Synthesis and characterization of water-soluble [Pd(triphosphine)(CH3CN)](BF4)2 complexes for CO2 reduction

Andrew M. Herring, Bryan D. Steffey, Alex Miedaner, Sheryl A. Wander, Daniel L DuBois

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Abstract

The syntheses of the triphosphine ligands RP(CH2CH2PR′2)2 (R = CH2CH2CH2OH and R′ = Et, HOPetpE; R = Ph and R′ = CH2CH2P(O)(OEt)2, etpEPO; R = Me2N and R′ = Et, MNetpE; R = i-Pr2N and R′ = Et, IPNetpE; R = Ph and R′ = NMe2, etpMN) are described. The reaction of [Pd(CH3CN)4](BF4)2 with these ligands forms [Pd(triphosphine)(CH3CN)](BF4)2 complexes that are all water soluble with the exception of [Pd(IPNeIpE)(CH3-CN)](BF4)2. The labile acetonitrile ligands are easily substituted by triethylphosphine to form [Pd(triphosphine)-(PEt3)](BF4)2 complexes. The triethylphosphine complexes undergo quasi-reversible two-electron reductions while the corresponding acetonitrile complexes undergo two, closely spaced, irreversible, one-electron reductions. [Pd-(HOPetpE)(CH3CN)](BF4)2 and [Pd(etpEPO)(CH3CN)](BF4)2 are catalysts for the electrochemical reduction of CO2 to CO in both dimethylformamide and buffered aqueous solutions. Kinetic studies are reported for [Pd-(HOPetpE)(CH3CN)](BF4)2 in dimethylformamide.

Original languageEnglish
Pages (from-to)1100-1109
Number of pages10
JournalInorganic Chemistry
Volume34
Issue number5
Publication statusPublished - 1995

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Dimethylformamide
Ligands
ligands
acetonitrile
Water
synthesis
water
Electrons
Carbon Monoxide
electrons
aqueous solutions
catalysts
Catalysts
Kinetics
kinetics

ASJC Scopus subject areas

  • Inorganic Chemistry

Cite this

Synthesis and characterization of water-soluble [Pd(triphosphine)(CH3CN)](BF4)2 complexes for CO2 reduction. / Herring, Andrew M.; Steffey, Bryan D.; Miedaner, Alex; Wander, Sheryl A.; DuBois, Daniel L.

In: Inorganic Chemistry, Vol. 34, No. 5, 1995, p. 1100-1109.

Research output: Contribution to journalArticle

Herring, Andrew M. ; Steffey, Bryan D. ; Miedaner, Alex ; Wander, Sheryl A. ; DuBois, Daniel L. / Synthesis and characterization of water-soluble [Pd(triphosphine)(CH3CN)](BF4)2 complexes for CO2 reduction. In: Inorganic Chemistry. 1995 ; Vol. 34, No. 5. pp. 1100-1109.
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N2 - The syntheses of the triphosphine ligands RP(CH2CH2PR′2)2 (R = CH2CH2CH2OH and R′ = Et, HOPetpE; R = Ph and R′ = CH2CH2P(O)(OEt)2, etpEPO; R = Me2N and R′ = Et, MNetpE; R = i-Pr2N and R′ = Et, IPNetpE; R = Ph and R′ = NMe2, etpMN) are described. The reaction of [Pd(CH3CN)4](BF4)2 with these ligands forms [Pd(triphosphine)(CH3CN)](BF4)2 complexes that are all water soluble with the exception of [Pd(IPNeIpE)(CH3-CN)](BF4)2. The labile acetonitrile ligands are easily substituted by triethylphosphine to form [Pd(triphosphine)-(PEt3)](BF4)2 complexes. The triethylphosphine complexes undergo quasi-reversible two-electron reductions while the corresponding acetonitrile complexes undergo two, closely spaced, irreversible, one-electron reductions. [Pd-(HOPetpE)(CH3CN)](BF4)2 and [Pd(etpEPO)(CH3CN)](BF4)2 are catalysts for the electrochemical reduction of CO2 to CO in both dimethylformamide and buffered aqueous solutions. Kinetic studies are reported for [Pd-(HOPetpE)(CH3CN)](BF4)2 in dimethylformamide.

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