Discrimination of Chiral Guests by Chiral Channels: Variable Temperature Studies by SXRD and Solid State 13C NMR of the Deoxycholic Acid Complexes of Camphorquinone and Endo-3-Bromocamphor

3a,12a-Dihydroxy-5b-cholan-24-oic acid (deoxycholic acid DCA) is able to discriminate between the R- and S-enantiomers of camphorquinone and endo-(1)-3-bromocamphor and select only the S-enantiomers from a racemic mixture. DCA forms novel well ordered 1:1 adducts with (1S)-(1)-camphorquinone and (1S...

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Main Authors: Mohamed I. M., Tahir, Nicholas, H. Rees, Stephen, J. Heyes, Andrew, R. Cowley, Keith, Prout
Format: Article
Language:English
English
Published: Wiley-Blackwell 2008
Online Access:http://psasir.upm.edu.my/id/eprint/5809/
http://psasir.upm.edu.my/id/eprint/5809/1/Discrimination%20of%20Chiral%20Guests%20by%20Chiral%20Channels.pdf
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author Mohamed I. M., Tahir
Nicholas, H. Rees
Stephen, J. Heyes
Andrew, R. Cowley
Keith, Prout
author_facet Mohamed I. M., Tahir
Nicholas, H. Rees
Stephen, J. Heyes
Andrew, R. Cowley
Keith, Prout
author_sort Mohamed I. M., Tahir
building UPM Institutional Repository
collection Online Access
description 3a,12a-Dihydroxy-5b-cholan-24-oic acid (deoxycholic acid DCA) is able to discriminate between the R- and S-enantiomers of camphorquinone and endo-(1)-3-bromocamphor and select only the S-enantiomers from a racemic mixture. DCA forms novel well ordered 1:1 adducts with (1S)-(1)-camphorquinone and (1S)-endo-(-)-3-bromocamphor, both of which have been characterized by single crystal X-ray diffraction SXRD). When DCA is cocrystallized with (RS)-camphorquinone and (RS)-endo-3-bromocamphor,1:1 adducts of the S-enantiomers are produced together with crystals of the free racemic guest. In contrast, in the absence of (1S)-(1)-camphorquinone, DCA forms a 2:1 adduct with (1R)-(2)-camphorquinone. In this 2:1 adduct the guest is disordered at ambient temperature and undergoes a phase change in the region 160–130 K similar to that observed for the ferrocene adduct, but with only partial ordering of the guest. The SXRD structure of the low temperature form and the variable temperature 13C CP/MAS NMR are reported. Cocrystallizing DCA with (1R)-endo-(1)-3-bromocamphor gives the free guest and a glassy solid.
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spelling upm-58092015-10-23T07:57:00Z http://psasir.upm.edu.my/id/eprint/5809/ Discrimination of Chiral Guests by Chiral Channels: Variable Temperature Studies by SXRD and Solid State 13C NMR of the Deoxycholic Acid Complexes of Camphorquinone and Endo-3-Bromocamphor Mohamed I. M., Tahir Nicholas, H. Rees Stephen, J. Heyes Andrew, R. Cowley Keith, Prout 3a,12a-Dihydroxy-5b-cholan-24-oic acid (deoxycholic acid DCA) is able to discriminate between the R- and S-enantiomers of camphorquinone and endo-(1)-3-bromocamphor and select only the S-enantiomers from a racemic mixture. DCA forms novel well ordered 1:1 adducts with (1S)-(1)-camphorquinone and (1S)-endo-(-)-3-bromocamphor, both of which have been characterized by single crystal X-ray diffraction SXRD). When DCA is cocrystallized with (RS)-camphorquinone and (RS)-endo-3-bromocamphor,1:1 adducts of the S-enantiomers are produced together with crystals of the free racemic guest. In contrast, in the absence of (1S)-(1)-camphorquinone, DCA forms a 2:1 adduct with (1R)-(2)-camphorquinone. In this 2:1 adduct the guest is disordered at ambient temperature and undergoes a phase change in the region 160–130 K similar to that observed for the ferrocene adduct, but with only partial ordering of the guest. The SXRD structure of the low temperature form and the variable temperature 13C CP/MAS NMR are reported. Cocrystallizing DCA with (1R)-endo-(1)-3-bromocamphor gives the free guest and a glassy solid. Wiley-Blackwell 2008 Article PeerReviewed application/pdf en http://psasir.upm.edu.my/id/eprint/5809/1/Discrimination%20of%20Chiral%20Guests%20by%20Chiral%20Channels.pdf Mohamed I. M., Tahir and Nicholas, H. Rees and Stephen, J. Heyes and Andrew, R. Cowley and Keith, Prout (2008) Discrimination of Chiral Guests by Chiral Channels: Variable Temperature Studies by SXRD and Solid State 13C NMR of the Deoxycholic Acid Complexes of Camphorquinone and Endo-3-Bromocamphor. Chirality, 20 (7). pp. 863-870. ISSN 0899-0042 http://dx.doi.org/10.1002/chir.20561 10.1002/chir.20561 English
spellingShingle Mohamed I. M., Tahir
Nicholas, H. Rees
Stephen, J. Heyes
Andrew, R. Cowley
Keith, Prout
Discrimination of Chiral Guests by Chiral Channels: Variable Temperature Studies by SXRD and Solid State 13C NMR of the Deoxycholic Acid Complexes of Camphorquinone and Endo-3-Bromocamphor
title Discrimination of Chiral Guests by Chiral Channels: Variable Temperature Studies by SXRD and Solid State 13C NMR of the Deoxycholic Acid Complexes of Camphorquinone and Endo-3-Bromocamphor
title_full Discrimination of Chiral Guests by Chiral Channels: Variable Temperature Studies by SXRD and Solid State 13C NMR of the Deoxycholic Acid Complexes of Camphorquinone and Endo-3-Bromocamphor
title_fullStr Discrimination of Chiral Guests by Chiral Channels: Variable Temperature Studies by SXRD and Solid State 13C NMR of the Deoxycholic Acid Complexes of Camphorquinone and Endo-3-Bromocamphor
title_full_unstemmed Discrimination of Chiral Guests by Chiral Channels: Variable Temperature Studies by SXRD and Solid State 13C NMR of the Deoxycholic Acid Complexes of Camphorquinone and Endo-3-Bromocamphor
title_short Discrimination of Chiral Guests by Chiral Channels: Variable Temperature Studies by SXRD and Solid State 13C NMR of the Deoxycholic Acid Complexes of Camphorquinone and Endo-3-Bromocamphor
title_sort discrimination of chiral guests by chiral channels: variable temperature studies by sxrd and solid state 13c nmr of the deoxycholic acid complexes of camphorquinone and endo-3-bromocamphor
url http://psasir.upm.edu.my/id/eprint/5809/
http://psasir.upm.edu.my/id/eprint/5809/
http://psasir.upm.edu.my/id/eprint/5809/
http://psasir.upm.edu.my/id/eprint/5809/1/Discrimination%20of%20Chiral%20Guests%20by%20Chiral%20Channels.pdf