Synthesis of cationic palladium(II) and platinum(II) complexes with a monodentate trialkylphosphoniumdithiocarboxylate ligand: molecular structure of trans-[Pd(C6F5)(PEt3)2(S2C–PEt3)]ClO4·CHCl3

Rafael Usón; Juan Forniés; Rafael Navarro; Miguel A. Usón; Maria P. Garcia; Alan J. Welch

doi:10.1039/DT9840000345

Synthesis of cationic palladium(II) and platinum(II) complexes with a monodentate trialkylphosphoniumdithiocarboxylate ligand: molecular structure of trans-[Pd(C₆F₅)(PEt₃)₂(S₂C–PEt₃)]ClO₄·CHCl₃

Rafael Usón^*, Juan Forniés, Rafael Navarro, Miguel A. Usón, Maria P. Garcia, Alan J. Welch

^*Corresponding author for this work

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Abstract

Reaction of trans-[M(OClO₃)(C₆F₅)(PR₃) ₂] with the zwitterion S₂C-PR′₃ affords the complexes trans-[M(C₆F₅)(PR₃)₂(S ₂C-PR′₃)]ClO₄ (M = Pd; R₃ = R′₃ = Et₃, Bu₃, or Et₂Ph; R = Bu, R′ = cyclo-C₆H₁₁; R = Ph, R′ = Et or cyclo-C₆H₁₁ M = Pt, R = R′ = Et or Bu). trans-[Pd(C₆F₅)(PEt₃)₂(S ₂C-PEt₃)]ClO₄ is also given by reaction of [Pd(C₆F₅)(PEt₃)₃]ClO₄ with CS₂. Reaction of [M(OClO₃)(C₆F₅)(bipy)] (bipy = 2,2′-bipyridyl) with S₂C-PR′₃ affords [M(C₆F₅)(bipy)(S₂C-PR′ ₃)]ClO₄ (M = Pd or Pt; R′ = Et, Bu, or cyclo-C₆A₁₁). A crystallographic study of trans-[Pd(C₆F₅)(PEt₃)₂(S ₂C-PEt₃)]ClO₄ (as its 1:1 chloroform solvate) shows that the cation contains a unidentate triethylphosphoniumdithiocarboxylate ligand, and ³¹P n.m.r. spectra of all products with two terminal phosphine ligands are consistent with trans stereochemistries. Crystals of trans-[Pd(C₆F₅)(PEt₃)₂(S ₂C-PEt₃)]ClO₄·CHCl₃ are monoclinic, space group P2₁/a, with a = 14.596 5(18), b = 15.356(3), c = 19.324 2(16) Å, β = 109.257(8)°, and Z = 4. Using 4 093 amplitudes the structure has been refined to R = 0.1049. The non-bonding Pd⋯S distance is 3.644(4) Å.

Original language	English
Pages (from-to)	345-350
Number of pages	6
Journal	Journal of the Chemical Society, Dalton Transactions
Issue number	3
DOIs	https://doi.org/10.1039/DT9840000345
Publication status	Published - 1984

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General Chemistry

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Usón, R., Forniés, J., Navarro, R., Usón, M. A., Garcia, M. P., & Welch, A. J. (1984). Synthesis of cationic palladium(II) and platinum(II) complexes with a monodentate trialkylphosphoniumdithiocarboxylate ligand: molecular structure of trans-[Pd(C₆F₅)(PEt₃)₂(S₂C–PEt₃)]ClO₄·CHCl₃. Journal of the Chemical Society, Dalton Transactions, (3), 345-350. https://doi.org/10.1039/DT9840000345

@article{afc1db8c0fc5467b9ceaac427de3d84a,

title = "Synthesis of cationic palladium(II) and platinum(II) complexes with a monodentate trialkylphosphoniumdithiocarboxylate ligand: molecular structure of trans-[Pd(C6F5)(PEt3)2(S2C–PEt3)]ClO4·CHCl3",

abstract = "Reaction of trans-[M(OClO3)(C6F5)(PR3) 2] with the zwitterion S2C-PR′3 affords the complexes trans-[M(C6F5)(PR3)2(S 2C-PR′3)]ClO4 (M = Pd; R3 = R′3 = Et3, Bu3, or Et2Ph; R = Bu, R′ = cyclo-C6H11; R = Ph, R′ = Et or cyclo-C6H11 M = Pt, R = R′ = Et or Bu). trans-[Pd(C6F5)(PEt3)2(S 2C-PEt3)]ClO4 is also given by reaction of [Pd(C6F5)(PEt3)3]ClO4 with CS2. Reaction of [M(OClO3)(C6F5)(bipy)] (bipy = 2,2′-bipyridyl) with S2C-PR′3 affords [M(C6F5)(bipy)(S2C-PR′ 3)]ClO4 (M = Pd or Pt; R′ = Et, Bu, or cyclo-C6A11). A crystallographic study of trans-[Pd(C6F5)(PEt3)2(S 2C-PEt3)]ClO4 (as its 1:1 chloroform solvate) shows that the cation contains a unidentate triethylphosphoniumdithiocarboxylate ligand, and 31P n.m.r. spectra of all products with two terminal phosphine ligands are consistent with trans stereochemistries. Crystals of trans-[Pd(C6F5)(PEt3)2(S 2C-PEt3)]ClO4·CHCl3 are monoclinic, space group P21/a, with a = 14.596 5(18), b = 15.356(3), c = 19.324 2(16) {\AA}, β = 109.257(8)°, and Z = 4. Using 4 093 amplitudes the structure has been refined to R = 0.1049. The non-bonding Pd⋯S distance is 3.644(4) {\AA}.",

author = "Rafael Us{\'o}n and Juan Forni{\'e}s and Rafael Navarro and Us{\'o}n, {Miguel A.} and Garcia, {Maria P.} and Welch, {Alan J.}",

year = "1984",

doi = "10.1039/DT9840000345",

language = "English",

pages = "345--350",

journal = "Journal of the Chemical Society, Dalton Transactions",

issn = "0300-9246",

number = "3",

}

Usón, R, Forniés, J, Navarro, R, Usón, MA, Garcia, MP & Welch, AJ 1984, 'Synthesis of cationic palladium(II) and platinum(II) complexes with a monodentate trialkylphosphoniumdithiocarboxylate ligand: molecular structure of trans-[Pd(C₆F₅)(PEt₃)₂(S₂C–PEt₃)]ClO₄·CHCl₃', Journal of the Chemical Society, Dalton Transactions, no. 3, pp. 345-350. https://doi.org/10.1039/DT9840000345

Synthesis of cationic palladium(II) and platinum(II) complexes with a monodentate trialkylphosphoniumdithiocarboxylate ligand: molecular structure of trans-[Pd(C₆F₅)(PEt₃)₂(S₂C–PEt₃)]ClO₄·CHCl₃. / Usón, Rafael; Forniés, Juan; Navarro, Rafael et al.
In: Journal of the Chemical Society, Dalton Transactions, No. 3, 1984, p. 345-350.

Research output: Contribution to journal › Article › peer-review

TY - JOUR

T1 - Synthesis of cationic palladium(II) and platinum(II) complexes with a monodentate trialkylphosphoniumdithiocarboxylate ligand: molecular structure of trans-[Pd(C6F5)(PEt3)2(S2C–PEt3)]ClO4·CHCl3

AU - Usón, Rafael

AU - Forniés, Juan

AU - Navarro, Rafael

AU - Usón, Miguel A.

AU - Garcia, Maria P.

AU - Welch, Alan J.

PY - 1984

Y1 - 1984

N2 - Reaction of trans-[M(OClO3)(C6F5)(PR3) 2] with the zwitterion S2C-PR′3 affords the complexes trans-[M(C6F5)(PR3)2(S 2C-PR′3)]ClO4 (M = Pd; R3 = R′3 = Et3, Bu3, or Et2Ph; R = Bu, R′ = cyclo-C6H11; R = Ph, R′ = Et or cyclo-C6H11 M = Pt, R = R′ = Et or Bu). trans-[Pd(C6F5)(PEt3)2(S 2C-PEt3)]ClO4 is also given by reaction of [Pd(C6F5)(PEt3)3]ClO4 with CS2. Reaction of [M(OClO3)(C6F5)(bipy)] (bipy = 2,2′-bipyridyl) with S2C-PR′3 affords [M(C6F5)(bipy)(S2C-PR′ 3)]ClO4 (M = Pd or Pt; R′ = Et, Bu, or cyclo-C6A11). A crystallographic study of trans-[Pd(C6F5)(PEt3)2(S 2C-PEt3)]ClO4 (as its 1:1 chloroform solvate) shows that the cation contains a unidentate triethylphosphoniumdithiocarboxylate ligand, and 31P n.m.r. spectra of all products with two terminal phosphine ligands are consistent with trans stereochemistries. Crystals of trans-[Pd(C6F5)(PEt3)2(S 2C-PEt3)]ClO4·CHCl3 are monoclinic, space group P21/a, with a = 14.596 5(18), b = 15.356(3), c = 19.324 2(16) Å, β = 109.257(8)°, and Z = 4. Using 4 093 amplitudes the structure has been refined to R = 0.1049. The non-bonding Pd⋯S distance is 3.644(4) Å.

AB - Reaction of trans-[M(OClO3)(C6F5)(PR3) 2] with the zwitterion S2C-PR′3 affords the complexes trans-[M(C6F5)(PR3)2(S 2C-PR′3)]ClO4 (M = Pd; R3 = R′3 = Et3, Bu3, or Et2Ph; R = Bu, R′ = cyclo-C6H11; R = Ph, R′ = Et or cyclo-C6H11 M = Pt, R = R′ = Et or Bu). trans-[Pd(C6F5)(PEt3)2(S 2C-PEt3)]ClO4 is also given by reaction of [Pd(C6F5)(PEt3)3]ClO4 with CS2. Reaction of [M(OClO3)(C6F5)(bipy)] (bipy = 2,2′-bipyridyl) with S2C-PR′3 affords [M(C6F5)(bipy)(S2C-PR′ 3)]ClO4 (M = Pd or Pt; R′ = Et, Bu, or cyclo-C6A11). A crystallographic study of trans-[Pd(C6F5)(PEt3)2(S 2C-PEt3)]ClO4 (as its 1:1 chloroform solvate) shows that the cation contains a unidentate triethylphosphoniumdithiocarboxylate ligand, and 31P n.m.r. spectra of all products with two terminal phosphine ligands are consistent with trans stereochemistries. Crystals of trans-[Pd(C6F5)(PEt3)2(S 2C-PEt3)]ClO4·CHCl3 are monoclinic, space group P21/a, with a = 14.596 5(18), b = 15.356(3), c = 19.324 2(16) Å, β = 109.257(8)°, and Z = 4. Using 4 093 amplitudes the structure has been refined to R = 0.1049. The non-bonding Pd⋯S distance is 3.644(4) Å.

UR - http://www.scopus.com/inward/record.url?scp=37049110544&partnerID=8YFLogxK

U2 - 10.1039/DT9840000345

DO - 10.1039/DT9840000345

M3 - Article

AN - SCOPUS:37049110544

SN - 0300-9246

SP - 345

EP - 350

JO - Journal of the Chemical Society, Dalton Transactions

JF - Journal of the Chemical Society, Dalton Transactions

IS - 3

ER -

Synthesis of cationic palladium(II) and platinum(II) complexes with a monodentate trialkylphosphoniumdithiocarboxylate ligand: molecular structure of trans-[Pd(C₆F₅)(PEt₃)₂(S₂C–PEt₃)]ClO₄·CHCl₃

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