Syntheses and X-ray crystal structures of zinc complexes with an amido-diamine ligand

Bing Luo; Benjamin E. Kucera; Wayne L. Gladfelter

doi:10.1016/j.poly.2005.06.041

Syntheses and X-ray crystal structures of zinc complexes with an amido-diamine ligand

Bing Luo, Benjamin E. Kucera, Wayne L. Gladfelter

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Abstract

The synthesis and characterization of complexes with a tridentate amido-diamine ligand -N(CH₂CH₂NMe₂) ₂, [ClZnN(CH₂CH₂NMe₂) ₂]₂ (1), [EtZnN(CH₂CH₂NMe ₂)₂]₂ (2), {Zn[N(CH₂CH ₂NMe₂)₂]₂}₂ (3) and [ⁱBu₂NZnN(CH₂CH₂NMe ₂)₂]₂ (4), are described. Compounds 1 (57% yield) and 2 (49% yield) were obtained from the reactions of ZnCl₂ with 1 equiv. of LiN(CH₂CH₂NMe₂)₂ and ZnEt₂ with excess HN(CH₂CH₂NMe ₂)₂, respectively. Compounds 3 (52% yield) and 4 (75% yield) were isolated from the reactions of [Zn(NⁱBu₂) ₂]₂ with HN(CH₂CH₂NMe ₂)₂ in 1:4 and 1:2 molar ratios, respectively. Mass spectral data and NMR analyses suggested that all four compounds were dimeric. The solid-state structures of compounds 2 and 3 were determined via X-ray crystallography. Both compounds were centrosymmetric containing a four-membered Zn₂N₂ ring with bridging amido ligands. In both structures, one NMe₂ group in each bridging ligand bonded to a Zn center forming a five-membered ring. The ethyl groups in 2 and the second -N(CH₂CH₂NMe₂)₂ ligand in 3 occupied the terminal positions.

Original language	English (US)
Pages (from-to)	279-285
Number of pages	7
Journal	Polyhedron
Volume	25
Issue number	2
DOIs	https://doi.org/10.1016/j.poly.2005.06.041
State	Published - Jan 23 2006

Bibliographical note

Funding Information:
We thank the National Science Foundation for the financial support through a Grant CHE-03159540.

Keywords

Amide
Amido
Dimer
Structure
Tridentate
Zinc

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title = "Syntheses and X-ray crystal structures of zinc complexes with an amido-diamine ligand",

abstract = "The synthesis and characterization of complexes with a tridentate amido-diamine ligand -N(CH2CH2NMe2) 2, [ClZnN(CH2CH2NMe2) 2]2 (1), [EtZnN(CH2CH2NMe 2)2]2 (2), {Zn[N(CH2CH 2NMe2)2]2}2 (3) and [iBu2NZnN(CH2CH2NMe 2)2]2 (4), are described. Compounds 1 (57% yield) and 2 (49% yield) were obtained from the reactions of ZnCl2 with 1 equiv. of LiN(CH2CH2NMe2)2 and ZnEt2 with excess HN(CH2CH2NMe 2)2, respectively. Compounds 3 (52% yield) and 4 (75% yield) were isolated from the reactions of [Zn(NiBu2) 2]2 with HN(CH2CH2NMe 2)2 in 1:4 and 1:2 molar ratios, respectively. Mass spectral data and NMR analyses suggested that all four compounds were dimeric. The solid-state structures of compounds 2 and 3 were determined via X-ray crystallography. Both compounds were centrosymmetric containing a four-membered Zn2N2 ring with bridging amido ligands. In both structures, one NMe2 group in each bridging ligand bonded to a Zn center forming a five-membered ring. The ethyl groups in 2 and the second -N(CH2CH2NMe2)2 ligand in 3 occupied the terminal positions.",

keywords = "Amide, Amido, Dimer, Structure, Tridentate, Zinc",

author = "Bing Luo and Kucera, {Benjamin E.} and Gladfelter, {Wayne L.}",

note = "Funding Information: We thank the National Science Foundation for the financial support through a Grant CHE-03159540. ",

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doi = "10.1016/j.poly.2005.06.041",

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T1 - Syntheses and X-ray crystal structures of zinc complexes with an amido-diamine ligand

AU - Luo, Bing

AU - Kucera, Benjamin E.

AU - Gladfelter, Wayne L.

N1 - Funding Information: We thank the National Science Foundation for the financial support through a Grant CHE-03159540.

PY - 2006/1/23

Y1 - 2006/1/23

N2 - The synthesis and characterization of complexes with a tridentate amido-diamine ligand -N(CH2CH2NMe2) 2, [ClZnN(CH2CH2NMe2) 2]2 (1), [EtZnN(CH2CH2NMe 2)2]2 (2), {Zn[N(CH2CH 2NMe2)2]2}2 (3) and [iBu2NZnN(CH2CH2NMe 2)2]2 (4), are described. Compounds 1 (57% yield) and 2 (49% yield) were obtained from the reactions of ZnCl2 with 1 equiv. of LiN(CH2CH2NMe2)2 and ZnEt2 with excess HN(CH2CH2NMe 2)2, respectively. Compounds 3 (52% yield) and 4 (75% yield) were isolated from the reactions of [Zn(NiBu2) 2]2 with HN(CH2CH2NMe 2)2 in 1:4 and 1:2 molar ratios, respectively. Mass spectral data and NMR analyses suggested that all four compounds were dimeric. The solid-state structures of compounds 2 and 3 were determined via X-ray crystallography. Both compounds were centrosymmetric containing a four-membered Zn2N2 ring with bridging amido ligands. In both structures, one NMe2 group in each bridging ligand bonded to a Zn center forming a five-membered ring. The ethyl groups in 2 and the second -N(CH2CH2NMe2)2 ligand in 3 occupied the terminal positions.

AB - The synthesis and characterization of complexes with a tridentate amido-diamine ligand -N(CH2CH2NMe2) 2, [ClZnN(CH2CH2NMe2) 2]2 (1), [EtZnN(CH2CH2NMe 2)2]2 (2), {Zn[N(CH2CH 2NMe2)2]2}2 (3) and [iBu2NZnN(CH2CH2NMe 2)2]2 (4), are described. Compounds 1 (57% yield) and 2 (49% yield) were obtained from the reactions of ZnCl2 with 1 equiv. of LiN(CH2CH2NMe2)2 and ZnEt2 with excess HN(CH2CH2NMe 2)2, respectively. Compounds 3 (52% yield) and 4 (75% yield) were isolated from the reactions of [Zn(NiBu2) 2]2 with HN(CH2CH2NMe 2)2 in 1:4 and 1:2 molar ratios, respectively. Mass spectral data and NMR analyses suggested that all four compounds were dimeric. The solid-state structures of compounds 2 and 3 were determined via X-ray crystallography. Both compounds were centrosymmetric containing a four-membered Zn2N2 ring with bridging amido ligands. In both structures, one NMe2 group in each bridging ligand bonded to a Zn center forming a five-membered ring. The ethyl groups in 2 and the second -N(CH2CH2NMe2)2 ligand in 3 occupied the terminal positions.

KW - Amide

KW - Amido

KW - Dimer

KW - Structure

KW - Tridentate

KW - Zinc

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VL - 25

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EP - 285

JO - Polyhedron

JF - Polyhedron

IS - 2

ER -

Syntheses and X-ray crystal structures of zinc complexes with an amido-diamine ligand

Abstract

Bibliographical note

Keywords

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