₀H₁₁)]

1999

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In thf (tetrahydrofuran) at reflux temperatures the compounds [Ru 3 (CO) 12 ] and [NHMe 3 ]-[nido-7-CB 10 H 13 ] give the anionic triruthenium complex [Ru 3 (CO) 8 (η 5 -7-CB 10 H 11 )] -, characterized as its [PPh 4 ] + salt (4a). Protonation of [NHMe 3 ][Ru 3 (CO) 8 (η 5 -7-CB 10 H 11 )] (4b) with HBF 4 ‚ Et 2 O yields the hydrido cluster complex [Ru 3 (µ-H)(CO) 8 (η 5 -7-CB 10 H 11 )] (5), the structure of which has been determined by X-ray diffraction. The molecule has a triangle of ruthenium atoms. One ruthenium atom is ligated by the η 5 -7-CB 10 H 11 cage system and carries two CO groups, while the other two ruthenium atoms each carry three CO molecules with a hydrido ligand bridging the metal-metal bond which joins them. In addition, these two metal atoms are linked to the cage through two exopolyhedral B-HFRu bonds. These are formed using boron atoms lying in sites with respect to the carbon in the open CBBBB face of the nido-CB 10 H 11 fragment ligating the Ru(CO) 2 group. Treatment of 4b in thf with [CuCl(PPh 3 ) 3 ] in the presence of TlPF 6 , or with Ag[BF 4 ] and PPh 3 , affords the bimetallic complexes [Ru 3 (µ-H)(CO) 7 (PPh 3 ){η 5 -10-M(PPh 3 )-7-CB 10 H 10 }] (M ) Cu (6a), Ag (6b)), respectively. The structure of 6a was established by X-ray diffraction. A triangle of ruthenium atoms is formed by Ru-(CO) 2 , Ru(CO) 3 , and Ru(CO) 2 (PPh 3 ) units. This triangle is bridged by a nido-10-Cu(PPh 3 )-7-CB 10 H 10 fragment, the open CBBBB face of which is η 5 -coordinated to the Ru(CO) 2 group.The two boron atoms lying in the -sites in the CBBBB ring coordinated to the Ru(CO) 2 moiety form exopolyhedral B-H F Ru and B-CufRu linkages, respectively, to the Ru-(CO) 2 (PPh 3 ) and Ru(CO) 3 groups, which have their Ru-Ru bond bridged by a hydrido ligand. A novel feature of the structure is a three-center-two-electron B-HFCu bond involving the B(2) site in the nido-10-Cu(PPh 3 )-7-CB 10 H 10 cage system. The reaction between 4b and [AuCl(PPh 3 )] gives [Ru 3 (µ-H)(CO) 8 {η 5 -10-Au(PPh 3 )-7-CB 10 H 10 }] (6c), the structure of which was also determined by X-ray crystallography. It is similar to that of 6a, except there is no exopolyhedral B-HFAu bond supplementing the B(10)-AufRu and Au-P bonds.

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Synthesis of cluster compounds via nucleophilic metal complexes; X-ray crystal structures of [Os₃Pt(µ-H)₂(CO)₁₀{(C₆H₁₁)₃P}] and [Os₂Pt₂(µ-H)₂(CO)₈(Ph₃P)₂]

Cited by 50 publications

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Replacement of hydrido-ligands in triruthenium complexes by triphenylphosphinegold groups. Crystal structures of [AuRu₃(µ-COMe)(CO)₁₀(PPh₃)], [AuRu₃(µ-H)₂(µ₃-COMe)(CO)₉(PPh₃)], and [Au₃Ru₃(µ₃-COMe)(CO)₉(PPh₃)₃]

Replacement of hydrido-ligands in triruthenium complexes by triphenylphosphinegold groups. Crystal structures of [AuRu₃(µ-COMe)(CO)₁₀(PPh₃)], [AuRu₃(µ-H)₂(µ₃-COMe)(CO)₉(PPh₃)], and [Au₃Ru₃(µ₃-COMe)(CO)₉(PPh₃)₃]

Replacement of hydrido-ligands in [Ru₃(µ-H)₃(µ-H)₃(µ₃-COMe)(CO)₉] and [Ru₄(µ-H)₄(CO)₁₂] by triphenylphosphinegold groups: X-ray crystal structures of [AuRu₃(µ-H)₂(µ-COMe)(CO)₉(PPh₃)], [Au₃Ru₃(µ-COMe)(CO)₉(PPh₃)₃], and [Au₃Ru₄(µ-H)(CO)₁₂(PPh₃)₃]

Synthesis and Reactions of the Triruthenamonocarboncarborane Cluster Complex [NHMe₃][Ru₃(CO)₈(η⁵-7-CB₁₀H₁₁)]

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Synthesis of cluster compounds via nucleophilic metal complexes; X-ray crystal structures of [Os3Pt(µ-H)2(CO)10{(C6H11)3P}] and [Os2Pt2(µ-H)2(CO)8(Ph3P)2]

Cited by 50 publications

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Replacement of hydrido-ligands in triruthenium complexes by triphenylphosphinegold groups. Crystal structures of [AuRu3(µ-COMe)(CO)10(PPh3)], [AuRu3(µ-H)2(µ3-COMe)(CO)9(PPh3)], and [Au3Ru3(µ3-COMe)(CO)9(PPh3)3]

Replacement of hydrido-ligands in triruthenium complexes by triphenylphosphinegold groups. Crystal structures of [AuRu3(µ-COMe)(CO)10(PPh3)], [AuRu3(µ-H)2(µ3-COMe)(CO)9(PPh3)], and [Au3Ru3(µ3-COMe)(CO)9(PPh3)3]

Replacement of hydrido-ligands in [Ru3(µ-H)3(µ-H)3(µ3-COMe)(CO)9] and [Ru4(µ-H)4(CO)12] by triphenylphosphinegold groups: X-ray crystal structures of [AuRu3(µ-H)2(µ-COMe)(CO)9(PPh3)], [Au3Ru3(µ-COMe)(CO)9(PPh3)3], and [Au3Ru4(µ-H)(CO)12(PPh3)3]

Synthesis and Reactions of the Triruthenamonocarboncarborane Cluster Complex [NHMe3][Ru3(CO)8(η5-7-CB10H11)]

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Synthesis of cluster compounds via nucleophilic metal complexes; X-ray crystal structures of [Os₃Pt(µ-H)₂(CO)₁₀{(C₆H₁₁)₃P}] and [Os₂Pt₂(µ-H)₂(CO)₈(Ph₃P)₂]

Replacement of hydrido-ligands in triruthenium complexes by triphenylphosphinegold groups. Crystal structures of [AuRu₃(µ-COMe)(CO)₁₀(PPh₃)], [AuRu₃(µ-H)₂(µ₃-COMe)(CO)₉(PPh₃)], and [Au₃Ru₃(µ₃-COMe)(CO)₉(PPh₃)₃]

Replacement of hydrido-ligands in triruthenium complexes by triphenylphosphinegold groups. Crystal structures of [AuRu₃(µ-COMe)(CO)₁₀(PPh₃)], [AuRu₃(µ-H)₂(µ₃-COMe)(CO)₉(PPh₃)], and [Au₃Ru₃(µ₃-COMe)(CO)₉(PPh₃)₃]

Synthesis and Reactions of the Triruthenamonocarboncarborane Cluster Complex [NHMe₃][Ru₃(CO)₈(η⁵-7-CB₁₀H₁₁)]