Synthesis and structural characterization of complexes of the {Cp * Rh} and {MeRe} cores with pyridine-2-thiol ligand types.

Peter B. Kettler; Yuanda Chang; David Rose; Jon Zubieta; Michael J. Abrams

doi:10.1016/0020-1693(95)04785-9

Synthesis and structural characterization of complexes of the {Cp * Rh} and {MeRe} cores with pyridine-2-thiol ligand types.

Peter B. Kettler, Yuanda Chang, David Rose, Jon Zubieta, Michael J. Abrams

Department of Chemistry

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

12 Scopus citations

Abstract

Complexes of trimethylsilyl substituted pyridine-2-thiol with rhenium and rhodium have been prepared and structurally characterized. The reaction of methyltrioxorhenium with 3-trimethylsilylpyridine-2-thiol in toluene at 0 °C affords dark green plates of MeReO( η²-2-SC₅H₃N-3-SiMe₃)₂ (4). The reaction of [Cp *RhCl₂]₂ with 3-trimethylsilylpyridine-2-thiol in THF, followed by extraction in hexanes and recrystallization yields Cp *Rh( η²-2-SC₅H₃N-3-SiMe₃)( η¹-2-SC₅H₃N-3-SiMe₃) (5). Crystal data: 4: monoclinic, P2₁/c, a= 12.898(3), b =13.660(3), c = 13.192(3) Å, β = 97.58(1)°, V = 2303(1) Å³, Z = 4, D_calc= 1.010 g cm^-3; structure solution and refinement based on 2297 reflections converged at a conventional residual of 0.0465. 5: orthorhombic, Pna2₁, a = 8.579(2), 6 = 23.315(5), c = 15.341 (3) Å, V = 3068(2) Å³, Z = 4, D_calc = 1.305 g cm^-3; 1455 reflections, R = 0.0572.

Original language	English (US)
Pages (from-to)	199-205
Number of pages	7
Journal	Inorganica Chimica Acta
Volume	244
Issue number	2
DOIs	https://doi.org/10.1016/0020-1693(95)04785-9
State	Published - Mar 15 1996

Keywords

Crystal structures
Rhenium complexes
Rhodium complexes
Thiol complexes

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

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10.1016/0020-1693(95)04785-9

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@article{36d61683183349c68db1b9b2403a2d3d,

title = "Synthesis and structural characterization of complexes of the {Cp * Rh} and {MeRe} cores with pyridine-2-thiol ligand types.",

abstract = "Complexes of trimethylsilyl substituted pyridine-2-thiol with rhenium and rhodium have been prepared and structurally characterized. The reaction of methyltrioxorhenium with 3-trimethylsilylpyridine-2-thiol in toluene at 0 °C affords dark green plates of MeReO( η2-2-SC5H3N-3-SiMe3)2 (4). The reaction of [Cp *RhCl2]2 with 3-trimethylsilylpyridine-2-thiol in THF, followed by extraction in hexanes and recrystallization yields Cp *Rh( η2-2-SC5H3N-3-SiMe3)( η1-2-SC5H3N-3-SiMe3) (5). Crystal data: 4: monoclinic, P21/c, a= 12.898(3), b =13.660(3), c = 13.192(3) {\AA}, β = 97.58(1)°, V = 2303(1) {\AA}3, Z = 4, Dcalc= 1.010 g cm-3; structure solution and refinement based on 2297 reflections converged at a conventional residual of 0.0465. 5: orthorhombic, Pna21, a = 8.579(2), 6 = 23.315(5), c = 15.341 (3) {\AA}, V = 3068(2) {\AA}3, Z = 4, Dcalc = 1.305 g cm-3; 1455 reflections, R = 0.0572.",

keywords = "Crystal structures, Rhenium complexes, Rhodium complexes, Thiol complexes",

author = "Kettler, {Peter B.} and Yuanda Chang and David Rose and Jon Zubieta and Abrams, {Michael J.}",

year = "1996",

month = mar,

day = "15",

doi = "10.1016/0020-1693(95)04785-9",

language = "English (US)",

volume = "244",

pages = "199--205",

journal = "Inorganica Chimica Acta",

issn = "0020-1693",

publisher = "Elsevier",

number = "2",

}

TY - JOUR

T1 - Synthesis and structural characterization of complexes of the {Cp * Rh} and {MeRe} cores with pyridine-2-thiol ligand types.

AU - Kettler, Peter B.

AU - Chang, Yuanda

AU - Rose, David

AU - Zubieta, Jon

AU - Abrams, Michael J.

PY - 1996/3/15

Y1 - 1996/3/15

N2 - Complexes of trimethylsilyl substituted pyridine-2-thiol with rhenium and rhodium have been prepared and structurally characterized. The reaction of methyltrioxorhenium with 3-trimethylsilylpyridine-2-thiol in toluene at 0 °C affords dark green plates of MeReO( η2-2-SC5H3N-3-SiMe3)2 (4). The reaction of [Cp *RhCl2]2 with 3-trimethylsilylpyridine-2-thiol in THF, followed by extraction in hexanes and recrystallization yields Cp *Rh( η2-2-SC5H3N-3-SiMe3)( η1-2-SC5H3N-3-SiMe3) (5). Crystal data: 4: monoclinic, P21/c, a= 12.898(3), b =13.660(3), c = 13.192(3) Å, β = 97.58(1)°, V = 2303(1) Å3, Z = 4, Dcalc= 1.010 g cm-3; structure solution and refinement based on 2297 reflections converged at a conventional residual of 0.0465. 5: orthorhombic, Pna21, a = 8.579(2), 6 = 23.315(5), c = 15.341 (3) Å, V = 3068(2) Å3, Z = 4, Dcalc = 1.305 g cm-3; 1455 reflections, R = 0.0572.

AB - Complexes of trimethylsilyl substituted pyridine-2-thiol with rhenium and rhodium have been prepared and structurally characterized. The reaction of methyltrioxorhenium with 3-trimethylsilylpyridine-2-thiol in toluene at 0 °C affords dark green plates of MeReO( η2-2-SC5H3N-3-SiMe3)2 (4). The reaction of [Cp *RhCl2]2 with 3-trimethylsilylpyridine-2-thiol in THF, followed by extraction in hexanes and recrystallization yields Cp *Rh( η2-2-SC5H3N-3-SiMe3)( η1-2-SC5H3N-3-SiMe3) (5). Crystal data: 4: monoclinic, P21/c, a= 12.898(3), b =13.660(3), c = 13.192(3) Å, β = 97.58(1)°, V = 2303(1) Å3, Z = 4, Dcalc= 1.010 g cm-3; structure solution and refinement based on 2297 reflections converged at a conventional residual of 0.0465. 5: orthorhombic, Pna21, a = 8.579(2), 6 = 23.315(5), c = 15.341 (3) Å, V = 3068(2) Å3, Z = 4, Dcalc = 1.305 g cm-3; 1455 reflections, R = 0.0572.

KW - Crystal structures

KW - Rhenium complexes

KW - Rhodium complexes

KW - Thiol complexes

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U2 - 10.1016/0020-1693(95)04785-9

DO - 10.1016/0020-1693(95)04785-9

M3 - Article

AN - SCOPUS:0001005343

SN - 0020-1693

VL - 244

SP - 199

EP - 205

JO - Inorganica Chimica Acta

JF - Inorganica Chimica Acta

IS - 2

ER -

Synthesis and structural characterization of complexes of the {Cp * Rh} and {MeRe} cores with pyridine-2-thiol ligand types.

Abstract

Keywords

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