Preparation and molecular structures of [Co,(S2O- S,S')(Me2PCH2CH2PMe2)2]ClO4 and [Co(S2PMe2)2(Me2PCH2CH2PMe2)]BF4

M. Kita, K. Kashiwabara, J. Fujita, S. Kurachi, Shigeru Ohba

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Abstract

The reaction of elemental sulfur S8 with [Co(dmpe)2](BF4)2 in a mixture of methanol and benzene gave a novel S,S'-coordinated disulfur oxide cobalt(III) complex, [Co(S2O-S,S')(dmpe)2]ClO4 (1), and a dimethyldithiophosphinato complex. [Co(S2PMe2)2(dmpe)]BF4 (2). The molecular structures of these complexes were determined by X-ray structure analyses. Crystal data for complex 1: monoclinic, P21/n, a=14.702(3), b=11.645(1), c=14.333(2) Å, β=109.90(2)°, V=2307.4(2) Å3. D(x)=1.55, D(m)=1.54(3) g cm-3. Z=4, R=0.039 for 4542 reflections. Crystal data for complex 2: orthorhombic, Pnc2, a=13.383(3), b=12.333(2), c=13.742(3) Å, V=2268.1(8) Å3, D(x)=1.60, D(m)=1.59(2) g cm-3, Z=4, R=0.075 for 2060 reflections. The central sulfur atom of the S-S-O group in complex 1 exerts a larger trans influence than does the terminal sulfur.

Original languageEnglish
Pages (from-to)3686-3692
Number of pages7
JournalBulletin of the Chemical Society of Japan
Volume66
Issue number12
Publication statusPublished - 1993
Externally publishedYes

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Sulfur
Molecular structure
Crystals
Benzene
Methanol
X rays
Atoms
perchlorate

ASJC Scopus subject areas

  • Chemistry(all)

Cite this

Preparation and molecular structures of [Co,(S2O- S,S')(Me2PCH2CH2PMe2)2]ClO4 and [Co(S2PMe2)2(Me2PCH2CH2PMe2)]BF4. / Kita, M.; Kashiwabara, K.; Fujita, J.; Kurachi, S.; Ohba, Shigeru.

In: Bulletin of the Chemical Society of Japan, Vol. 66, No. 12, 1993, p. 3686-3692.

Research output: Contribution to journalArticle

Kita, M. ; Kashiwabara, K. ; Fujita, J. ; Kurachi, S. ; Ohba, Shigeru. / Preparation and molecular structures of [Co,(S2O- S,S')(Me2PCH2CH2PMe2)2]ClO4 and [Co(S2PMe2)2(Me2PCH2CH2PMe2)]BF4. In: Bulletin of the Chemical Society of Japan. 1993 ; Vol. 66, No. 12. pp. 3686-3692.
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title = "Preparation and molecular structures of [Co,(S2O- S,S')(Me2PCH2CH2PMe2)2]ClO4 and [Co(S2PMe2)2(Me2PCH2CH2PMe2)]BF4",
abstract = "The reaction of elemental sulfur S8 with [Co(dmpe)2](BF4)2 in a mixture of methanol and benzene gave a novel S,S'-coordinated disulfur oxide cobalt(III) complex, [Co(S2O-S,S')(dmpe)2]ClO4 (1), and a dimethyldithiophosphinato complex. [Co(S2PMe2)2(dmpe)]BF4 (2). The molecular structures of these complexes were determined by X-ray structure analyses. Crystal data for complex 1: monoclinic, P21/n, a=14.702(3), b=11.645(1), c=14.333(2) {\AA}, β=109.90(2)°, V=2307.4(2) {\AA}3. D(x)=1.55, D(m)=1.54(3) g cm-3. Z=4, R=0.039 for 4542 reflections. Crystal data for complex 2: orthorhombic, Pnc2, a=13.383(3), b=12.333(2), c=13.742(3) {\AA}, V=2268.1(8) {\AA}3, D(x)=1.60, D(m)=1.59(2) g cm-3, Z=4, R=0.075 for 2060 reflections. The central sulfur atom of the S-S-O group in complex 1 exerts a larger trans influence than does the terminal sulfur.",
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T1 - Preparation and molecular structures of [Co,(S2O- S,S')(Me2PCH2CH2PMe2)2]ClO4 and [Co(S2PMe2)2(Me2PCH2CH2PMe2)]BF4

AU - Kita, M.

AU - Kashiwabara, K.

AU - Fujita, J.

AU - Kurachi, S.

AU - Ohba, Shigeru

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N2 - The reaction of elemental sulfur S8 with [Co(dmpe)2](BF4)2 in a mixture of methanol and benzene gave a novel S,S'-coordinated disulfur oxide cobalt(III) complex, [Co(S2O-S,S')(dmpe)2]ClO4 (1), and a dimethyldithiophosphinato complex. [Co(S2PMe2)2(dmpe)]BF4 (2). The molecular structures of these complexes were determined by X-ray structure analyses. Crystal data for complex 1: monoclinic, P21/n, a=14.702(3), b=11.645(1), c=14.333(2) Å, β=109.90(2)°, V=2307.4(2) Å3. D(x)=1.55, D(m)=1.54(3) g cm-3. Z=4, R=0.039 for 4542 reflections. Crystal data for complex 2: orthorhombic, Pnc2, a=13.383(3), b=12.333(2), c=13.742(3) Å, V=2268.1(8) Å3, D(x)=1.60, D(m)=1.59(2) g cm-3, Z=4, R=0.075 for 2060 reflections. The central sulfur atom of the S-S-O group in complex 1 exerts a larger trans influence than does the terminal sulfur.

AB - The reaction of elemental sulfur S8 with [Co(dmpe)2](BF4)2 in a mixture of methanol and benzene gave a novel S,S'-coordinated disulfur oxide cobalt(III) complex, [Co(S2O-S,S')(dmpe)2]ClO4 (1), and a dimethyldithiophosphinato complex. [Co(S2PMe2)2(dmpe)]BF4 (2). The molecular structures of these complexes were determined by X-ray structure analyses. Crystal data for complex 1: monoclinic, P21/n, a=14.702(3), b=11.645(1), c=14.333(2) Å, β=109.90(2)°, V=2307.4(2) Å3. D(x)=1.55, D(m)=1.54(3) g cm-3. Z=4, R=0.039 for 4542 reflections. Crystal data for complex 2: orthorhombic, Pnc2, a=13.383(3), b=12.333(2), c=13.742(3) Å, V=2268.1(8) Å3, D(x)=1.60, D(m)=1.59(2) g cm-3, Z=4, R=0.075 for 2060 reflections. The central sulfur atom of the S-S-O group in complex 1 exerts a larger trans influence than does the terminal sulfur.

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