Generation of metal formyl complexes using nickel and platinum hydrides as reducing agents

Alex Miedaner; Daniel L DuBois; Calvin J. Curtis; R. Curtis Haltiwanger

Generation of metal formyl complexes using nickel and platinum hydrides as reducing agents

Alex Miedaner, Daniel L DuBois, Calvin J. Curtis, R. Curtis Haltiwanger

Pacific Northwest National Laboratory

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

56 Citations (Scopus)

Abstract

The five-coordinate nickel hydride complex [Ni(dmpe)₂H]PF₆ (1) [dmpe = 1,2-bis-(dimethylphosphino)ethane] was synthesized by protonation of Ni(dmpe)₂ with NH₄PF₆. The platinum analog, [Pt(dmpe)₂H]PF₆ (2), and [Pt(depe)₂H]PF₆ (3) [depe = 1,2-bis(diethylphospnino)ethane] were synthesized by reduction of the corresponding Pt(II) complexes with NaBH₄ on alumina. Complexes 1 and 3 can also be synthesized electrochemically. Reduction of Ni-(dmpe)₂ ²⁺ by two electrons in the presence of ammonium ion generates 1, and reduction of Pt(depe)₂ ²⁺ in methanol or wet acetonitrile produces 3. These hydrides react with a variety of cationic metal carbonyl complexes to produce known metal formyl complexes. The structure of 3 was determined by X-ray diffraction. Complex 3 crystallizes in a monoclinic unit cell with P2₁/c symmetry with a = 14.258 (4) Å, b = 9.648 (3) Å, c= 21.898 (5) Å, β = 91.17 (2)°, V = 3011.7 (14) Å³, Z = 4, and d_calcd = 1.662 g/cm³. Full-matrix least-squares refinement converged with residuals R = 4.52% and R_w = 5.90%.

Original language	English
Pages (from-to)	299-303
Number of pages	5
Journal	Organometallics
Volume	12
Issue number	2
Publication status	Published - 1993

ASJC Scopus subject areas

Inorganic Chemistry
Organic Chemistry

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@article{10f5681dcbc34967af1ddf28da6bf144,

title = "Generation of metal formyl complexes using nickel and platinum hydrides as reducing agents",

abstract = "The five-coordinate nickel hydride complex [Ni(dmpe)2H]PF6 (1) [dmpe = 1,2-bis-(dimethylphosphino)ethane] was synthesized by protonation of Ni(dmpe)2 with NH4PF6. The platinum analog, [Pt(dmpe)2H]PF6 (2), and [Pt(depe)2H]PF6 (3) [depe = 1,2-bis(diethylphospnino)ethane] were synthesized by reduction of the corresponding Pt(II) complexes with NaBH4 on alumina. Complexes 1 and 3 can also be synthesized electrochemically. Reduction of Ni-(dmpe)2 2+ by two electrons in the presence of ammonium ion generates 1, and reduction of Pt(depe)2 2+ in methanol or wet acetonitrile produces 3. These hydrides react with a variety of cationic metal carbonyl complexes to produce known metal formyl complexes. The structure of 3 was determined by X-ray diffraction. Complex 3 crystallizes in a monoclinic unit cell with P21/c symmetry with a = 14.258 (4) {\AA}, b = 9.648 (3) {\AA}, c= 21.898 (5) {\AA}, β = 91.17 (2)°, V = 3011.7 (14) {\AA}3, Z = 4, and dcalcd = 1.662 g/cm3. Full-matrix least-squares refinement converged with residuals R = 4.52% and Rw = 5.90%.",

author = "Alex Miedaner and DuBois, {Daniel L} and Curtis, {Calvin J.} and Haltiwanger, {R. Curtis}",

year = "1993",

language = "English",

volume = "12",

pages = "299--303",

journal = "Organometallics",

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publisher = "American Chemical Society",

number = "2",

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T1 - Generation of metal formyl complexes using nickel and platinum hydrides as reducing agents

AU - Miedaner, Alex

AU - DuBois, Daniel L

AU - Curtis, Calvin J.

AU - Haltiwanger, R. Curtis

PY - 1993

Y1 - 1993

N2 - The five-coordinate nickel hydride complex [Ni(dmpe)2H]PF6 (1) [dmpe = 1,2-bis-(dimethylphosphino)ethane] was synthesized by protonation of Ni(dmpe)2 with NH4PF6. The platinum analog, [Pt(dmpe)2H]PF6 (2), and [Pt(depe)2H]PF6 (3) [depe = 1,2-bis(diethylphospnino)ethane] were synthesized by reduction of the corresponding Pt(II) complexes with NaBH4 on alumina. Complexes 1 and 3 can also be synthesized electrochemically. Reduction of Ni-(dmpe)2 2+ by two electrons in the presence of ammonium ion generates 1, and reduction of Pt(depe)2 2+ in methanol or wet acetonitrile produces 3. These hydrides react with a variety of cationic metal carbonyl complexes to produce known metal formyl complexes. The structure of 3 was determined by X-ray diffraction. Complex 3 crystallizes in a monoclinic unit cell with P21/c symmetry with a = 14.258 (4) Å, b = 9.648 (3) Å, c= 21.898 (5) Å, β = 91.17 (2)°, V = 3011.7 (14) Å3, Z = 4, and dcalcd = 1.662 g/cm3. Full-matrix least-squares refinement converged with residuals R = 4.52% and Rw = 5.90%.

AB - The five-coordinate nickel hydride complex [Ni(dmpe)2H]PF6 (1) [dmpe = 1,2-bis-(dimethylphosphino)ethane] was synthesized by protonation of Ni(dmpe)2 with NH4PF6. The platinum analog, [Pt(dmpe)2H]PF6 (2), and [Pt(depe)2H]PF6 (3) [depe = 1,2-bis(diethylphospnino)ethane] were synthesized by reduction of the corresponding Pt(II) complexes with NaBH4 on alumina. Complexes 1 and 3 can also be synthesized electrochemically. Reduction of Ni-(dmpe)2 2+ by two electrons in the presence of ammonium ion generates 1, and reduction of Pt(depe)2 2+ in methanol or wet acetonitrile produces 3. These hydrides react with a variety of cationic metal carbonyl complexes to produce known metal formyl complexes. The structure of 3 was determined by X-ray diffraction. Complex 3 crystallizes in a monoclinic unit cell with P21/c symmetry with a = 14.258 (4) Å, b = 9.648 (3) Å, c= 21.898 (5) Å, β = 91.17 (2)°, V = 3011.7 (14) Å3, Z = 4, and dcalcd = 1.662 g/cm3. Full-matrix least-squares refinement converged with residuals R = 4.52% and Rw = 5.90%.

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