Copper diamidocarbene complexes: characterization of monomeric to tetrameric species

Lee R. Collins; John P. Lowe; Mary F. Mahon; Rebecca C. Poulten; Michael K. Whittlesey

doi:10.1021/ic4031014

Copper diamidocarbene complexes: characterization of monomeric to tetrameric species

Lee R. Collins, John P. Lowe, Mary F. Mahon, Rebecca C. Poulten, Michael K. Whittlesey

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Abstract

Treatment of CuCl with 1 equiv of the in situ prepared N-mesityl- substituted diamidocarbene 6-MesDAC produced a mixture of the dimeric and trimeric copper complexes [(6-MesDAC)CuCl] (1) and [(6-MesDAC) (CuCl)] (2). Combining CuCl with isolated, free 6-MesDAC in 1:1 and 3:2 ratios gave just 1 and 2, respectively, while increasing the ratio to >5:1 allowed the isolation of small amounts of the tetrameric copper complex [(6-MesDAC)(CuCl)] (3). Efforts to bring about metathesis reactions of 1 with MOBu (M = Li, Na, K) proved successful only for M = Li to afford the spectroscopically characterized ate product [(6-MesDAC)CuCl·LiOBu·2THF] (5). Attempts to crystallize this species instead gave a 1:1 mixture of 1 and the monomer [(6-MesDAC)CuCl] (6). The X-ray structures of 1-3 and 1 + 6, along with the cation [Cu(6-MesDAC)] (4), have been determined.

Original language	English
Pages (from-to)	2699-2707
Number of pages	9
Journal	Inorganic Chemistry
Volume	53
Issue number	5
Early online date	11 Feb 2014
DOIs	https://doi.org/10.1021/ic4031014
Publication status	Published - 3 Mar 2014

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500 MHZ NMR SPECTROMETER TO SUPPORT ORGANIC, BIO-ORGANIC AND INORGANIC CHEMISTRY
Whittlesey, M., Danson, M., Frost, C., Kohn, R., Lowe, J., Weller, A. & Williams, J.
Engineering and Physical Sciences Research Council
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title = "Copper diamidocarbene complexes: characterization of monomeric to tetrameric species",

abstract = "Treatment of CuCl with 1 equiv of the in situ prepared N-mesityl- substituted diamidocarbene 6-MesDAC produced a mixture of the dimeric and trimeric copper complexes [(6-MesDAC)CuCl] (1) and [(6-MesDAC) (CuCl)] (2). Combining CuCl with isolated, free 6-MesDAC in 1:1 and 3:2 ratios gave just 1 and 2, respectively, while increasing the ratio to >5:1 allowed the isolation of small amounts of the tetrameric copper complex [(6-MesDAC)(CuCl)] (3). Efforts to bring about metathesis reactions of 1 with MOBu (M = Li, Na, K) proved successful only for M = Li to afford the spectroscopically characterized ate product [(6-MesDAC)CuCl·LiOBu·2THF] (5). Attempts to crystallize this species instead gave a 1:1 mixture of 1 and the monomer [(6-MesDAC)CuCl] (6). The X-ray structures of 1-3 and 1 + 6, along with the cation [Cu(6-MesDAC)] (4), have been determined.",

author = "Collins, {Lee R.} and Lowe, {John P.} and Mahon, {Mary F.} and Poulten, {Rebecca C.} and Whittlesey, {Michael K.}",

year = "2014",

month = mar,

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doi = "10.1021/ic4031014",

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volume = "53",

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journal = "Inorganic Chemistry",

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T1 - Copper diamidocarbene complexes

T2 - characterization of monomeric to tetrameric species

AU - Collins, Lee R.

AU - Lowe, John P.

AU - Mahon, Mary F.

AU - Poulten, Rebecca C.

AU - Whittlesey, Michael K.

PY - 2014/3/3

Y1 - 2014/3/3

N2 - Treatment of CuCl with 1 equiv of the in situ prepared N-mesityl- substituted diamidocarbene 6-MesDAC produced a mixture of the dimeric and trimeric copper complexes [(6-MesDAC)CuCl] (1) and [(6-MesDAC) (CuCl)] (2). Combining CuCl with isolated, free 6-MesDAC in 1:1 and 3:2 ratios gave just 1 and 2, respectively, while increasing the ratio to >5:1 allowed the isolation of small amounts of the tetrameric copper complex [(6-MesDAC)(CuCl)] (3). Efforts to bring about metathesis reactions of 1 with MOBu (M = Li, Na, K) proved successful only for M = Li to afford the spectroscopically characterized ate product [(6-MesDAC)CuCl·LiOBu·2THF] (5). Attempts to crystallize this species instead gave a 1:1 mixture of 1 and the monomer [(6-MesDAC)CuCl] (6). The X-ray structures of 1-3 and 1 + 6, along with the cation [Cu(6-MesDAC)] (4), have been determined.

AB - Treatment of CuCl with 1 equiv of the in situ prepared N-mesityl- substituted diamidocarbene 6-MesDAC produced a mixture of the dimeric and trimeric copper complexes [(6-MesDAC)CuCl] (1) and [(6-MesDAC) (CuCl)] (2). Combining CuCl with isolated, free 6-MesDAC in 1:1 and 3:2 ratios gave just 1 and 2, respectively, while increasing the ratio to >5:1 allowed the isolation of small amounts of the tetrameric copper complex [(6-MesDAC)(CuCl)] (3). Efforts to bring about metathesis reactions of 1 with MOBu (M = Li, Na, K) proved successful only for M = Li to afford the spectroscopically characterized ate product [(6-MesDAC)CuCl·LiOBu·2THF] (5). Attempts to crystallize this species instead gave a 1:1 mixture of 1 and the monomer [(6-MesDAC)CuCl] (6). The X-ray structures of 1-3 and 1 + 6, along with the cation [Cu(6-MesDAC)] (4), have been determined.

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JO - Inorganic Chemistry

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Copper diamidocarbene complexes: characterization of monomeric to tetrameric species

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500 MHZ NMR SPECTROMETER TO SUPPORT ORGANIC, BIO-ORGANIC AND INORGANIC CHEMISTRY

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