Synthesis and Characterization of Rhenium Thiolate Complexes. Crystal and Molecular Structures of [NBu4][ReO(H2O)Br4 ]·2H2O,[Bu4N][ReOBr4(OPPh3)], [ReO(SC5H4N)3],[ReO(SC4H 3N2)3][ReO(OH)(SC5H4N-3,

David J. Rose; Kevin P. Maresca; Peter B. Kettler; Yuan Da Chang; Victoria Soghomomian; Qin Chen; Michael J. Abrams; Scott K. Larsen; Jon Zubieta

doi:10.1021/ic950881o

Synthesis and Characterization of Rhenium Thiolate Complexes. Crystal and Molecular Structures of [NBu₄][ReO(H₂O)Br₄ ]·2H₂O,[Bu₄N][ReOBr₄(OPPh₃)], [ReO(SC₅H₄N)₃],[ReO(SC₄H ₃N₂)₃][ReO(OH)(SC₅H₄N-3,

David J. Rose, Kevin P. Maresca, Peter B. Kettler, Yuan Da Chang, Victoria Soghomomian, Qin Chen, Michael J. Abrams, Scott K. Larsen, Jon Zubieta

Department of Chemistry

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

45 Scopus citations

Abstract

The syntheses and characterizations of six monomeric rhenium thiolate complexes and the structural characterization of two useful rhenium starting materials are presented. Pyridine-2-thiol (1) and its derivatives 3-(trimethylsilyl)-pyridine-2-thiol (2), 3,6-bis(dimethyl-tert-butylsilyl)pyridine-2-thiol (3), and pyrimidine-2-thiol (4) were reacted with [Bu₄N][ReOBr₄(H₂O)]·2H₂O (5), [Bu₄N][ReOBr₄(OPPh₃)] (6), [ReO₂(C₅H₅N)₄], and [Re{N₂CO(C₆H₅)}Cl₂(PPh ₃)₂] to give [ReO(C₅H₄NS)₃] (7), [ReO(C₈H₁₂NSiS)₃] (8), [ReO(OH)(C₁₁H₂₀NSi₂S)₂] (9), [Re{N₂CO(C₆H₅)}Cl(PPh₃) ₂(C₅H₄NS)] (10), [ReO(C₄H₃N₂S)₃] (11), and [Re{P(C₆H₅)₃}(C₄H₃N ₂S)₃] (12). Crystal data: 5, C₁₆H₄₂NO₄Br₄Re₄, tetragonal, I4̄, a = 8.779(2) Å, b = 11.614(2) Å, c = 9.397(2) Å, β = 114.67(3)°, V = 870.7(4) Å³, Z = 2, 422 reflections, R = 0.0457; 6, C₃₄H₅₁NO₂PBr₄Re, triclinic, P1̄, a = 14.437(3) Å, b = 16.589(3) Å, c = 16.783(3) Å, α = 94.87(3)°, β= 97.62(3)°, γ = 93.80(3)°, V = 3957(2) Å³, Z = 4, 6141 reflections, R = 0.0758; 7, C₁₅H₁₂N₃OS₃Re, monoclinic, P2₁/c, a = 11.533(2) Å, b = 11.385(2) Å, c = 14.039(3) Å, β= 107.97(3)°, V = 1749.8(9) Å³, Z = 4, 1869 reflections, R = 0.0322; 9, C₃₄H₆₅N₂O₂S₂Si ₄Re, triclinic, P1̄, a = 8.072(2) Å, b = 11.409(2) Å, c = 12.402(3) Å, α = 79.67(3)°, β= 74.05(3)°, γ = 86.18(3)°, V = 1080.2(5) Å³, Z = 1, 4630 reflections, R = 0.0525; 10, C₄₈H₃₉N₃OSP₂ClRe, triclinic, P1̄, a = 10.842(2) Å, b = 13.660 (3) Å, c = 17.665(4) Å, α = 86.37(3)°, β = 89.93(3)°, γ = 77.22(3)°, V = 2080.2(10) Å³, Z = 2, 4329 reflections, R = 0.0437; 11, C₁₂H₉N₆OS₃Re, orthorhombic, Pbca, a = 8.240(2) Å, b = 13.373(3) Å, C = 29.388(6) Å, V = 3238.4(16) Å³, Z = 8, 1400 reflections, R = 0.0512; 12, C₃₁H₂₆N₆S₃PCl₂Re, triclinic, P1̄, a = 9.224(2) Å, b = 12.050(2) Å, c = 17.665(4) Å, α = 89.25(3)°, β= 85.70(3)°, γ = 67.94(3)°, V = 1604.0(8) Å³, Z = 2, 3592 reflections, R = 0.0697.

Original language	English (US)
Pages (from-to)	3548-3558
Number of pages	11
Journal	Inorganic Chemistry
Volume	35
Issue number	12
DOIs	https://doi.org/10.1021/ic950881o
State	Published - 1996

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry

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10.1021/ic950881o

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Rose, D. J., Maresca, K. P., Kettler, P. B., Da Chang, Y., Soghomomian, V., Chen, Q., Abrams, M. J., Larsen, S. K., & Zubieta, J. (1996). Synthesis and Characterization of Rhenium Thiolate Complexes. Crystal and Molecular Structures of [NBu₄][ReO(H₂O)Br₄ ]·2H₂O,[Bu₄N][ReOBr₄(OPPh₃)], [ReO(SC₅H₄N)₃],[ReO(SC₄H ₃N₂)₃][ReO(OH)(SC₅H₄N-3, Inorganic Chemistry, 35(12), 3548-3558. https://doi.org/10.1021/ic950881o

Synthesis and Characterization of Rhenium Thiolate Complexes. Crystal and Molecular Structures of [NBu₄][ReO(H₂O)Br₄ ]·2H₂O,[Bu₄N][ReOBr₄(OPPh₃)], [ReO(SC₅H₄N)₃],[ReO(SC₄H ₃N₂)₃][ReO(OH)(SC₅H₄N-3, / Rose, David J.; Maresca, Kevin P.; Kettler, Peter B. et al.
In: Inorganic Chemistry, Vol. 35, No. 12, 1996, p. 3548-3558.

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

Rose, DJ, Maresca, KP, Kettler, PB, Da Chang, Y, Soghomomian, V, Chen, Q, Abrams, MJ, Larsen, SK & Zubieta, J 1996, 'Synthesis and Characterization of Rhenium Thiolate Complexes. Crystal and Molecular Structures of [NBu₄][ReO(H₂O)Br₄ ]·2H₂O,[Bu₄N][ReOBr₄(OPPh₃)], [ReO(SC₅H₄N)₃],[ReO(SC₄H ₃N₂)₃][ReO(OH)(SC₅H₄N-3,', Inorganic Chemistry, vol. 35, no. 12, pp. 3548-3558. https://doi.org/10.1021/ic950881o

@article{d31ae8ad1f004e01bcdec2830a469cfe,

title = "Synthesis and Characterization of Rhenium Thiolate Complexes. Crystal and Molecular Structures of [NBu4][ReO(H2O)Br4 ]·2H2O,[Bu4N][ReOBr4(OPPh3)], [ReO(SC5H4N)3],[ReO(SC4H 3N2)3][ReO(OH)(SC5H4N-3,",

abstract = "The syntheses and characterizations of six monomeric rhenium thiolate complexes and the structural characterization of two useful rhenium starting materials are presented. Pyridine-2-thiol (1) and its derivatives 3-(trimethylsilyl)-pyridine-2-thiol (2), 3,6-bis(dimethyl-tert-butylsilyl)pyridine-2-thiol (3), and pyrimidine-2-thiol (4) were reacted with [Bu4N][ReOBr4(H2O)]·2H2O (5), [Bu4N][ReOBr4(OPPh3)] (6), [ReO2(C5H5N)4], and [Re{N2CO(C6H5)}Cl2(PPh 3)2] to give [ReO(C5H4NS)3] (7), [ReO(C8H12NSiS)3] (8), [ReO(OH)(C11H20NSi2S)2] (9), [Re{N2CO(C6H5)}Cl(PPh3) 2(C5H4NS)] (10), [ReO(C4H3N2S)3] (11), and [Re{P(C6H5)3}(C4H3N 2S)3] (12). Crystal data: 5, C16H42NO4Br4Re4, tetragonal, I{\=4}, a = 8.779(2) {\AA}, b = 11.614(2) {\AA}, c = 9.397(2) {\AA}, β = 114.67(3)°, V = 870.7(4) {\AA}3, Z = 2, 422 reflections, R = 0.0457; 6, C34H51NO2PBr4Re, triclinic, P{\=1}, a = 14.437(3) {\AA}, b = 16.589(3) {\AA}, c = 16.783(3) {\AA}, α = 94.87(3)°, β= 97.62(3)°, γ = 93.80(3)°, V = 3957(2) {\AA}3, Z = 4, 6141 reflections, R = 0.0758; 7, C15H12N3OS3Re, monoclinic, P21/c, a = 11.533(2) {\AA}, b = 11.385(2) {\AA}, c = 14.039(3) {\AA}, β= 107.97(3)°, V = 1749.8(9) {\AA}3, Z = 4, 1869 reflections, R = 0.0322; 9, C34H65N2O2S2Si 4Re, triclinic, P{\=1}, a = 8.072(2) {\AA}, b = 11.409(2) {\AA}, c = 12.402(3) {\AA}, α = 79.67(3)°, β= 74.05(3)°, γ = 86.18(3)°, V = 1080.2(5) {\AA}3, Z = 1, 4630 reflections, R = 0.0525; 10, C48H39N3OSP2ClRe, triclinic, P{\=1}, a = 10.842(2) {\AA}, b = 13.660 (3) {\AA}, c = 17.665(4) {\AA}, α = 86.37(3)°, β = 89.93(3)°, γ = 77.22(3)°, V = 2080.2(10) {\AA}3, Z = 2, 4329 reflections, R = 0.0437; 11, C12H9N6OS3Re, orthorhombic, Pbca, a = 8.240(2) {\AA}, b = 13.373(3) {\AA}, C = 29.388(6) {\AA}, V = 3238.4(16) {\AA}3, Z = 8, 1400 reflections, R = 0.0512; 12, C31H26N6S3PCl2Re, triclinic, P{\=1}, a = 9.224(2) {\AA}, b = 12.050(2) {\AA}, c = 17.665(4) {\AA}, α = 89.25(3)°, β= 85.70(3)°, γ = 67.94(3)°, V = 1604.0(8) {\AA}3, Z = 2, 3592 reflections, R = 0.0697.",

author = "Rose, {David J.} and Maresca, {Kevin P.} and Kettler, {Peter B.} and {Da Chang}, Yuan and Victoria Soghomomian and Qin Chen and Abrams, {Michael J.} and Larsen, {Scott K.} and Jon Zubieta",

year = "1996",

doi = "10.1021/ic950881o",

language = "English (US)",

volume = "35",

pages = "3548--3558",

journal = "Inorganic Chemistry",

issn = "0020-1669",

publisher = "American Chemical Society",

number = "12",

}

TY - JOUR

T1 - Synthesis and Characterization of Rhenium Thiolate Complexes. Crystal and Molecular Structures of [NBu4][ReO(H2O)Br4 ]·2H2O,[Bu4N][ReOBr4(OPPh3)], [ReO(SC5H4N)3],[ReO(SC4H 3N2)3][ReO(OH)(SC5H4N-3,

AU - Rose, David J.

AU - Maresca, Kevin P.

AU - Kettler, Peter B.

AU - Da Chang, Yuan

AU - Soghomomian, Victoria

AU - Chen, Qin

AU - Abrams, Michael J.

AU - Larsen, Scott K.

AU - Zubieta, Jon

PY - 1996

Y1 - 1996

N2 - The syntheses and characterizations of six monomeric rhenium thiolate complexes and the structural characterization of two useful rhenium starting materials are presented. Pyridine-2-thiol (1) and its derivatives 3-(trimethylsilyl)-pyridine-2-thiol (2), 3,6-bis(dimethyl-tert-butylsilyl)pyridine-2-thiol (3), and pyrimidine-2-thiol (4) were reacted with [Bu4N][ReOBr4(H2O)]·2H2O (5), [Bu4N][ReOBr4(OPPh3)] (6), [ReO2(C5H5N)4], and [Re{N2CO(C6H5)}Cl2(PPh 3)2] to give [ReO(C5H4NS)3] (7), [ReO(C8H12NSiS)3] (8), [ReO(OH)(C11H20NSi2S)2] (9), [Re{N2CO(C6H5)}Cl(PPh3) 2(C5H4NS)] (10), [ReO(C4H3N2S)3] (11), and [Re{P(C6H5)3}(C4H3N 2S)3] (12). Crystal data: 5, C16H42NO4Br4Re4, tetragonal, I4̄, a = 8.779(2) Å, b = 11.614(2) Å, c = 9.397(2) Å, β = 114.67(3)°, V = 870.7(4) Å3, Z = 2, 422 reflections, R = 0.0457; 6, C34H51NO2PBr4Re, triclinic, P1̄, a = 14.437(3) Å, b = 16.589(3) Å, c = 16.783(3) Å, α = 94.87(3)°, β= 97.62(3)°, γ = 93.80(3)°, V = 3957(2) Å3, Z = 4, 6141 reflections, R = 0.0758; 7, C15H12N3OS3Re, monoclinic, P21/c, a = 11.533(2) Å, b = 11.385(2) Å, c = 14.039(3) Å, β= 107.97(3)°, V = 1749.8(9) Å3, Z = 4, 1869 reflections, R = 0.0322; 9, C34H65N2O2S2Si 4Re, triclinic, P1̄, a = 8.072(2) Å, b = 11.409(2) Å, c = 12.402(3) Å, α = 79.67(3)°, β= 74.05(3)°, γ = 86.18(3)°, V = 1080.2(5) Å3, Z = 1, 4630 reflections, R = 0.0525; 10, C48H39N3OSP2ClRe, triclinic, P1̄, a = 10.842(2) Å, b = 13.660 (3) Å, c = 17.665(4) Å, α = 86.37(3)°, β = 89.93(3)°, γ = 77.22(3)°, V = 2080.2(10) Å3, Z = 2, 4329 reflections, R = 0.0437; 11, C12H9N6OS3Re, orthorhombic, Pbca, a = 8.240(2) Å, b = 13.373(3) Å, C = 29.388(6) Å, V = 3238.4(16) Å3, Z = 8, 1400 reflections, R = 0.0512; 12, C31H26N6S3PCl2Re, triclinic, P1̄, a = 9.224(2) Å, b = 12.050(2) Å, c = 17.665(4) Å, α = 89.25(3)°, β= 85.70(3)°, γ = 67.94(3)°, V = 1604.0(8) Å3, Z = 2, 3592 reflections, R = 0.0697.

AB - The syntheses and characterizations of six monomeric rhenium thiolate complexes and the structural characterization of two useful rhenium starting materials are presented. Pyridine-2-thiol (1) and its derivatives 3-(trimethylsilyl)-pyridine-2-thiol (2), 3,6-bis(dimethyl-tert-butylsilyl)pyridine-2-thiol (3), and pyrimidine-2-thiol (4) were reacted with [Bu4N][ReOBr4(H2O)]·2H2O (5), [Bu4N][ReOBr4(OPPh3)] (6), [ReO2(C5H5N)4], and [Re{N2CO(C6H5)}Cl2(PPh 3)2] to give [ReO(C5H4NS)3] (7), [ReO(C8H12NSiS)3] (8), [ReO(OH)(C11H20NSi2S)2] (9), [Re{N2CO(C6H5)}Cl(PPh3) 2(C5H4NS)] (10), [ReO(C4H3N2S)3] (11), and [Re{P(C6H5)3}(C4H3N 2S)3] (12). Crystal data: 5, C16H42NO4Br4Re4, tetragonal, I4̄, a = 8.779(2) Å, b = 11.614(2) Å, c = 9.397(2) Å, β = 114.67(3)°, V = 870.7(4) Å3, Z = 2, 422 reflections, R = 0.0457; 6, C34H51NO2PBr4Re, triclinic, P1̄, a = 14.437(3) Å, b = 16.589(3) Å, c = 16.783(3) Å, α = 94.87(3)°, β= 97.62(3)°, γ = 93.80(3)°, V = 3957(2) Å3, Z = 4, 6141 reflections, R = 0.0758; 7, C15H12N3OS3Re, monoclinic, P21/c, a = 11.533(2) Å, b = 11.385(2) Å, c = 14.039(3) Å, β= 107.97(3)°, V = 1749.8(9) Å3, Z = 4, 1869 reflections, R = 0.0322; 9, C34H65N2O2S2Si 4Re, triclinic, P1̄, a = 8.072(2) Å, b = 11.409(2) Å, c = 12.402(3) Å, α = 79.67(3)°, β= 74.05(3)°, γ = 86.18(3)°, V = 1080.2(5) Å3, Z = 1, 4630 reflections, R = 0.0525; 10, C48H39N3OSP2ClRe, triclinic, P1̄, a = 10.842(2) Å, b = 13.660 (3) Å, c = 17.665(4) Å, α = 86.37(3)°, β = 89.93(3)°, γ = 77.22(3)°, V = 2080.2(10) Å3, Z = 2, 4329 reflections, R = 0.0437; 11, C12H9N6OS3Re, orthorhombic, Pbca, a = 8.240(2) Å, b = 13.373(3) Å, C = 29.388(6) Å, V = 3238.4(16) Å3, Z = 8, 1400 reflections, R = 0.0512; 12, C31H26N6S3PCl2Re, triclinic, P1̄, a = 9.224(2) Å, b = 12.050(2) Å, c = 17.665(4) Å, α = 89.25(3)°, β= 85.70(3)°, γ = 67.94(3)°, V = 1604.0(8) Å3, Z = 2, 3592 reflections, R = 0.0697.

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Synthesis and Characterization of Rhenium Thiolate Complexes. Crystal and Molecular Structures of [NBu₄][ReO(H₂O)Br₄ ]·2H₂O,[Bu₄N][ReOBr₄(OPPh₃)], [ReO(SC₅H₄N)₃],[ReO(SC₄H ₃N₂)₃][ReO(OH)(SC₅H₄N-3,

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