Compounds with M3Se3 (M = Li, Zn) rings: Synthesis and characterization of [Zn(CH2SiMe3)Se-2,4,6-t-Bu3C6H 2]3·0.5C6H14 and [Li(THF)Se-2,4,6-t-Bu3C6H2] 3·PhMe

Karin Ruhlandt, Philip P. Power

Research output: Contribution to journalArticle

21 Citations (Scopus)

Abstract

The synthesis and structural characterization of two six-membered ring species containing selenium are described. The compound [Zn(CH2SiMe3)SeMes*]3·0.5 C6H14 (Mes* = 2,4,6-t-Bu3C6H2), (1) was synthesized by the reaction Zn(CH2SiMe3)2 with 1 equiv of HSeMes* in hexane whereas [Li(THF)SeMes*]3·PhMe (2) was obtained by the lithiation of HSeMes* with n-BuLi in the presence of 1 equiv of THF. Each molecule has an M3Se3 core (M = Li, Zn) structure. Unlike the corresponding sulfur species, 1 has a nonplanar Zn3Se3 array and represents the first structure of this type for a selenium compound. The nonplanar Li3Se3 core in 2 involves pyramidal coordination at selenium and almost planar lithium coordination. Both species were characterized by 1H NMR and IR spectroscopy and X-ray crystallography. Crystal data with Mo Kα (λ = 0.710 69 Å) at 130 K are as follows: 1, a = 10.355(5) Å, b = 18.850(8) Å, c = 20.885(8) Å, α = 83.67(3)°, β = 86.92(4)°, γ = 77.62(4)°, V = 3956(3) Å3, Z = 2, space group P1, 7550 (I > 3σ(I)) data, R = 0.077; 2, a = 9.973(5) Å, b = 18.466(7) Å, c = 21.735(9) Å, α = 74.26(3)°, β = 79.45(4)°, γ = 78.21(2), V = 3725(3) Å3, Z = 2, space group P1, 5357 (I > 2σ(I)) data, R = 0.069.

Original languageEnglish (US)
Pages (from-to)4505-4508
Number of pages4
JournalInorganic Chemistry
Volume32
Issue number21
StatePublished - 1993
Externally publishedYes

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Selenium
selenium
selenium compounds
Selenium Compounds
rings
X ray crystallography
Hexanes
synthesis
Lithium
Sulfur
Nuclear magnetic resonance spectroscopy
crystallography
Infrared spectroscopy
sulfur
lithium
nuclear magnetic resonance
Crystals
Molecules
spectroscopy
crystals

ASJC Scopus subject areas

  • Inorganic Chemistry

Cite this

@article{309facf27b2c4aa790c80c274b2e6f26,
title = "Compounds with M3Se3 (M = Li, Zn) rings: Synthesis and characterization of [Zn(CH2SiMe3)Se-2,4,6-t-Bu3C6H 2]3·0.5C6H14 and [Li(THF)Se-2,4,6-t-Bu3C6H2] 3·PhMe",
abstract = "The synthesis and structural characterization of two six-membered ring species containing selenium are described. The compound [Zn(CH2SiMe3)SeMes*]3·0.5 C6H14 (Mes* = 2,4,6-t-Bu3C6H2), (1) was synthesized by the reaction Zn(CH2SiMe3)2 with 1 equiv of HSeMes* in hexane whereas [Li(THF)SeMes*]3·PhMe (2) was obtained by the lithiation of HSeMes* with n-BuLi in the presence of 1 equiv of THF. Each molecule has an M3Se3 core (M = Li, Zn) structure. Unlike the corresponding sulfur species, 1 has a nonplanar Zn3Se3 array and represents the first structure of this type for a selenium compound. The nonplanar Li3Se3 core in 2 involves pyramidal coordination at selenium and almost planar lithium coordination. Both species were characterized by 1H NMR and IR spectroscopy and X-ray crystallography. Crystal data with Mo Kα (λ = 0.710 69 {\AA}) at 130 K are as follows: 1, a = 10.355(5) {\AA}, b = 18.850(8) {\AA}, c = 20.885(8) {\AA}, α = 83.67(3)°, β = 86.92(4)°, γ = 77.62(4)°, V = 3956(3) {\AA}3, Z = 2, space group P1, 7550 (I > 3σ(I)) data, R = 0.077; 2, a = 9.973(5) {\AA}, b = 18.466(7) {\AA}, c = 21.735(9) {\AA}, α = 74.26(3)°, β = 79.45(4)°, γ = 78.21(2), V = 3725(3) {\AA}3, Z = 2, space group P1, 5357 (I > 2σ(I)) data, R = 0.069.",
author = "Karin Ruhlandt and Power, {Philip P.}",
year = "1993",
language = "English (US)",
volume = "32",
pages = "4505--4508",
journal = "Inorganic Chemistry",
issn = "0020-1669",
publisher = "American Chemical Society",
number = "21",

}

TY - JOUR

T1 - Compounds with M3Se3 (M = Li, Zn) rings

T2 - Synthesis and characterization of [Zn(CH2SiMe3)Se-2,4,6-t-Bu3C6H 2]3·0.5C6H14 and [Li(THF)Se-2,4,6-t-Bu3C6H2] 3·PhMe

AU - Ruhlandt, Karin

AU - Power, Philip P.

PY - 1993

Y1 - 1993

N2 - The synthesis and structural characterization of two six-membered ring species containing selenium are described. The compound [Zn(CH2SiMe3)SeMes*]3·0.5 C6H14 (Mes* = 2,4,6-t-Bu3C6H2), (1) was synthesized by the reaction Zn(CH2SiMe3)2 with 1 equiv of HSeMes* in hexane whereas [Li(THF)SeMes*]3·PhMe (2) was obtained by the lithiation of HSeMes* with n-BuLi in the presence of 1 equiv of THF. Each molecule has an M3Se3 core (M = Li, Zn) structure. Unlike the corresponding sulfur species, 1 has a nonplanar Zn3Se3 array and represents the first structure of this type for a selenium compound. The nonplanar Li3Se3 core in 2 involves pyramidal coordination at selenium and almost planar lithium coordination. Both species were characterized by 1H NMR and IR spectroscopy and X-ray crystallography. Crystal data with Mo Kα (λ = 0.710 69 Å) at 130 K are as follows: 1, a = 10.355(5) Å, b = 18.850(8) Å, c = 20.885(8) Å, α = 83.67(3)°, β = 86.92(4)°, γ = 77.62(4)°, V = 3956(3) Å3, Z = 2, space group P1, 7550 (I > 3σ(I)) data, R = 0.077; 2, a = 9.973(5) Å, b = 18.466(7) Å, c = 21.735(9) Å, α = 74.26(3)°, β = 79.45(4)°, γ = 78.21(2), V = 3725(3) Å3, Z = 2, space group P1, 5357 (I > 2σ(I)) data, R = 0.069.

AB - The synthesis and structural characterization of two six-membered ring species containing selenium are described. The compound [Zn(CH2SiMe3)SeMes*]3·0.5 C6H14 (Mes* = 2,4,6-t-Bu3C6H2), (1) was synthesized by the reaction Zn(CH2SiMe3)2 with 1 equiv of HSeMes* in hexane whereas [Li(THF)SeMes*]3·PhMe (2) was obtained by the lithiation of HSeMes* with n-BuLi in the presence of 1 equiv of THF. Each molecule has an M3Se3 core (M = Li, Zn) structure. Unlike the corresponding sulfur species, 1 has a nonplanar Zn3Se3 array and represents the first structure of this type for a selenium compound. The nonplanar Li3Se3 core in 2 involves pyramidal coordination at selenium and almost planar lithium coordination. Both species were characterized by 1H NMR and IR spectroscopy and X-ray crystallography. Crystal data with Mo Kα (λ = 0.710 69 Å) at 130 K are as follows: 1, a = 10.355(5) Å, b = 18.850(8) Å, c = 20.885(8) Å, α = 83.67(3)°, β = 86.92(4)°, γ = 77.62(4)°, V = 3956(3) Å3, Z = 2, space group P1, 7550 (I > 3σ(I)) data, R = 0.077; 2, a = 9.973(5) Å, b = 18.466(7) Å, c = 21.735(9) Å, α = 74.26(3)°, β = 79.45(4)°, γ = 78.21(2), V = 3725(3) Å3, Z = 2, space group P1, 5357 (I > 2σ(I)) data, R = 0.069.

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