Synthesis and structural characterization of a binuclear Mo(V)-oxo complex which contains both thiolate and tertiary phosphine ligands, [Mo2O4(2,4,6-i-Pr3C6H2S)2(PPh3)2]

Philip T. Blower; John R. Dilworth; Deborah Macherone; Jon Zubieta

doi:10.1016/S0020-1693(00)85879-X

Synthesis and structural characterization of a binuclear Mo(V)-oxo complex which contains both thiolate and tertiary phosphine ligands, [Mo₂O₄(2,4,6-i-Pr₃C₆H₂S)₂(PPh₃)₂]

Philip T. Blower, John R. Dilworth, Deborah Macherone, Jon Zubieta

Department of Chemistry

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Abstract

The reaction of [MoCl₄(PPh₃)₂] with 2,4,6-i-Pr₃C₆H₂SH (TIPTH) in CH₂Cl₂ followed by introduction of an excess of O₂, yields the binuclear Mo(V) complex, [Mo₂O₄(2,4,6-i-Pr₃C₆H₂S)₂(PPh₃)₂]. An X-ray diffraction study of this complex revealed the presence of the common [Mo₂O₄]²⁺ core, with each Mo(V) center additionally coordinated to the phosphorus donor of a triphenylphosphine and to the sulfur donor of a terminally ligated TIPT group. Crystal data for [Mo₂O₄(2,4,6-i-Pr₃C₆H₂S)₂]: orthorhombic space group Pccn, a = 29.772(4), b =22.193(4), c= 19.016(3) Å, V= 12564.6(11) Å³, D_calc = 1.32 g cm^-3, Z = 8. Structure solution and refinement based on 1279 reflections (Mo Koα, λ = 0.71073 Å, 2° ≤ 2θ ≤ 45°) converged at a conventional discrepancy value of 0.063.

Original language	English (US)
Pages (from-to)	203-208
Number of pages	6
Journal	Inorganica Chimica Acta
Volume	179
Issue number	2
DOIs	https://doi.org/10.1016/S0020-1693(00)85879-X
State	Published - Jan 15 1991

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

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Synthesis and structural characterization of a binuclear Mo(V)-oxo complex which contains both thiolate and tertiary phosphine ligands, [Mo₂O₄(2,4,6-i-Pr₃C₆H₂S)₂(PPh₃)₂]. / Blower, Philip T.; Dilworth, John R.; Macherone, Deborah et al.
In: Inorganica Chimica Acta, Vol. 179, No. 2, 15.01.1991, p. 203-208.

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

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title = "Synthesis and structural characterization of a binuclear Mo(V)-oxo complex which contains both thiolate and tertiary phosphine ligands, [Mo2O4(2,4,6-i-Pr3C6H2S)2(PPh3)2]",

abstract = "The reaction of [MoCl4(PPh3)2] with 2,4,6-i-Pr3C6H2SH (TIPTH) in CH2Cl2 followed by introduction of an excess of O2, yields the binuclear Mo(V) complex, [Mo2O4(2,4,6-i-Pr3C6H2S)2(PPh3)2]. An X-ray diffraction study of this complex revealed the presence of the common [Mo2O4]2+ core, with each Mo(V) center additionally coordinated to the phosphorus donor of a triphenylphosphine and to the sulfur donor of a terminally ligated TIPT group. Crystal data for [Mo2O4(2,4,6-i-Pr3C6H2S)2]: orthorhombic space group Pccn, a = 29.772(4), b =22.193(4), c= 19.016(3) {\AA}, V= 12564.6(11) {\AA}3, Dcalc = 1.32 g cm-3, Z = 8. Structure solution and refinement based on 1279 reflections (Mo Koα, λ = 0.71073 {\AA}, 2° ≤ 2θ ≤ 45°) converged at a conventional discrepancy value of 0.063.",

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T1 - Synthesis and structural characterization of a binuclear Mo(V)-oxo complex which contains both thiolate and tertiary phosphine ligands, [Mo2O4(2,4,6-i-Pr3C6H2S)2(PPh3)2]

AU - Blower, Philip T.

AU - Dilworth, John R.

AU - Macherone, Deborah

AU - Zubieta, Jon

PY - 1991/1/15

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N2 - The reaction of [MoCl4(PPh3)2] with 2,4,6-i-Pr3C6H2SH (TIPTH) in CH2Cl2 followed by introduction of an excess of O2, yields the binuclear Mo(V) complex, [Mo2O4(2,4,6-i-Pr3C6H2S)2(PPh3)2]. An X-ray diffraction study of this complex revealed the presence of the common [Mo2O4]2+ core, with each Mo(V) center additionally coordinated to the phosphorus donor of a triphenylphosphine and to the sulfur donor of a terminally ligated TIPT group. Crystal data for [Mo2O4(2,4,6-i-Pr3C6H2S)2]: orthorhombic space group Pccn, a = 29.772(4), b =22.193(4), c= 19.016(3) Å, V= 12564.6(11) Å3, Dcalc = 1.32 g cm-3, Z = 8. Structure solution and refinement based on 1279 reflections (Mo Koα, λ = 0.71073 Å, 2° ≤ 2θ ≤ 45°) converged at a conventional discrepancy value of 0.063.

AB - The reaction of [MoCl4(PPh3)2] with 2,4,6-i-Pr3C6H2SH (TIPTH) in CH2Cl2 followed by introduction of an excess of O2, yields the binuclear Mo(V) complex, [Mo2O4(2,4,6-i-Pr3C6H2S)2(PPh3)2]. An X-ray diffraction study of this complex revealed the presence of the common [Mo2O4]2+ core, with each Mo(V) center additionally coordinated to the phosphorus donor of a triphenylphosphine and to the sulfur donor of a terminally ligated TIPT group. Crystal data for [Mo2O4(2,4,6-i-Pr3C6H2S)2]: orthorhombic space group Pccn, a = 29.772(4), b =22.193(4), c= 19.016(3) Å, V= 12564.6(11) Å3, Dcalc = 1.32 g cm-3, Z = 8. Structure solution and refinement based on 1279 reflections (Mo Koα, λ = 0.71073 Å, 2° ≤ 2θ ≤ 45°) converged at a conventional discrepancy value of 0.063.

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Synthesis and structural characterization of a binuclear Mo(V)-oxo complex which contains both thiolate and tertiary phosphine ligands, [Mo₂O₄(2,4,6-i-Pr₃C₆H₂S)₂(PPh₃)₂]

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