Exploring the solid state and solution structural chemistry of the utility amide potassium hexamethyldisilazide (KHMDS)

Ana I. Ojeda-Amador; Antonio J. Martínez-Martínez; Gemma M. Robertson; Stuart D. Robertson; Alan R. Kennedy; Charles T. O'Hara

doi:10.1039/C7DT01118K

Exploring the solid state and solution structural chemistry of the utility amide potassium hexamethyldisilazide (KHMDS)

Ana I. Ojeda-Amador, Antonio J. Martínez-Martínez, Gemma M. Robertson, Stuart D. Robertson, Alan R. Kennedy, Charles T. O'Hara

Pure And Applied Chemistry

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

10 Citations (Scopus)

54 Downloads (Pure)

Abstract

The structural chemistry of eleven donor complexes of the important Brønsted base potassium 1,1,1,3,3,3-hexamethyldisilazide (KHMDS) has been studied. Depending on the donor, each complex adopted one of four general structural motifs. Specifically, in this study the donors employed were toluene (to give polymeric 1 and dimeric 2), THF (dimeric 3), N,N,N',N'-tetramethylethylenediamine (TMEDA) (dimeric 4), (R,R)-N,N,N',N'-tetramethyl-1,2-diaminocyclohexane [(R,R)-TMCDA] (dimeric 5), 12-crown-4 (dimeric 6), N,N,N',N'-tetramethyldiaminoethyl ether (TMDAE) (tetranuclear dimeric 8 and monomeric 10), N,N,N',N',N''-pentamethyldiethylentriamine (PMDETA) (tetranuclear dimeric 7), tris[2-dimethyl(amino)ethyl]amine (Me₆TREN) (tetranuclear dimeric 9) and tris{2-(2-methoxyethoxy)ethyl}amine (TMEEA) (monomeric 11). The complexes were also studied in solution by ¹H and ¹³C NMR spectroscopy as well as DOSY NMR spectroscopy.

Original language	English
Pages (from-to)	6392-6403
Number of pages	12
Journal	Dalton Transactions
Volume	46
Issue number	19
Early online date	3 May 2017
DOIs	https://doi.org/10.1039/C7DT01118K
Publication status	Published - 15 May 2017

Keywords

structural chemistry
Brønsted base potassium
structural motifs
spectroscopic analysis

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http://pubs.rsc.org/en/Journals/JournalIssues/DT

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Lithium Cuprates to Copper Lithiates: A New Dawn in Metal Catalysed Chemistry
O'Hara, C.
EPSRC (Engineering and Physical Sciences Research Council)
1/07/13 → 30/06/15
Project: Research
Chiral Concepts in s-Block Metal Amide Chemistry | Ojeda Amador, Ana Isabel
O'Hara, C., Mulvey, R. & Ojeda Amador, A. I.
EPSRC (Engineering and Physical Sciences Research Council)
1/10/12 → 21/11/16
Project: Research Fellowship - Internally Allocated

x-ray diffractometer
Alan Kennedy (Manager)
Pure And Applied Chemistry
Facility/equipment: Equipment

Synthesis of multicomponent heavy alkali metal amide systems and extensions to zirconium chemistry
Author: Ojeda Amador, A. I., 21 Nov 2016
Supervisor: O'Hara, C. (Supervisor) & Mulvey, R. (Supervisor)
Student thesis: Doctoral Thesis

Cite this

@article{afa6b5bb9931461f8d3a5bda095ecded,

title = "Exploring the solid state and solution structural chemistry of the utility amide potassium hexamethyldisilazide (KHMDS)",

abstract = "The structural chemistry of eleven donor complexes of the important Br{\o}nsted base potassium 1,1,1,3,3,3-hexamethyldisilazide (KHMDS) has been studied. Depending on the donor, each complex adopted one of four general structural motifs. Specifically, in this study the donors employed were toluene (to give polymeric 1 and dimeric 2), THF (dimeric 3), N,N,N',N'-tetramethylethylenediamine (TMEDA) (dimeric 4), (R,R)-N,N,N',N'-tetramethyl-1,2-diaminocyclohexane [(R,R)-TMCDA] (dimeric 5), 12-crown-4 (dimeric 6), N,N,N',N'-tetramethyldiaminoethyl ether (TMDAE) (tetranuclear dimeric 8 and monomeric 10), N,N,N',N',N''-pentamethyldiethylentriamine (PMDETA) (tetranuclear dimeric 7), tris[2-dimethyl(amino)ethyl]amine (Me6TREN) (tetranuclear dimeric 9) and tris{2-(2-methoxyethoxy)ethyl}amine (TMEEA) (monomeric 11). The complexes were also studied in solution by 1H and 13C NMR spectroscopy as well as DOSY NMR spectroscopy.",

keywords = "structural chemistry, Br{\o}nsted base potassium, structural motifs, spectroscopic analysis",

author = "Ojeda-Amador, {Ana I.} and Mart{\'i}nez-Mart{\'i}nez, {Antonio J.} and Robertson, {Gemma M.} and Robertson, {Stuart D.} and Kennedy, {Alan R.} and O'Hara, {Charles T.}",

year = "2017",

month = may,

day = "15",

doi = "10.1039/C7DT01118K",

language = "English",

volume = "46",

pages = "6392--6403",

journal = "Dalton Transactions",

issn = "1477-9226",

publisher = "Royal Society of Chemistry",

number = "19",

}

Exploring the solid state and solution structural chemistry of the utility amide potassium hexamethyldisilazide (KHMDS). / Ojeda-Amador, Ana I.; Martínez-Martínez, Antonio J.; Robertson, Gemma M.; Robertson, Stuart D.; Kennedy, Alan R.; O'Hara, Charles T.

In: Dalton Transactions, Vol. 46, No. 19, 15.05.2017, p. 6392-6403.

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

TY - JOUR

T1 - Exploring the solid state and solution structural chemistry of the utility amide potassium hexamethyldisilazide (KHMDS)

AU - Ojeda-Amador, Ana I.

AU - Martínez-Martínez, Antonio J.

AU - Robertson, Gemma M.

AU - Robertson, Stuart D.

AU - Kennedy, Alan R.

AU - O'Hara, Charles T.

PY - 2017/5/15

Y1 - 2017/5/15

N2 - The structural chemistry of eleven donor complexes of the important Brønsted base potassium 1,1,1,3,3,3-hexamethyldisilazide (KHMDS) has been studied. Depending on the donor, each complex adopted one of four general structural motifs. Specifically, in this study the donors employed were toluene (to give polymeric 1 and dimeric 2), THF (dimeric 3), N,N,N',N'-tetramethylethylenediamine (TMEDA) (dimeric 4), (R,R)-N,N,N',N'-tetramethyl-1,2-diaminocyclohexane [(R,R)-TMCDA] (dimeric 5), 12-crown-4 (dimeric 6), N,N,N',N'-tetramethyldiaminoethyl ether (TMDAE) (tetranuclear dimeric 8 and monomeric 10), N,N,N',N',N''-pentamethyldiethylentriamine (PMDETA) (tetranuclear dimeric 7), tris[2-dimethyl(amino)ethyl]amine (Me6TREN) (tetranuclear dimeric 9) and tris{2-(2-methoxyethoxy)ethyl}amine (TMEEA) (monomeric 11). The complexes were also studied in solution by 1H and 13C NMR spectroscopy as well as DOSY NMR spectroscopy.

AB - The structural chemistry of eleven donor complexes of the important Brønsted base potassium 1,1,1,3,3,3-hexamethyldisilazide (KHMDS) has been studied. Depending on the donor, each complex adopted one of four general structural motifs. Specifically, in this study the donors employed were toluene (to give polymeric 1 and dimeric 2), THF (dimeric 3), N,N,N',N'-tetramethylethylenediamine (TMEDA) (dimeric 4), (R,R)-N,N,N',N'-tetramethyl-1,2-diaminocyclohexane [(R,R)-TMCDA] (dimeric 5), 12-crown-4 (dimeric 6), N,N,N',N'-tetramethyldiaminoethyl ether (TMDAE) (tetranuclear dimeric 8 and monomeric 10), N,N,N',N',N''-pentamethyldiethylentriamine (PMDETA) (tetranuclear dimeric 7), tris[2-dimethyl(amino)ethyl]amine (Me6TREN) (tetranuclear dimeric 9) and tris{2-(2-methoxyethoxy)ethyl}amine (TMEEA) (monomeric 11). The complexes were also studied in solution by 1H and 13C NMR spectroscopy as well as DOSY NMR spectroscopy.

KW - structural chemistry

KW - Brønsted base potassium

KW - structural motifs

KW - spectroscopic analysis

UR - http://pubs.rsc.org/en/Journals/JournalIssues/DT

U2 - 10.1039/C7DT01118K

DO - 10.1039/C7DT01118K

M3 - Article

VL - 46

SP - 6392

EP - 6403

JO - Dalton Transactions

JF - Dalton Transactions

SN - 1477-9226

IS - 19

ER -

Exploring the solid state and solution structural chemistry of the utility amide potassium hexamethyldisilazide (KHMDS)

Abstract

Keywords

Access to Document

Lithium Cuprates to Copper Lithiates: A New Dawn in Metal Catalysed Chemistry

Chiral Concepts in s-Block Metal Amide Chemistry | Ojeda Amador, Ana Isabel

x-ray diffractometer

Synthesis of multicomponent heavy alkali metal amide systems and extensions to zirconium chemistry

Cite this