Preparation and crystal and molecular structure of [MoO(SCH2CH2PPh2)2]

Joseph Chatt; Jonathan R. Dilworth; James A. Schmutz; Jon A. Zubieta

doi:10.1039/DT9790001595

Preparation and crystal and molecular structure of [MoO(SCH₂CH₂PPh₂)₂]

Joseph Chatt, Jonathan R. Dilworth, James A. Schmutz, Jon A. Zubieta

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

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Abstract

The title complex has been prepared by reaction of [MoO₂(acac)₂] (acac = pentane-2,4-dionate) with an excess of Ph₂PCH₂CH₂SH in methanol or toluene. The oxo-group can be protonated with anhydrous HBF₄ in benzene to give [Mo(OH₂)(SCH₂CH₂PPh₂) ₂][BF₄]₂ but does not undergo condensation-type reactions with hydrazines even under forcing conditions. The complex [MoO(SCH₂CH₂PPh₂)₂] crystallises in the orthorhombic space group P2₁2₁2₁ with four molecules in a unit cell of dimensions a = 10.263(3), b = 10.246(1), and c = 26.657(5) Å. The structure has been solved using 2 179 symmetry-independent reflections with I > 2.58σ(I) collected by counter techniques using Cu-K_α radiation. Refinement by full-matrix least squares, using anisotropic temperature factors for all non-carbon and non-hydrogen atoms, gives a final R factor of 0.063. The co-ordination polyhedron is intermediate between trigonal-bipyramidal and square-pyramidal geometries. The bond distances to Mo are Mo-O 1.733(9), Mo-S(av.) 2.360(4), and Mo-P(av.) 2.484(4) Å.

Original language	English (US)
Pages (from-to)	1595-1599
Number of pages	5
Journal	Journal of the Chemical Society, Dalton Transactions
Issue number	10
DOIs	https://doi.org/10.1039/DT9790001595
State	Published - 1979
Externally published	Yes

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Chemistry(all)

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@article{6c6960f0f7284c37890062c51082d735,

title = "Preparation and crystal and molecular structure of [MoO(SCH2CH2PPh2)2]",

abstract = "The title complex has been prepared by reaction of [MoO2(acac)2] (acac = pentane-2,4-dionate) with an excess of Ph2PCH2CH2SH in methanol or toluene. The oxo-group can be protonated with anhydrous HBF4 in benzene to give [Mo(OH2)(SCH2CH2PPh2) 2][BF4]2 but does not undergo condensation-type reactions with hydrazines even under forcing conditions. The complex [MoO(SCH2CH2PPh2)2] crystallises in the orthorhombic space group P212121 with four molecules in a unit cell of dimensions a = 10.263(3), b = 10.246(1), and c = 26.657(5) {\AA}. The structure has been solved using 2 179 symmetry-independent reflections with I > 2.58σ(I) collected by counter techniques using Cu-Kα radiation. Refinement by full-matrix least squares, using anisotropic temperature factors for all non-carbon and non-hydrogen atoms, gives a final R factor of 0.063. The co-ordination polyhedron is intermediate between trigonal-bipyramidal and square-pyramidal geometries. The bond distances to Mo are Mo-O 1.733(9), Mo-S(av.) 2.360(4), and Mo-P(av.) 2.484(4) {\AA}.",

author = "Joseph Chatt and Dilworth, {Jonathan R.} and Schmutz, {James A.} and Zubieta, {Jon A.}",

note = "Funding Information: There are nosignificant intermolecular interactions as shown in theunit-cell packing stereogram (Figure 2).The structural investigation was supported by a grant(number GM22566A) from the National Institutes ofHealth (to J , A. Copyright: Copyright 2007 Elsevier B.V., All rights reserved.",

year = "1979",

doi = "10.1039/DT9790001595",

language = "English (US)",

pages = "1595--1599",

journal = "Dalton Transactions",

issn = "0300-9246",

publisher = "Royal Society of Chemistry",

number = "10",

}

TY - JOUR

T1 - Preparation and crystal and molecular structure of [MoO(SCH2CH2PPh2)2]

AU - Chatt, Joseph

AU - Dilworth, Jonathan R.

AU - Schmutz, James A.

AU - Zubieta, Jon A.

N1 - Funding Information: There are nosignificant intermolecular interactions as shown in theunit-cell packing stereogram (Figure 2).The structural investigation was supported by a grant(number GM22566A) from the National Institutes ofHealth (to J , A. Copyright: Copyright 2007 Elsevier B.V., All rights reserved.

PY - 1979

Y1 - 1979

N2 - The title complex has been prepared by reaction of [MoO2(acac)2] (acac = pentane-2,4-dionate) with an excess of Ph2PCH2CH2SH in methanol or toluene. The oxo-group can be protonated with anhydrous HBF4 in benzene to give [Mo(OH2)(SCH2CH2PPh2) 2][BF4]2 but does not undergo condensation-type reactions with hydrazines even under forcing conditions. The complex [MoO(SCH2CH2PPh2)2] crystallises in the orthorhombic space group P212121 with four molecules in a unit cell of dimensions a = 10.263(3), b = 10.246(1), and c = 26.657(5) Å. The structure has been solved using 2 179 symmetry-independent reflections with I > 2.58σ(I) collected by counter techniques using Cu-Kα radiation. Refinement by full-matrix least squares, using anisotropic temperature factors for all non-carbon and non-hydrogen atoms, gives a final R factor of 0.063. The co-ordination polyhedron is intermediate between trigonal-bipyramidal and square-pyramidal geometries. The bond distances to Mo are Mo-O 1.733(9), Mo-S(av.) 2.360(4), and Mo-P(av.) 2.484(4) Å.

AB - The title complex has been prepared by reaction of [MoO2(acac)2] (acac = pentane-2,4-dionate) with an excess of Ph2PCH2CH2SH in methanol or toluene. The oxo-group can be protonated with anhydrous HBF4 in benzene to give [Mo(OH2)(SCH2CH2PPh2) 2][BF4]2 but does not undergo condensation-type reactions with hydrazines even under forcing conditions. The complex [MoO(SCH2CH2PPh2)2] crystallises in the orthorhombic space group P212121 with four molecules in a unit cell of dimensions a = 10.263(3), b = 10.246(1), and c = 26.657(5) Å. The structure has been solved using 2 179 symmetry-independent reflections with I > 2.58σ(I) collected by counter techniques using Cu-Kα radiation. Refinement by full-matrix least squares, using anisotropic temperature factors for all non-carbon and non-hydrogen atoms, gives a final R factor of 0.063. The co-ordination polyhedron is intermediate between trigonal-bipyramidal and square-pyramidal geometries. The bond distances to Mo are Mo-O 1.733(9), Mo-S(av.) 2.360(4), and Mo-P(av.) 2.484(4) Å.

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U2 - 10.1039/DT9790001595

DO - 10.1039/DT9790001595

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SN - 0300-9246

SP - 1595

EP - 1599

JO - Dalton Transactions

JF - Dalton Transactions

IS - 10

ER -

Preparation and crystal and molecular structure of [MoO(SCH₂CH₂PPh₂)₂]

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