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

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

Pacific Northwest National Laboratory

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

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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 language	English
Pages (from-to)	1100-1109
Number of pages	10
Journal	Inorganic Chemistry
Volume	34
Issue number	5
Publication status	Published - 1995

ASJC Scopus subject areas

Inorganic Chemistry

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@article{b5499394686a4df8bfb7a762f6bb1c0e,

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

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.",

author = "Herring, {Andrew M.} and Steffey, {Bryan D.} and Alex Miedaner and Wander, {Sheryl A.} and DuBois, {Daniel L}",

year = "1995",

language = "English",

volume = "34",

pages = "1100--1109",

journal = "Inorganic Chemistry",

issn = "0020-1669",

publisher = "American Chemical Society",

number = "5",

}

TY - JOUR

T1 - Synthesis and characterization of water-soluble [Pd(triphosphine)(CH3CN)](BF4)2 complexes for CO2 reduction

AU - Herring, Andrew M.

AU - Steffey, Bryan D.

AU - Miedaner, Alex

AU - Wander, Sheryl A.

AU - DuBois, Daniel L

PY - 1995

Y1 - 1995

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.

AB - 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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VL - 34

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JO - Inorganic Chemistry

JF - Inorganic Chemistry

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