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

doi:10.1246/bcsj.64.2942

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)CH₂CH₂SCH_3, and Molecular Structure of [Ni(rac(P)-L)₂](BF₄)₂

Tetsuji Kitagawa, Masakazu Kita, Kazuo Kashiwabara, Junnosuke Fujita

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

9 Citations (Scopus)

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 language	English
Pages (from-to)	2942-2947
Number of pages	6
Journal	Bulletin of the Chemical Society of Japan
Volume	64
Issue number	10
DOIs	https://doi.org/10.1246/bcsj.64.2942
Publication status	Published - Oct 1991
Externally published	Yes

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Chemistry(all)

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Kitagawa, T., Kita, M., Kashiwabara, K., & Fujita, J. (1991). 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)CH₂CH₂SCH_3, and Molecular Structure of [Ni(rac(P)-L)₂](BF₄)₂. Bulletin of the Chemical Society of Japan, 64(10), 2942-2947. https://doi.org/10.1246/bcsj.64.2942

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)CH₂CH₂SCH_3, and Molecular Structure of [Ni(rac(P)-L)₂](BF₄)₂. / Kitagawa, Tetsuji; Kita, Masakazu; Kashiwabara, Kazuo et al.

In: Bulletin of the Chemical Society of Japan, Vol. 64, No. 10, 10.1991, p. 2942-2947.

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

Kitagawa, T, Kita, M, Kashiwabara, K & Fujita, J 1991, '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)CH₂CH₂SCH_3, and Molecular Structure of [Ni(rac(P)-L)₂](BF₄)₂', Bulletin of the Chemical Society of Japan, vol. 64, no. 10, pp. 2942-2947. https://doi.org/10.1246/bcsj.64.2942

Kitagawa T, Kita M, Kashiwabara K, Fujita J. 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)CH₂CH₂SCH_3, and Molecular Structure of [Ni(rac(P)-L)₂](BF₄)₂. Bulletin of the Chemical Society of Japan. 1991 Oct;64(10):2942-2947. doi: 10.1246/bcsj.64.2942

Kitagawa, Tetsuji ; Kita, Masakazu ; Kashiwabara, Kazuo et al. / 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)CH₂CH₂SCH_3, and Molecular Structure of [Ni(rac(P)-L)₂](BF₄)₂. In: Bulletin of the Chemical Society of Japan. 1991 ; Vol. 64, No. 10. pp. 2942-2947.

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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",

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doi = "10.1246/bcsj.64.2942",

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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

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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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