Synthesis and characterization of palladium and nickel complexes with positively charged triphosphine ligands and their use as electrochemical CO2-reduction catalysts

Alex Miedaner; Bruce C. Noll; Daniel L DuBois

Synthesis and characterization of palladium and nickel complexes with positively charged triphosphine ligands and their use as electrochemical CO2-reduction catalysts

Alex Miedaner, Bruce C. Noll, Daniel L DuBois

Pacific Northwest National Laboratory

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Abstract

The synthesis and characterization of [M(Bu₃P⁺etpE)Br](BF₄)₂ (where M = Ni or Pd and Bu₃P⁺etpE = [(Bu₃PCH₂CH₂)P(CH₂CH ₂PEt₂)₂]⁺) and [M(etpPBu₃ ⁺)Br]Br(BF₄)₄ (where M = Ni or Pd and etpPBu₃ ⁺ = {PhP[CH₂CH₂P(CH₂CH₂PBu ₃)₂]₂}⁴⁺) are described. The structure of [Ni(etpPBu₃ ⁺)Br]Br(BF₄)₄ has been determined by X-ray diffraction. Treatment of [Pd-(Bu₃P⁺etpE)Br](BF₄)₂ with AgBF₄ in acetonitrile produced [Pd(Bu₃P⁺etpE)(CH₃CN)](BF₄) ₃. The latter compound has also been characterized by single-crystal X-ray diffraction methods. Electrochemical studies indicate that this compound and its closely related methyl analog, [Pd(Me₃P⁺etpE)(CH₃CN)](BF₄) ₃, are catalysts for the electrochemical reduction of CO₂ to CO in acidic dimethylformamide solutions. Kinetic and mechanistic studies of this catalytic reaction are reported.

Original language	English
Pages (from-to)	5779-5791
Number of pages	13
Journal	Organometallics
Volume	16
Issue number	26
Publication status	Published - Dec 23 1997

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ASJC Scopus subject areas

Inorganic Chemistry
Organic Chemistry

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Miedaner, A., Noll, B. C., & DuBois, D. L. (1997). Synthesis and characterization of palladium and nickel complexes with positively charged triphosphine ligands and their use as electrochemical CO2-reduction catalysts. Organometallics, 16(26), 5779-5791.

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title = "Synthesis and characterization of palladium and nickel complexes with positively charged triphosphine ligands and their use as electrochemical CO2-reduction catalysts",

abstract = "The synthesis and characterization of [M(Bu3P+etpE)Br](BF4)2 (where M = Ni or Pd and Bu3P+etpE = [(Bu3PCH2CH2)P(CH2CH 2PEt2)2]+) and [M(etpPBu3 +)Br]Br(BF4)4 (where M = Ni or Pd and etpPBu3 + = {PhP[CH2CH2P(CH2CH2PBu 3)2]2}4+) are described. The structure of [Ni(etpPBu3 +)Br]Br(BF4)4 has been determined by X-ray diffraction. Treatment of [Pd-(Bu3P+etpE)Br](BF4)2 with AgBF4 in acetonitrile produced [Pd(Bu3P+etpE)(CH3CN)](BF4) 3. The latter compound has also been characterized by single-crystal X-ray diffraction methods. Electrochemical studies indicate that this compound and its closely related methyl analog, [Pd(Me3P+etpE)(CH3CN)](BF4) 3, are catalysts for the electrochemical reduction of CO2 to CO in acidic dimethylformamide solutions. Kinetic and mechanistic studies of this catalytic reaction are reported.",

author = "Alex Miedaner and Noll, {Bruce C.} and DuBois, {Daniel L}",

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T1 - Synthesis and characterization of palladium and nickel complexes with positively charged triphosphine ligands and their use as electrochemical CO2-reduction catalysts

AU - Miedaner, Alex

AU - Noll, Bruce C.

AU - DuBois, Daniel L

PY - 1997/12/23

Y1 - 1997/12/23

N2 - The synthesis and characterization of [M(Bu3P+etpE)Br](BF4)2 (where M = Ni or Pd and Bu3P+etpE = [(Bu3PCH2CH2)P(CH2CH 2PEt2)2]+) and [M(etpPBu3 +)Br]Br(BF4)4 (where M = Ni or Pd and etpPBu3 + = {PhP[CH2CH2P(CH2CH2PBu 3)2]2}4+) are described. The structure of [Ni(etpPBu3 +)Br]Br(BF4)4 has been determined by X-ray diffraction. Treatment of [Pd-(Bu3P+etpE)Br](BF4)2 with AgBF4 in acetonitrile produced [Pd(Bu3P+etpE)(CH3CN)](BF4) 3. The latter compound has also been characterized by single-crystal X-ray diffraction methods. Electrochemical studies indicate that this compound and its closely related methyl analog, [Pd(Me3P+etpE)(CH3CN)](BF4) 3, are catalysts for the electrochemical reduction of CO2 to CO in acidic dimethylformamide solutions. Kinetic and mechanistic studies of this catalytic reaction are reported.

AB - The synthesis and characterization of [M(Bu3P+etpE)Br](BF4)2 (where M = Ni or Pd and Bu3P+etpE = [(Bu3PCH2CH2)P(CH2CH 2PEt2)2]+) and [M(etpPBu3 +)Br]Br(BF4)4 (where M = Ni or Pd and etpPBu3 + = {PhP[CH2CH2P(CH2CH2PBu 3)2]2}4+) are described. The structure of [Ni(etpPBu3 +)Br]Br(BF4)4 has been determined by X-ray diffraction. Treatment of [Pd-(Bu3P+etpE)Br](BF4)2 with AgBF4 in acetonitrile produced [Pd(Bu3P+etpE)(CH3CN)](BF4) 3. The latter compound has also been characterized by single-crystal X-ray diffraction methods. Electrochemical studies indicate that this compound and its closely related methyl analog, [Pd(Me3P+etpE)(CH3CN)](BF4) 3, are catalysts for the electrochemical reduction of CO2 to CO in acidic dimethylformamide solutions. Kinetic and mechanistic studies of this catalytic reaction are reported.

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Synthesis and characterization of palladium and nickel complexes with positively charged triphosphine ligands and their use as electrochemical CO2-reduction catalysts

Abstract

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