Syntheses and Crystal Structures of Bis(dimethyldithiocarbamato)-(4,6-diphenyl-4,6-diphosphanonane-1,9-diammonium) cobalt(III) and Chloro(4,9-diphenyl-4,9-diphosphadodecane-1,12-diamine)nickel(II) Complexes

Kazuo Kashiwabara, Masayuki Watanabe, Masakazu Kita, Takayoshi Suzuki

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Abstract

The reaction of tetramethylthiuram disulfide with a methanol solution containing CoCl2·6H2O and 4,6-diphenyl-4,6-diphosphanonane-1,9-diamine (313NPPN) gave complexes of [Co(dtc)2{rac(P)- or meso(P)-313HNPPNH}]3+ (313HNPPNH=diprotonated form of 313NPPN, dtc=dimethyldithiocarbamate ion). The crystal structure of the perchlorate salt of the meso(P) isomer was determined by X-ray analysis. Crystal data: monoclinic, P21/c, a=10.789(2), b=30.325(9), c=12.888(2) Å, β=102.06(1)°, V=4123(1) Å3, Dx=1.55 g cm-3, Z=4, and R=0.077 for 3347 reflections. The 313HNPPNH ligand in the complex coordinates to the Co(III) center through two phosphorus atoms as a didentate four-membered chelate ligand. The crystal structure of [Co(dtc)2{NH2(CH2)3P(CH 2OH)(C6H5)}]B(C6H5) 4, which formed as a by-product in the preparation of the above Co(III)-313HNPPNH complexes, was also determined. Crystal data: triclinic, P1̄, a=13.817(2), b=15.277(3), c=10.737(2) Å, α=109.90(1), β=94.14(2), γ=101.00(1)°, V=2068.8(7) Å3, Dx=1.31 g cm-3, Z=2, and R=0.053 for 4303 reflections. [NiCl{rac(P)-343NPPN}]PF6 (343NPPN=4,9-diphenyl-4,9-diphosphadodecane-1,12-diamine) was prepared by the reaction of 343NPPN with NiCl2·6H2O, and the crystal structure was determined. Crystal data: monoclinic, P21/n, a=8.367(2), b=24.058(2), c=13.988(2) Å, β=106.17(1)°, V=2704(1) Å3, Dx=1.54 g cm-3, Z=4, and R=0.053 for 3043 reflections. The geometry of the complex is a distorted square pyramid with a chloride ion at the apical position, and the 343NPPN ligand functions as a tetradentate chelate ligand.

Original languageEnglish
Pages (from-to)1947-1953
Number of pages7
JournalBulletin of the Chemical Society of Japan
Volume69
Issue number7
Publication statusPublished - 1996
Externally publishedYes

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Diamines
Cobalt
Nickel
Crystal structure
Ligands
Crystals
Dimethyldithiocarbamate
Thiram
Ions
X ray analysis
Isomers
Phosphorus
Byproducts
Methanol
Chlorides
Salts
Atoms
Geometry
diphenyl

ASJC Scopus subject areas

  • Chemistry(all)

Cite this

@article{6040e6d058cb40f5b0f617def0aa20af,
title = "Syntheses and Crystal Structures of Bis(dimethyldithiocarbamato)-(4,6-diphenyl-4,6-diphosphanonane-1,9-diammonium) cobalt(III) and Chloro(4,9-diphenyl-4,9-diphosphadodecane-1,12-diamine)nickel(II) Complexes",
abstract = "The reaction of tetramethylthiuram disulfide with a methanol solution containing CoCl2·6H2O and 4,6-diphenyl-4,6-diphosphanonane-1,9-diamine (313NPPN) gave complexes of [Co(dtc)2{rac(P)- or meso(P)-313HNPPNH}]3+ (313HNPPNH=diprotonated form of 313NPPN, dtc=dimethyldithiocarbamate ion). The crystal structure of the perchlorate salt of the meso(P) isomer was determined by X-ray analysis. Crystal data: monoclinic, P21/c, a=10.789(2), b=30.325(9), c=12.888(2) {\AA}, β=102.06(1)°, V=4123(1) {\AA}3, Dx=1.55 g cm-3, Z=4, and R=0.077 for 3347 reflections. The 313HNPPNH ligand in the complex coordinates to the Co(III) center through two phosphorus atoms as a didentate four-membered chelate ligand. The crystal structure of [Co(dtc)2{NH2(CH2)3P(CH 2OH)(C6H5)}]B(C6H5) 4, which formed as a by-product in the preparation of the above Co(III)-313HNPPNH complexes, was also determined. Crystal data: triclinic, P1̄, a=13.817(2), b=15.277(3), c=10.737(2) {\AA}, α=109.90(1), β=94.14(2), γ=101.00(1)°, V=2068.8(7) {\AA}3, Dx=1.31 g cm-3, Z=2, and R=0.053 for 4303 reflections. [NiCl{rac(P)-343NPPN}]PF6 (343NPPN=4,9-diphenyl-4,9-diphosphadodecane-1,12-diamine) was prepared by the reaction of 343NPPN with NiCl2·6H2O, and the crystal structure was determined. Crystal data: monoclinic, P21/n, a=8.367(2), b=24.058(2), c=13.988(2) {\AA}, β=106.17(1)°, V=2704(1) {\AA}3, Dx=1.54 g cm-3, Z=4, and R=0.053 for 3043 reflections. The geometry of the complex is a distorted square pyramid with a chloride ion at the apical position, and the 343NPPN ligand functions as a tetradentate chelate ligand.",
author = "Kazuo Kashiwabara and Masayuki Watanabe and Masakazu Kita and Takayoshi Suzuki",
year = "1996",
language = "English",
volume = "69",
pages = "1947--1953",
journal = "Bulletin of the Chemical Society of Japan",
issn = "0009-2673",
publisher = "Chemical Society of Japan",
number = "7",

}

TY - JOUR

T1 - Syntheses and Crystal Structures of Bis(dimethyldithiocarbamato)-(4,6-diphenyl-4,6-diphosphanonane-1,9-diammonium) cobalt(III) and Chloro(4,9-diphenyl-4,9-diphosphadodecane-1,12-diamine)nickel(II) Complexes

AU - Kashiwabara, Kazuo

AU - Watanabe, Masayuki

AU - Kita, Masakazu

AU - Suzuki, Takayoshi

PY - 1996

Y1 - 1996

N2 - The reaction of tetramethylthiuram disulfide with a methanol solution containing CoCl2·6H2O and 4,6-diphenyl-4,6-diphosphanonane-1,9-diamine (313NPPN) gave complexes of [Co(dtc)2{rac(P)- or meso(P)-313HNPPNH}]3+ (313HNPPNH=diprotonated form of 313NPPN, dtc=dimethyldithiocarbamate ion). The crystal structure of the perchlorate salt of the meso(P) isomer was determined by X-ray analysis. Crystal data: monoclinic, P21/c, a=10.789(2), b=30.325(9), c=12.888(2) Å, β=102.06(1)°, V=4123(1) Å3, Dx=1.55 g cm-3, Z=4, and R=0.077 for 3347 reflections. The 313HNPPNH ligand in the complex coordinates to the Co(III) center through two phosphorus atoms as a didentate four-membered chelate ligand. The crystal structure of [Co(dtc)2{NH2(CH2)3P(CH 2OH)(C6H5)}]B(C6H5) 4, which formed as a by-product in the preparation of the above Co(III)-313HNPPNH complexes, was also determined. Crystal data: triclinic, P1̄, a=13.817(2), b=15.277(3), c=10.737(2) Å, α=109.90(1), β=94.14(2), γ=101.00(1)°, V=2068.8(7) Å3, Dx=1.31 g cm-3, Z=2, and R=0.053 for 4303 reflections. [NiCl{rac(P)-343NPPN}]PF6 (343NPPN=4,9-diphenyl-4,9-diphosphadodecane-1,12-diamine) was prepared by the reaction of 343NPPN with NiCl2·6H2O, and the crystal structure was determined. Crystal data: monoclinic, P21/n, a=8.367(2), b=24.058(2), c=13.988(2) Å, β=106.17(1)°, V=2704(1) Å3, Dx=1.54 g cm-3, Z=4, and R=0.053 for 3043 reflections. The geometry of the complex is a distorted square pyramid with a chloride ion at the apical position, and the 343NPPN ligand functions as a tetradentate chelate ligand.

AB - The reaction of tetramethylthiuram disulfide with a methanol solution containing CoCl2·6H2O and 4,6-diphenyl-4,6-diphosphanonane-1,9-diamine (313NPPN) gave complexes of [Co(dtc)2{rac(P)- or meso(P)-313HNPPNH}]3+ (313HNPPNH=diprotonated form of 313NPPN, dtc=dimethyldithiocarbamate ion). The crystal structure of the perchlorate salt of the meso(P) isomer was determined by X-ray analysis. Crystal data: monoclinic, P21/c, a=10.789(2), b=30.325(9), c=12.888(2) Å, β=102.06(1)°, V=4123(1) Å3, Dx=1.55 g cm-3, Z=4, and R=0.077 for 3347 reflections. The 313HNPPNH ligand in the complex coordinates to the Co(III) center through two phosphorus atoms as a didentate four-membered chelate ligand. The crystal structure of [Co(dtc)2{NH2(CH2)3P(CH 2OH)(C6H5)}]B(C6H5) 4, which formed as a by-product in the preparation of the above Co(III)-313HNPPNH complexes, was also determined. Crystal data: triclinic, P1̄, a=13.817(2), b=15.277(3), c=10.737(2) Å, α=109.90(1), β=94.14(2), γ=101.00(1)°, V=2068.8(7) Å3, Dx=1.31 g cm-3, Z=2, and R=0.053 for 4303 reflections. [NiCl{rac(P)-343NPPN}]PF6 (343NPPN=4,9-diphenyl-4,9-diphosphadodecane-1,12-diamine) was prepared by the reaction of 343NPPN with NiCl2·6H2O, and the crystal structure was determined. Crystal data: monoclinic, P21/n, a=8.367(2), b=24.058(2), c=13.988(2) Å, β=106.17(1)°, V=2704(1) Å3, Dx=1.54 g cm-3, Z=4, and R=0.053 for 3043 reflections. The geometry of the complex is a distorted square pyramid with a chloride ion at the apical position, and the 343NPPN ligand functions as a tetradentate chelate ligand.

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M3 - Article

AN - SCOPUS:2742520176

VL - 69

SP - 1947

EP - 1953

JO - Bulletin of the Chemical Society of Japan

JF - Bulletin of the Chemical Society of Japan

SN - 0009-2673

IS - 7

ER -