Synthesis and Characterization of Unusual Dichloro(amido)-Bridged Zirconium Complexes. X-ray Crystal Structures of (Me2N)3Zr(μ-Cl)2(μ-NMe 2)Zr(NMe2)2(THF) and Cl(Me2N)2Zr(μ-Cl)2(μ-NMe 2)Zr(NMe2)2(THF)

Zhongzhi Wu, Jonathan B. Diminnie, Ziling Xue

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Abstract

Reactions of 3 and 2 equiv of lithium dimethylamide with ZrCl4 in THF afford dinuclear complexes (Me2N)3-Zr(μ-Cl)2(μ-NMe 2)Zr(NMe2)2(THF) (1) and Cl(Me2N)2Zr(μ-Cl)2(μ-NMe 2)Zr(NMe2)2(THF) (2), respectively. These complexes were found to have unusual structures containing dichloro(amido) bridges between Zr atoms. Both complexes 1 and 2 crystallize in the monoclinic space group P21/c (a = 8.735(3) Å, b = 21.498(7) Å, c = 13.997(5) Å, β= 92.56(3)°, Z = 4 for 1; a = 8.550(3) Å, b = 20.673(7) Å, c = 14.229(6) Å, β = 95.11(3)°, Z = 4 for 2). Each Zr atom in 1 and 2 has a trigonal antiprismatic coordination geometry. Reaction of 1 equiv of lithium dimethylamide with ZrCl4 in THF gave the monosubstituted complex as the LiCl adduct (Me2N)(THF)ZrCl2(μ-Cl)2Li(THF)2 (4), which crystallizes in the triclinic space group P1 (a = 10.078(6) Å, b = 11.003(7) Å, c = 11.039(6) Å, α = 84.75(5)°, β= 78.38(5)°. γ = 66.65(5)°. Ζ= 2). In 4, the Zr atom has a distorted octahedral coordination geometry. These new amido complexes add to the missing members of the Zr(NMe2)xCl4-x series. The dynamic NMR of 1 has also been studied.

Original languageEnglish (US)
Pages (from-to)2570-2574
Number of pages5
JournalInorganic Chemistry
Volume37
Issue number10
StatePublished - May 18 1998

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Crystal structure
Lithium
X rays
Atoms
crystal structure
synthesis
lithium
atoms
x rays
Geometry
geometry
adducts
Nuclear magnetic resonance
nuclear magnetic resonance
zirconium chloride

All Science Journal Classification (ASJC) codes

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry

Cite this

@article{8dfeb13fa7a14354a32079e01f4d7e43,
title = "Synthesis and Characterization of Unusual Dichloro(amido)-Bridged Zirconium Complexes. X-ray Crystal Structures of (Me2N)3Zr(μ-Cl)2(μ-NMe 2)Zr(NMe2)2(THF) and Cl(Me2N)2Zr(μ-Cl)2(μ-NMe 2)Zr(NMe2)2(THF)",
abstract = "Reactions of 3 and 2 equiv of lithium dimethylamide with ZrCl4 in THF afford dinuclear complexes (Me2N)3-Zr(μ-Cl)2(μ-NMe 2)Zr(NMe2)2(THF) (1) and Cl(Me2N)2Zr(μ-Cl)2(μ-NMe 2)Zr(NMe2)2(THF) (2), respectively. These complexes were found to have unusual structures containing dichloro(amido) bridges between Zr atoms. Both complexes 1 and 2 crystallize in the monoclinic space group P21/c (a = 8.735(3) {\AA}, b = 21.498(7) {\AA}, c = 13.997(5) {\AA}, β= 92.56(3)°, Z = 4 for 1; a = 8.550(3) {\AA}, b = 20.673(7) {\AA}, c = 14.229(6) {\AA}, β = 95.11(3)°, Z = 4 for 2). Each Zr atom in 1 and 2 has a trigonal antiprismatic coordination geometry. Reaction of 1 equiv of lithium dimethylamide with ZrCl4 in THF gave the monosubstituted complex as the LiCl adduct (Me2N)(THF)ZrCl2(μ-Cl)2Li(THF)2 (4), which crystallizes in the triclinic space group P1 (a = 10.078(6) {\AA}, b = 11.003(7) {\AA}, c = 11.039(6) {\AA}, α = 84.75(5)°, β= 78.38(5)°. γ = 66.65(5)°. Ζ= 2). In 4, the Zr atom has a distorted octahedral coordination geometry. These new amido complexes add to the missing members of the Zr(NMe2)xCl4-x series. The dynamic NMR of 1 has also been studied.",
author = "Zhongzhi Wu and Diminnie, {Jonathan B.} and Ziling Xue",
year = "1998",
month = "5",
day = "18",
language = "English (US)",
volume = "37",
pages = "2570--2574",
journal = "Inorganic Chemistry",
issn = "0020-1669",
publisher = "American Chemical Society",
number = "10",

}

TY - JOUR

T1 - Synthesis and Characterization of Unusual Dichloro(amido)-Bridged Zirconium Complexes. X-ray Crystal Structures of (Me2N)3Zr(μ-Cl)2(μ-NMe 2)Zr(NMe2)2(THF) and Cl(Me2N)2Zr(μ-Cl)2(μ-NMe 2)Zr(NMe2)2(THF)

AU - Wu, Zhongzhi

AU - Diminnie, Jonathan B.

AU - Xue, Ziling

PY - 1998/5/18

Y1 - 1998/5/18

N2 - Reactions of 3 and 2 equiv of lithium dimethylamide with ZrCl4 in THF afford dinuclear complexes (Me2N)3-Zr(μ-Cl)2(μ-NMe 2)Zr(NMe2)2(THF) (1) and Cl(Me2N)2Zr(μ-Cl)2(μ-NMe 2)Zr(NMe2)2(THF) (2), respectively. These complexes were found to have unusual structures containing dichloro(amido) bridges between Zr atoms. Both complexes 1 and 2 crystallize in the monoclinic space group P21/c (a = 8.735(3) Å, b = 21.498(7) Å, c = 13.997(5) Å, β= 92.56(3)°, Z = 4 for 1; a = 8.550(3) Å, b = 20.673(7) Å, c = 14.229(6) Å, β = 95.11(3)°, Z = 4 for 2). Each Zr atom in 1 and 2 has a trigonal antiprismatic coordination geometry. Reaction of 1 equiv of lithium dimethylamide with ZrCl4 in THF gave the monosubstituted complex as the LiCl adduct (Me2N)(THF)ZrCl2(μ-Cl)2Li(THF)2 (4), which crystallizes in the triclinic space group P1 (a = 10.078(6) Å, b = 11.003(7) Å, c = 11.039(6) Å, α = 84.75(5)°, β= 78.38(5)°. γ = 66.65(5)°. Ζ= 2). In 4, the Zr atom has a distorted octahedral coordination geometry. These new amido complexes add to the missing members of the Zr(NMe2)xCl4-x series. The dynamic NMR of 1 has also been studied.

AB - Reactions of 3 and 2 equiv of lithium dimethylamide with ZrCl4 in THF afford dinuclear complexes (Me2N)3-Zr(μ-Cl)2(μ-NMe 2)Zr(NMe2)2(THF) (1) and Cl(Me2N)2Zr(μ-Cl)2(μ-NMe 2)Zr(NMe2)2(THF) (2), respectively. These complexes were found to have unusual structures containing dichloro(amido) bridges between Zr atoms. Both complexes 1 and 2 crystallize in the monoclinic space group P21/c (a = 8.735(3) Å, b = 21.498(7) Å, c = 13.997(5) Å, β= 92.56(3)°, Z = 4 for 1; a = 8.550(3) Å, b = 20.673(7) Å, c = 14.229(6) Å, β = 95.11(3)°, Z = 4 for 2). Each Zr atom in 1 and 2 has a trigonal antiprismatic coordination geometry. Reaction of 1 equiv of lithium dimethylamide with ZrCl4 in THF gave the monosubstituted complex as the LiCl adduct (Me2N)(THF)ZrCl2(μ-Cl)2Li(THF)2 (4), which crystallizes in the triclinic space group P1 (a = 10.078(6) Å, b = 11.003(7) Å, c = 11.039(6) Å, α = 84.75(5)°, β= 78.38(5)°. γ = 66.65(5)°. Ζ= 2). In 4, the Zr atom has a distorted octahedral coordination geometry. These new amido complexes add to the missing members of the Zr(NMe2)xCl4-x series. The dynamic NMR of 1 has also been studied.

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M3 - Article

VL - 37

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