Synthesis and characterization of the strontium thiolate Sr(SMes*)2(THF)4·2THF (Mes* = 2,4,6-tBu3C6H2) and selenolate Sr(SeMes*)2(THF)4·2THF. Structural investigation of SrI2(THF)5

Karin Ruhlandt, Kelly Davis, Sona Dalal, Ulrich Englich, Mathias O. Senge

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Abstract

The syntheses and structural characterization of the strontium thiolate Sr(SMes*)2(THF)4·2THF, 1 (Mes* = 2,4,6-tBu3C6H2), and selenolate Sr(SeMes*)2(THF)4·2THF, 2, are described. We also report the synthesis and structural characterization of SrI2(THF)5, 3, the apparent starting material for the synthesis of 1 and 2. 3 exhibits pentagonal bipyramidal geometry at the strontium atom. 3 can be prepared by dissolving SrI2 in THF, while the treatment of 3 with 2 equiv of the sterically demanding potassium thiolate and selenolate in THF affords 1 and 2 in good yields. 1 and 2 exhibit distorted octahedral environments at the metal center, with the degree of distortion much more significant for the thiolato derivative. 1 and 2 were characterized by 1H NMR and IR spectroscopy, elemental analysis, and X-ray crystallography; 3 was characterized by single-crystal structure analysis. Crystal data with Mo Kα (λ = 0.710 73 (Å) at 213 K are as follows. 1: a = 18.535(4) Å, b = 19.222(4) Å, c = 18.775(4) Å, β = 107.30(3)°, V = 6387(2) Å3, Z = 4, monoclinic, space group I2/a, 2254 (I > 3σ(I)) data, R = 0.071. 2: a = 18.330(4) Å, b = 19.498(4) Å, c = 18.608(4) Å, β = 105.52(3)°, V = 6408(3) Å3, Z = 4, monoclinic, space group I2/a, 2331 (I > 3σ(I)) data, R = 0.057. 3: a = 8.851(1) Å, c = 35.353(7) Å, V = 2770(1) Å3, Z = 4, tetragonal, space group P43212, 939 (I > 3σ(I)) data, R = 0.069.

Original languageEnglish (US)
Pages (from-to)2587-2592
Number of pages6
JournalInorganic Chemistry
Volume34
Issue number10
StatePublished - 1995

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Strontium
strontium
synthesis
X ray crystallography
Nuclear magnetic resonance spectroscopy
crystallography
Infrared spectroscopy
potassium
Potassium
dissolving
Crystal structure
Metals
Single crystals
Derivatives
Atoms
nuclear magnetic resonance
Crystals
crystal structure
Geometry
single crystals

ASJC Scopus subject areas

  • Inorganic Chemistry

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@article{5aa2701bf4514b2d9111385b2e3a4bd9,
title = "Synthesis and characterization of the strontium thiolate Sr(SMes*)2(THF)4·2THF (Mes* = 2,4,6-tBu3C6H2) and selenolate Sr(SeMes*)2(THF)4·2THF. Structural investigation of SrI2(THF)5",
abstract = "The syntheses and structural characterization of the strontium thiolate Sr(SMes*)2(THF)4·2THF, 1 (Mes* = 2,4,6-tBu3C6H2), and selenolate Sr(SeMes*)2(THF)4·2THF, 2, are described. We also report the synthesis and structural characterization of SrI2(THF)5, 3, the apparent starting material for the synthesis of 1 and 2. 3 exhibits pentagonal bipyramidal geometry at the strontium atom. 3 can be prepared by dissolving SrI2 in THF, while the treatment of 3 with 2 equiv of the sterically demanding potassium thiolate and selenolate in THF affords 1 and 2 in good yields. 1 and 2 exhibit distorted octahedral environments at the metal center, with the degree of distortion much more significant for the thiolato derivative. 1 and 2 were characterized by 1H NMR and IR spectroscopy, elemental analysis, and X-ray crystallography; 3 was characterized by single-crystal structure analysis. Crystal data with Mo Kα (λ = 0.710 73 ({\AA}) at 213 K are as follows. 1: a = 18.535(4) {\AA}, b = 19.222(4) {\AA}, c = 18.775(4) {\AA}, β = 107.30(3)°, V = 6387(2) {\AA}3, Z = 4, monoclinic, space group I2/a, 2254 (I > 3σ(I)) data, R = 0.071. 2: a = 18.330(4) {\AA}, b = 19.498(4) {\AA}, c = 18.608(4) {\AA}, β = 105.52(3)°, V = 6408(3) {\AA}3, Z = 4, monoclinic, space group I2/a, 2331 (I > 3σ(I)) data, R = 0.057. 3: a = 8.851(1) {\AA}, c = 35.353(7) {\AA}, V = 2770(1) {\AA}3, Z = 4, tetragonal, space group P43212, 939 (I > 3σ(I)) data, R = 0.069.",
author = "Karin Ruhlandt and Kelly Davis and Sona Dalal and Ulrich Englich and Senge, {Mathias O.}",
year = "1995",
language = "English (US)",
volume = "34",
pages = "2587--2592",
journal = "Inorganic Chemistry",
issn = "0020-1669",
publisher = "American Chemical Society",
number = "10",

}

TY - JOUR

T1 - Synthesis and characterization of the strontium thiolate Sr(SMes*)2(THF)4·2THF (Mes* = 2,4,6-tBu3C6H2) and selenolate Sr(SeMes*)2(THF)4·2THF. Structural investigation of SrI2(THF)5

AU - Ruhlandt, Karin

AU - Davis, Kelly

AU - Dalal, Sona

AU - Englich, Ulrich

AU - Senge, Mathias O.

PY - 1995

Y1 - 1995

N2 - The syntheses and structural characterization of the strontium thiolate Sr(SMes*)2(THF)4·2THF, 1 (Mes* = 2,4,6-tBu3C6H2), and selenolate Sr(SeMes*)2(THF)4·2THF, 2, are described. We also report the synthesis and structural characterization of SrI2(THF)5, 3, the apparent starting material for the synthesis of 1 and 2. 3 exhibits pentagonal bipyramidal geometry at the strontium atom. 3 can be prepared by dissolving SrI2 in THF, while the treatment of 3 with 2 equiv of the sterically demanding potassium thiolate and selenolate in THF affords 1 and 2 in good yields. 1 and 2 exhibit distorted octahedral environments at the metal center, with the degree of distortion much more significant for the thiolato derivative. 1 and 2 were characterized by 1H NMR and IR spectroscopy, elemental analysis, and X-ray crystallography; 3 was characterized by single-crystal structure analysis. Crystal data with Mo Kα (λ = 0.710 73 (Å) at 213 K are as follows. 1: a = 18.535(4) Å, b = 19.222(4) Å, c = 18.775(4) Å, β = 107.30(3)°, V = 6387(2) Å3, Z = 4, monoclinic, space group I2/a, 2254 (I > 3σ(I)) data, R = 0.071. 2: a = 18.330(4) Å, b = 19.498(4) Å, c = 18.608(4) Å, β = 105.52(3)°, V = 6408(3) Å3, Z = 4, monoclinic, space group I2/a, 2331 (I > 3σ(I)) data, R = 0.057. 3: a = 8.851(1) Å, c = 35.353(7) Å, V = 2770(1) Å3, Z = 4, tetragonal, space group P43212, 939 (I > 3σ(I)) data, R = 0.069.

AB - The syntheses and structural characterization of the strontium thiolate Sr(SMes*)2(THF)4·2THF, 1 (Mes* = 2,4,6-tBu3C6H2), and selenolate Sr(SeMes*)2(THF)4·2THF, 2, are described. We also report the synthesis and structural characterization of SrI2(THF)5, 3, the apparent starting material for the synthesis of 1 and 2. 3 exhibits pentagonal bipyramidal geometry at the strontium atom. 3 can be prepared by dissolving SrI2 in THF, while the treatment of 3 with 2 equiv of the sterically demanding potassium thiolate and selenolate in THF affords 1 and 2 in good yields. 1 and 2 exhibit distorted octahedral environments at the metal center, with the degree of distortion much more significant for the thiolato derivative. 1 and 2 were characterized by 1H NMR and IR spectroscopy, elemental analysis, and X-ray crystallography; 3 was characterized by single-crystal structure analysis. Crystal data with Mo Kα (λ = 0.710 73 (Å) at 213 K are as follows. 1: a = 18.535(4) Å, b = 19.222(4) Å, c = 18.775(4) Å, β = 107.30(3)°, V = 6387(2) Å3, Z = 4, monoclinic, space group I2/a, 2254 (I > 3σ(I)) data, R = 0.071. 2: a = 18.330(4) Å, b = 19.498(4) Å, c = 18.608(4) Å, β = 105.52(3)°, V = 6408(3) Å3, Z = 4, monoclinic, space group I2/a, 2331 (I > 3σ(I)) data, R = 0.057. 3: a = 8.851(1) Å, c = 35.353(7) Å, V = 2770(1) Å3, Z = 4, tetragonal, space group P43212, 939 (I > 3σ(I)) data, R = 0.069.

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