Synthesis and solution multinuclear nuclear magnetic resonance studies of homoleptic copper(I) complexes of group 15 donor ligands

Jane R. Black; William Levason; Mark D. Spicer; Michael Webster

doi:10.1039/DT9930003129

Synthesis and solution multinuclear nuclear magnetic resonance studies of homoleptic copper(I) complexes of group 15 donor ligands

Jane R. Black^*, William Levason, Mark D. Spicer, Michael Webster

^*Corresponding author for this work

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

66 Citations (Scopus)

Abstract

The homoleptic complexes [CuL₄]Y (L = PMe₃, PMe₂Ph, PMePh₂, PPh₃, PPh₂H, PPhH₂, AsMe₃, AsMe₂Ph, AsMePh₂, AsPh₃, SbMe₃, SbEt₃ or SbPh₃; Y = PF₆ or BF₄) and [Cu(L-L)₂]Y [L-L = Me₂P(CH₂)₂PMe₂, o-C₆H₄(PMe₂)₂, Ph₂P(CH₂)_nPPh₂ (n = 1-4), cis-Ph₂PCH=CHPPh₂, o-C₆H₄(PPh₂)₂, o-C₆H₄(AsMe₂)₂, cis-Ph₂AsCH=CHAsPh₂, o-C₆H₄(SbMe₂)₂, Me₂Sb(CH₂)₃SbMe₂ or Ph₂Sb(CH₂)₃SbPh₂] have been prepared from [Cu(MeCN)₄]Y and L or L-L. The ⁶³Cu and, where appropriate, ³¹P-{¹H} NMR spectra, have been recorded from CH₂Cl₂ solutions of the complexes over the temperature range 300-175 K, including the first reported ⁶³Cu resonances from arsenic and antimony donor ligand compounds. The effects of ligand size and geometry upon the ⁶³Cu NMR spectra are discussed and typical copper chemical-shift ranges for Group 15 donor ligand compounds established. The structure of [Cu(cis-Ph₂AsCH=CHAsPh₂)₂]PF₆ has been established by X-ray crystallography: orthorhombic, space group P2₁2₁2₁, a = 14.775(6), b = 16.991(5), c = 21.027(6) Å, Z = 4. The copper atom is in a distorted tetrahedral environment [Cu-As 2.348(3)-2.358(3) Å].

Original language	English
Pages (from-to)	3129-3136
Number of pages	8
Journal	Journal of the Chemical Society, Dalton Transactions
Issue number	20
DOIs	https://doi.org/10.1039/DT9930003129
Publication status	Published - 1993
Externally published	Yes

ASJC Scopus subject areas

General Chemistry

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10.1039/DT9930003129

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@article{3953b4e5f7374b00b923855aafa4b0de,

title = "Synthesis and solution multinuclear nuclear magnetic resonance studies of homoleptic copper(I) complexes of group 15 donor ligands",

abstract = "The homoleptic complexes [CuL4]Y (L = PMe3, PMe2Ph, PMePh2, PPh3, PPh2H, PPhH2, AsMe3, AsMe2Ph, AsMePh2, AsPh3, SbMe3, SbEt3 or SbPh3; Y = PF6 or BF4) and [Cu(L-L)2]Y [L-L = Me2P(CH2)2PMe2, o-C6H4(PMe2)2, Ph2P(CH2)nPPh2 (n = 1-4), cis-Ph2PCH=CHPPh2, o-C6H4(PPh2)2, o-C6H4(AsMe2)2, cis-Ph2AsCH=CHAsPh2, o-C6H4(SbMe2)2, Me2Sb(CH2)3SbMe2 or Ph2Sb(CH2)3SbPh2] have been prepared from [Cu(MeCN)4]Y and L or L-L. The 63Cu and, where appropriate, 31P-{1H} NMR spectra, have been recorded from CH2Cl2 solutions of the complexes over the temperature range 300-175 K, including the first reported 63Cu resonances from arsenic and antimony donor ligand compounds. The effects of ligand size and geometry upon the 63Cu NMR spectra are discussed and typical copper chemical-shift ranges for Group 15 donor ligand compounds established. The structure of [Cu(cis-Ph2AsCH=CHAsPh2)2]PF6 has been established by X-ray crystallography: orthorhombic, space group P212121, a = 14.775(6), b = 16.991(5), c = 21.027(6) {\AA}, Z = 4. The copper atom is in a distorted tetrahedral environment [Cu-As 2.348(3)-2.358(3) {\AA}].",

author = "Black, {Jane R.} and William Levason and Spicer, {Mark D.} and Michael Webster",

year = "1993",

doi = "10.1039/DT9930003129",

language = "English",

pages = "3129--3136",

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

issn = "1472-7773",

publisher = "Royal Society of Chemistry",

number = "20",

}

TY - JOUR

T1 - Synthesis and solution multinuclear nuclear magnetic resonance studies of homoleptic copper(I) complexes of group 15 donor ligands

AU - Black, Jane R.

AU - Levason, William

AU - Spicer, Mark D.

AU - Webster, Michael

PY - 1993

Y1 - 1993

N2 - The homoleptic complexes [CuL4]Y (L = PMe3, PMe2Ph, PMePh2, PPh3, PPh2H, PPhH2, AsMe3, AsMe2Ph, AsMePh2, AsPh3, SbMe3, SbEt3 or SbPh3; Y = PF6 or BF4) and [Cu(L-L)2]Y [L-L = Me2P(CH2)2PMe2, o-C6H4(PMe2)2, Ph2P(CH2)nPPh2 (n = 1-4), cis-Ph2PCH=CHPPh2, o-C6H4(PPh2)2, o-C6H4(AsMe2)2, cis-Ph2AsCH=CHAsPh2, o-C6H4(SbMe2)2, Me2Sb(CH2)3SbMe2 or Ph2Sb(CH2)3SbPh2] have been prepared from [Cu(MeCN)4]Y and L or L-L. The 63Cu and, where appropriate, 31P-{1H} NMR spectra, have been recorded from CH2Cl2 solutions of the complexes over the temperature range 300-175 K, including the first reported 63Cu resonances from arsenic and antimony donor ligand compounds. The effects of ligand size and geometry upon the 63Cu NMR spectra are discussed and typical copper chemical-shift ranges for Group 15 donor ligand compounds established. The structure of [Cu(cis-Ph2AsCH=CHAsPh2)2]PF6 has been established by X-ray crystallography: orthorhombic, space group P212121, a = 14.775(6), b = 16.991(5), c = 21.027(6) Å, Z = 4. The copper atom is in a distorted tetrahedral environment [Cu-As 2.348(3)-2.358(3) Å].

AB - The homoleptic complexes [CuL4]Y (L = PMe3, PMe2Ph, PMePh2, PPh3, PPh2H, PPhH2, AsMe3, AsMe2Ph, AsMePh2, AsPh3, SbMe3, SbEt3 or SbPh3; Y = PF6 or BF4) and [Cu(L-L)2]Y [L-L = Me2P(CH2)2PMe2, o-C6H4(PMe2)2, Ph2P(CH2)nPPh2 (n = 1-4), cis-Ph2PCH=CHPPh2, o-C6H4(PPh2)2, o-C6H4(AsMe2)2, cis-Ph2AsCH=CHAsPh2, o-C6H4(SbMe2)2, Me2Sb(CH2)3SbMe2 or Ph2Sb(CH2)3SbPh2] have been prepared from [Cu(MeCN)4]Y and L or L-L. The 63Cu and, where appropriate, 31P-{1H} NMR spectra, have been recorded from CH2Cl2 solutions of the complexes over the temperature range 300-175 K, including the first reported 63Cu resonances from arsenic and antimony donor ligand compounds. The effects of ligand size and geometry upon the 63Cu NMR spectra are discussed and typical copper chemical-shift ranges for Group 15 donor ligand compounds established. The structure of [Cu(cis-Ph2AsCH=CHAsPh2)2]PF6 has been established by X-ray crystallography: orthorhombic, space group P212121, a = 14.775(6), b = 16.991(5), c = 21.027(6) Å, Z = 4. The copper atom is in a distorted tetrahedral environment [Cu-As 2.348(3)-2.358(3) Å].

U2 - 10.1039/DT9930003129

DO - 10.1039/DT9930003129

M3 - Article

AN - SCOPUS:37049085937

SN - 1472-7773

SP - 3129

EP - 3136

JO - Journal of the Chemical Society, Dalton Transactions

JF - Journal of the Chemical Society, Dalton Transactions

IS - 20

ER -

Synthesis and solution multinuclear nuclear magnetic resonance studies of homoleptic copper(I) complexes of group 15 donor ligands

Abstract

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