Structural characterization of MoOCl3(THF)2, the pre-reagent for Kauffmann olefination reactions

Christoph Vitzthumecker; Fred Robinson; Arno Pfitzner

doi:10.1007/s00706-016-1881-9

Structural characterization of MoOCl₃(THF)₂, the pre-reagent for Kauffmann olefination reactions

Christoph Vitzthumecker, Fred Robinson, Arno Pfitzner

Department of Chemistry

University of Regensburg

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

3 Citations (SciVal)

Abstract

Single crystals of molybdenum-oxy-di-tetrahydrofuran-trichloride were obtained by the reaction of Mo₂Cl₁₀, tetrahydrofuran, sulfur, and P₄S₃ in carbon disulfide after layering the solution with n-hexane. Single crystal structure determination at T = 123 K reveals that MoOCl₃(THF)₂ crystalizes in the orthorhombic space group P2₁2₁2₁ with the lattice constants a = 7.8620(9) Å, b = 12.302(1) Å, c = 14.043(2) Å, V = 1304.10(3) Å³, and Z = 4. EPR experiments on the solid compound showed a g value of 1.94 at 347.46 mT, which accords to a Mo(V) species. The electronic structure of the title compound was investigated with DFT methods.

Original language	English
Pages (from-to)	629-633
Number of pages	5
Journal	Chemical Monthly
Volume	148
Issue number	4
Early online date	19 Jan 2017
DOIs	https://doi.org/10.1007/s00706-016-1881-9
Publication status	Published - 1 Apr 2017

Keywords

EPR spectroscopy
Kauffmann olefination
Quantum chemical calculations
X-ray structure determination

ASJC Scopus subject areas

General Chemistry

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10.1007/s00706-016-1881-9

Cite this

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title = "Structural characterization of MoOCl3(THF)2, the pre-reagent for Kauffmann olefination reactions",

abstract = "Single crystals of molybdenum-oxy-di-tetrahydrofuran-trichloride were obtained by the reaction of Mo2Cl10, tetrahydrofuran, sulfur, and P4S3 in carbon disulfide after layering the solution with n-hexane. Single crystal structure determination at T = 123 K reveals that MoOCl3(THF)2 crystalizes in the orthorhombic space group P212121 with the lattice constants a = 7.8620(9) {\AA}, b = 12.302(1) {\AA}, c = 14.043(2) {\AA}, V = 1304.10(3) {\AA}3, and Z = 4. EPR experiments on the solid compound showed a g value of 1.94 at 347.46 mT, which accords to a Mo(V) species. The electronic structure of the title compound was investigated with DFT methods.",

keywords = "EPR spectroscopy, Kauffmann olefination, Quantum chemical calculations, X-ray structure determination",

author = "Christoph Vitzthumecker and Fred Robinson and Arno Pfitzner",

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doi = "10.1007/s00706-016-1881-9",

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journal = "Chemical Monthly",

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T1 - Structural characterization of MoOCl3(THF)2, the pre-reagent for Kauffmann olefination reactions

AU - Vitzthumecker, Christoph

AU - Robinson, Fred

AU - Pfitzner, Arno

PY - 2017/4/1

Y1 - 2017/4/1

N2 - Single crystals of molybdenum-oxy-di-tetrahydrofuran-trichloride were obtained by the reaction of Mo2Cl10, tetrahydrofuran, sulfur, and P4S3 in carbon disulfide after layering the solution with n-hexane. Single crystal structure determination at T = 123 K reveals that MoOCl3(THF)2 crystalizes in the orthorhombic space group P212121 with the lattice constants a = 7.8620(9) Å, b = 12.302(1) Å, c = 14.043(2) Å, V = 1304.10(3) Å3, and Z = 4. EPR experiments on the solid compound showed a g value of 1.94 at 347.46 mT, which accords to a Mo(V) species. The electronic structure of the title compound was investigated with DFT methods.

AB - Single crystals of molybdenum-oxy-di-tetrahydrofuran-trichloride were obtained by the reaction of Mo2Cl10, tetrahydrofuran, sulfur, and P4S3 in carbon disulfide after layering the solution with n-hexane. Single crystal structure determination at T = 123 K reveals that MoOCl3(THF)2 crystalizes in the orthorhombic space group P212121 with the lattice constants a = 7.8620(9) Å, b = 12.302(1) Å, c = 14.043(2) Å, V = 1304.10(3) Å3, and Z = 4. EPR experiments on the solid compound showed a g value of 1.94 at 347.46 mT, which accords to a Mo(V) species. The electronic structure of the title compound was investigated with DFT methods.

KW - EPR spectroscopy

KW - Kauffmann olefination

KW - Quantum chemical calculations

KW - X-ray structure determination

UR - http://www.scopus.com/inward/record.url?scp=85009914411&partnerID=8YFLogxK

U2 - 10.1007/s00706-016-1881-9

DO - 10.1007/s00706-016-1881-9

M3 - Article

AN - SCOPUS:85009914411

SN - 0026-9247

VL - 148

SP - 629

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JO - Chemical Monthly

JF - Chemical Monthly

IS - 4

ER -

Structural characterization of MoOCl₃(THF)₂, the pre-reagent for Kauffmann olefination reactions

Abstract

Keywords

ASJC Scopus subject areas

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Structural characterization of MoOCl3(THF)2, the pre-reagent for Kauffmann olefination reactions

Abstract

Keywords

ASJC Scopus subject areas

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Structural characterization of MoOCl₃(THF)₂, the pre-reagent for Kauffmann olefination reactions