Preparation and characterization of cobalt(III), Nickel(II), and Copper(I) Complexes Containing 5, 8-Diphenyl-5, 8-diphospha-2, 11-dithiadodecane (L), CH3SCH2CH2P(C6H5)CH2CH2P(C6H5)CH2CH2SCH3, and Molecular Structure of [Ni(rac(P)-L)2](BF4)2

Tetsuji Kitagawa, Masakazu Kita, Kazuo Kashiwabara, Junnosuke Fujita

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Abstract

Δ-RR,∧-SS-[Co(acac)2(rac(P)-L)]+ and [Co(acac)2(raeso(P)-L)]+ were obtained by reaction of [Co(acac)3] (acac=2, 4-pentanedionate ion) with 5, 8-diphenyl-5, 8-diphospha-2, 11-dithiadodecane (L) in 1:1 molar ratio in dichloromethane in the presence of active charcoal, no Δ-SS,∧-RR isomer of the rac(P)-L complex being formed. Five-coordinate [Ni(rac(P)-L)2]2+ and [Ni(raeso(P)-L)2]2+ were yielded by reaction of Ni(II) and L in 1:2 molar ratio in methanol, and the molecular structure of less soluble [Ni(rac(P)-L)2](BF4)2 was determined by X-ray analysis. Crystal data: monoclinic, space group P21/n, a=17.136(3), b=20.134(5), c=14.106(3) Å, β=93.30(2)°, V=4859(2) Å3, Z=4, R=0.089 for 8001 reflections. The Ni atom is surrounded square pyramidally by four P atoms in the basal plane and one S atom at the apical position with distances of the Ni-P: 2.214(2)-2.234(2) Å and the Ni-S: 2.603(2) Å. Both [Ni(rac(P)-L)2]2+ and [Ni(meso(P)-L)2]2+ in CH2Cl2 solutions exchange four -SCH3 groups at the apical positin on the NMR time scale. White [Cu(rac(P)-L)]BF4 was precipitated selectively by reaction of Cu(BF4)2 • 6H2O and L in 1:1 molar ratio in ethanol.

Original languageEnglish
Pages (from-to)2942-2947
Number of pages6
JournalBulletin of the Chemical Society of Japan
Volume64
Issue number10
Publication statusPublished - Oct 1 1991
Externally publishedYes

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Cobalt
Nickel
Molecular structure
Copper
Atoms
Charcoal
Methylene Chloride
X ray analysis
Isomers
Methanol
Ion exchange
Ethanol
Nuclear magnetic resonance
Ions
Crystals
diphenyl

ASJC Scopus subject areas

  • Chemistry(all)

Cite this

@article{f534a7dfdb5643e4add4bd6489726ac3,
title = "Preparation and characterization of cobalt(III), Nickel(II), and Copper(I) Complexes Containing 5, 8-Diphenyl-5, 8-diphospha-2, 11-dithiadodecane (L), CH3SCH2CH2P(C6H5)CH2CH2P(C6H5)CH2CH2SCH3, and Molecular Structure of [Ni(rac(P)-L)2](BF4)2",
abstract = "Δ-RR,∧-SS-[Co(acac)2(rac(P)-L)]+ and [Co(acac)2(raeso(P)-L)]+ were obtained by reaction of [Co(acac)3] (acac=2, 4-pentanedionate ion) with 5, 8-diphenyl-5, 8-diphospha-2, 11-dithiadodecane (L) in 1:1 molar ratio in dichloromethane in the presence of active charcoal, no Δ-SS,∧-RR isomer of the rac(P)-L complex being formed. Five-coordinate [Ni(rac(P)-L)2]2+ and [Ni(raeso(P)-L)2]2+ were yielded by reaction of Ni(II) and L in 1:2 molar ratio in methanol, and the molecular structure of less soluble [Ni(rac(P)-L)2](BF4)2 was determined by X-ray analysis. Crystal data: monoclinic, space group P21/n, a=17.136(3), b=20.134(5), c=14.106(3) {\AA}, β=93.30(2)°, V=4859(2) {\AA}3, Z=4, R=0.089 for 8001 reflections. The Ni atom is surrounded square pyramidally by four P atoms in the basal plane and one S atom at the apical position with distances of the Ni-P: 2.214(2)-2.234(2) {\AA} and the Ni-S: 2.603(2) {\AA}. Both [Ni(rac(P)-L)2]2+ and [Ni(meso(P)-L)2]2+ in CH2Cl2 solutions exchange four -SCH3 groups at the apical positin on the NMR time scale. White [Cu(rac(P)-L)]BF4 was precipitated selectively by reaction of Cu(BF4)2 • 6H2O and L in 1:1 molar ratio in ethanol.",
author = "Tetsuji Kitagawa and Masakazu Kita and Kazuo Kashiwabara and Junnosuke Fujita",
year = "1991",
month = "10",
day = "1",
language = "English",
volume = "64",
pages = "2942--2947",
journal = "Bulletin of the Chemical Society of Japan",
issn = "0009-2673",
publisher = "Chemical Society of Japan",
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TY - JOUR

T1 - Preparation and characterization of cobalt(III), Nickel(II), and Copper(I) Complexes Containing 5, 8-Diphenyl-5, 8-diphospha-2, 11-dithiadodecane (L), CH3SCH2CH2P(C6H5)CH2CH2P(C6H5)CH2CH2SCH3, and Molecular Structure of [Ni(rac(P)-L)2](BF4)2

AU - Kitagawa, Tetsuji

AU - Kita, Masakazu

AU - Kashiwabara, Kazuo

AU - Fujita, Junnosuke

PY - 1991/10/1

Y1 - 1991/10/1

N2 - Δ-RR,∧-SS-[Co(acac)2(rac(P)-L)]+ and [Co(acac)2(raeso(P)-L)]+ were obtained by reaction of [Co(acac)3] (acac=2, 4-pentanedionate ion) with 5, 8-diphenyl-5, 8-diphospha-2, 11-dithiadodecane (L) in 1:1 molar ratio in dichloromethane in the presence of active charcoal, no Δ-SS,∧-RR isomer of the rac(P)-L complex being formed. Five-coordinate [Ni(rac(P)-L)2]2+ and [Ni(raeso(P)-L)2]2+ were yielded by reaction of Ni(II) and L in 1:2 molar ratio in methanol, and the molecular structure of less soluble [Ni(rac(P)-L)2](BF4)2 was determined by X-ray analysis. Crystal data: monoclinic, space group P21/n, a=17.136(3), b=20.134(5), c=14.106(3) Å, β=93.30(2)°, V=4859(2) Å3, Z=4, R=0.089 for 8001 reflections. The Ni atom is surrounded square pyramidally by four P atoms in the basal plane and one S atom at the apical position with distances of the Ni-P: 2.214(2)-2.234(2) Å and the Ni-S: 2.603(2) Å. Both [Ni(rac(P)-L)2]2+ and [Ni(meso(P)-L)2]2+ in CH2Cl2 solutions exchange four -SCH3 groups at the apical positin on the NMR time scale. White [Cu(rac(P)-L)]BF4 was precipitated selectively by reaction of Cu(BF4)2 • 6H2O and L in 1:1 molar ratio in ethanol.

AB - Δ-RR,∧-SS-[Co(acac)2(rac(P)-L)]+ and [Co(acac)2(raeso(P)-L)]+ were obtained by reaction of [Co(acac)3] (acac=2, 4-pentanedionate ion) with 5, 8-diphenyl-5, 8-diphospha-2, 11-dithiadodecane (L) in 1:1 molar ratio in dichloromethane in the presence of active charcoal, no Δ-SS,∧-RR isomer of the rac(P)-L complex being formed. Five-coordinate [Ni(rac(P)-L)2]2+ and [Ni(raeso(P)-L)2]2+ were yielded by reaction of Ni(II) and L in 1:2 molar ratio in methanol, and the molecular structure of less soluble [Ni(rac(P)-L)2](BF4)2 was determined by X-ray analysis. Crystal data: monoclinic, space group P21/n, a=17.136(3), b=20.134(5), c=14.106(3) Å, β=93.30(2)°, V=4859(2) Å3, Z=4, R=0.089 for 8001 reflections. The Ni atom is surrounded square pyramidally by four P atoms in the basal plane and one S atom at the apical position with distances of the Ni-P: 2.214(2)-2.234(2) Å and the Ni-S: 2.603(2) Å. Both [Ni(rac(P)-L)2]2+ and [Ni(meso(P)-L)2]2+ in CH2Cl2 solutions exchange four -SCH3 groups at the apical positin on the NMR time scale. White [Cu(rac(P)-L)]BF4 was precipitated selectively by reaction of Cu(BF4)2 • 6H2O and L in 1:1 molar ratio in ethanol.

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