31P and 195Pt nmr studies on the triangular cluster complexes [Pt3(μ-CO)3(tertiary phosphine)4]

Moor, A.; Pregosin, Paul S.; Venanzi, L. M.

doi:10.1016/s0020-1693(00)89131-8

Cited by 38 publications

(4 citation statements)

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“…6b and 6c consist of a Fe(CO) 2 (PPh 3 ) group attached to [Pt 2 (μ 2 -η 1 :η 1 -C 4 Ph 2 )(CO) 2 (PPh 3 ) 2 ]. For 6b , a 31 P NMR resonance arising from the Fe(CO) 2 (PPh 3 ) group was observed at 65.7 ppm, while resonances arising from the Pt 2 (PhCCCCPh)(CO) 2 (PPh 3 ) 2 group appeared at 29.94 ( 1 J Pt,P = 2841.8 Hz) and 25.11 ppm ( 1 J Pt,P = 3991.5 Hz) with a nuclear spin system A 2 M 2 , but 2 J Pt,P as observed for 6a could not be discerned in this case. Clusters with a disymmetrical alkyne, [Pt 2 M(C 2 R 2 )(CO) 5 (PPh 3 ) 2 ] (M = Fe, R = Ph, 6d and iso -6d ; R = OCOCH 3 , M = Fe, 6e ; R = OCOCH 3 , M = Ru, 6f ) were analogously prepared, except for the cases of 6e and 6f , which were prepared by addition reactions of a M(CO) 3 (M = Fe, Ru) group to the Pt(I) dimer, [Pt 2 {μ 2 - η 1 :η 1 -C 2 (CO 2 CH 3 ) 2 }(CO) 2 (PPh 3 ) 2 ] …”

Section: Resultsmentioning

confidence: 99%

Some Mixed Transition Metal Compounds of 1,3-Diyne with Metallacycles Derived by Cross-Coupling of Alkynyl Ligands and Sequential C−C Bond Coupling between 1,3-Diyne and Carbon Monoxide

et al. 2004

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By treating cis-Pt(CtCPh) 2 (dppe) (1) with Mn 2 (CO) 9 (CH 3 CN) in refluxing toluene, crosscoupling of alkynyl ligands occurs to afford mixed transition metal compound of 3,4-diphenyl-1,3-butadiyne, [Mn 2 Pt(µ 3 -η 1 :η 1 :η 2 :η 4 -PhCCCCPh)(CO) 6 (dppe)] (2) in 19-38% isolated yield. 2 has a structure formed by an unprecedented heterometal complexation of 1-manganacyclo-2,3,4-pentatriene. The Pt(II) acetylide, by treating with Ru 3 (CO) 9 (PPh 3 ) 3 , directly converts into a π-complex of 1,3-diyne, Pt(η 2 -PhCCCCPh)(dppe) (4), in 38% yield. By reacting π-alkyne compound Pt(η 2 -PhCC-CtCPh)(PPh 3 ) 2 with Fe(CO) 5 and Ru 3 (CO) 12 , bimetallic [FePt(µ 3η 1 :η 1 :η 2 -COC 4 Ph 2 )(CO) 3 (PPh 3 ) 2 ] (5a) and triangular cluster [MPt 2 (µ 3 -η 1 :η 1 :η 2 -PhCC-CtCPh)-(CO) 5 (PPh 3 ) 2 ] (6a) have successionally been isolated in considerable yields. A dimetallic analogue of alkyne [FePt{µ 2 -η 1 :η) Fe, 6d and iso-6d; R 1 ) R 2 ) OCOCH 3 , n ) 2, M ) Fe, 6e; M ) Ru, 6f} have consecutively been prepared. Crystal structures of five of the compounds have been determined.

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Section: Resultsmentioning

confidence: 99%

Some Mixed Transition Metal Compounds of 1,3-Diyne with Metallacycles Derived by Cross-Coupling of Alkynyl Ligands and Sequential C−C Bond Coupling between 1,3-Diyne and Carbon Monoxide

et al. 2004

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“…Considering that complex 5 can still add two electrons (for tertiary phosphines the triangulo complexes Pt 3 (μ-CO) 3 (PR 3 ) 4 have been reported), 1a,, the 44e - electron complex 2 can, in principle, add a total of 6 electrons, retaining its triangulo structure and original NEV.…”

Section: Resultsmentioning

confidence: 99%

CO-Induced Reductive Elimination of P(t-Bu)₂H from the Platinum(II) Dinuclear Derivative Pt₂[μ-P(t-Bu)₂]₂(H)₂[P(t-Bu)₂H]₂, Affording Mononuclear Platinum(0) or Triangulo Triplatinum(I,I,II) Derivatives

Leoni¹,

Manetti²,

Pasquali³

et al. 1996

Inorg. Chem.

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Carbon monoxide (1 atm) quantitatively converts the Pt(II) dinuclear derivative Pt2[μ-P(t-Bu)2]2(H)2[P(t-Bu)2H]2 (1) into the new PtI 2PtII triangulo cluster Pt3[μ-P(t-Bu)2]3(H)(CO)2 (2). The 44e- species 2 was characterized by IR and multinuclear NMR spectroscopy and by a single-crystal X-ray diffraction study. Complex 2 is formed through the slow CO-induced reductive elimination of P(t-Bu)2H from 1, affording the intermediate mononuclear Pt(0) carbonyl derivative Pt[P(t-Bu)2H]2(CO)2 (4), which equilibrates with the carbonyl-bridged triangulo derivative Pt3[P(t-Bu)2H]3(μ-CO)3 (5); these are the main products under high pressures of CO. Two alternative mechanisms were examined for the subsequent formation of complex 2, the first being the rapid condensation of complex 4 with unreacted 1 while the second assumes 5 as the direct precursor of 2. Although the first mechanism cannot be conclusively rejected, the second seems the most appropriate, since under high pressures of CO/H2 complex 2 was shown to equilibrate with 5. In the presence of an excess of other phosphines, the carbonylation of 1 yields quantitatively the mononuclear monocarbonyl derivatives Pt(PR3)3(CO) (R3 = Ph3, Et3, t-Bu2H).

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“…By contrast, magnitudes in trinuclear clusters, where the geometry is essentially similar but there is a metal-metal bond, are much larger: 'J(P-P), 20-160 Hz; 'J(Pt-P), 120-5 19 Hz (17,23,31,32). Clearly the values for the present complex, "J(P-P) < 5 Hz, "(Pt-P) = -25 Hz, fall into the non metal-metal bonded ranges.…”

Section: Discussionmentioning

confidence: 95%

Crystal and molecular structure and ³¹P and ¹⁹⁵Pt nmr spectroscopy of [Pt₃S₂(PMe₂Ph)₆][BEt₄]₂; a trinuclear complex containing triply-bridging sulphide ligands

Bushnell¹,

Dixon²,

Ono³

et al. 1984

Can. J. Chem.

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An X-ray diffraction study of [Pt3S2(PMe2Ph)6][BEt4]2 shows that it crystallises in the monoclinic space group, C2/c, with a = 15.447(2), b = 18.033(3), c = 26.505(5) Å, β = 96.73(2)°. The cation consists of three, distorted, square-planar cis-PtS2(PMe2Ph)2 moieties combined by sharing of the two sulphur atoms to produce a central Pt3S2 unit with C2 symmetry and Pt—Pt distances of 3.182(1) Å (one edge) and 3.108(1) Å (two edges). Complete analysis and computer simulation of 31P{1H} and 195Pt{1H} nuclear magnetic resonance spectra give values for 1J(Pt—P), 3202 Hz; 3J(Pt—P), −25 Hz; and 2J(Pt—Pt), 476 Hz. The structure is compared with previous results for analogous Ni and Pd complexes and the structural and nmr parameters are discussed with reference to the possibility of metal–metal interactions.

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31P and 195Pt nmr studies on the triangular cluster complexes [Pt3(μ-CO)3(tertiary phosphine)4]

Cited by 38 publications

References 11 publications

Some Mixed Transition Metal Compounds of 1,3-Diyne with Metallacycles Derived by Cross-Coupling of Alkynyl Ligands and Sequential C−C Bond Coupling between 1,3-Diyne and Carbon Monoxide

Some Mixed Transition Metal Compounds of 1,3-Diyne with Metallacycles Derived by Cross-Coupling of Alkynyl Ligands and Sequential C−C Bond Coupling between 1,3-Diyne and Carbon Monoxide

CO-Induced Reductive Elimination of P(t-Bu)₂H from the Platinum(II) Dinuclear Derivative Pt₂[μ-P(t-Bu)₂]₂(H)₂[P(t-Bu)₂H]₂, Affording Mononuclear Platinum(0) or Triangulo Triplatinum(I,I,II) Derivatives

Crystal and molecular structure and ³¹P and ¹⁹⁵Pt nmr spectroscopy of [Pt₃S₂(PMe₂Ph)₆][BEt₄]₂; a trinuclear complex containing triply-bridging sulphide ligands

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31P and 195Pt nmr studies on the triangular cluster complexes [Pt3(μ-CO)3(tertiary phosphine)4]

Cited by 38 publications

References 11 publications

Some Mixed Transition Metal Compounds of 1,3-Diyne with Metallacycles Derived by Cross-Coupling of Alkynyl Ligands and Sequential C−C Bond Coupling between 1,3-Diyne and Carbon Monoxide

Some Mixed Transition Metal Compounds of 1,3-Diyne with Metallacycles Derived by Cross-Coupling of Alkynyl Ligands and Sequential C−C Bond Coupling between 1,3-Diyne and Carbon Monoxide

CO-Induced Reductive Elimination of P(t-Bu)2H from the Platinum(II) Dinuclear Derivative Pt2[μ-P(t-Bu)2]2(H)2[P(t-Bu)2H]2, Affording Mononuclear Platinum(0) or Triangulo Triplatinum(I,I,II) Derivatives

Crystal and molecular structure and 31P and 195Pt nmr spectroscopy of [Pt3S2(PMe2Ph)6][BEt4]2; a trinuclear complex containing triply-bridging sulphide ligands

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CO-Induced Reductive Elimination of P(t-Bu)₂H from the Platinum(II) Dinuclear Derivative Pt₂[μ-P(t-Bu)₂]₂(H)₂[P(t-Bu)₂H]₂, Affording Mononuclear Platinum(0) or Triangulo Triplatinum(I,I,II) Derivatives

Crystal and molecular structure and ³¹P and ¹⁹⁵Pt nmr spectroscopy of [Pt₃S₂(PMe₂Ph)₆][BEt₄]₂; a trinuclear complex containing triply-bridging sulphide ligands