Final published version
Research output: Contribution to Journal/Magazine › Journal article › peer-review
Research output: Contribution to Journal/Magazine › Journal article › peer-review
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TY - JOUR
T1 - Chromatographic separation of stereoisomers of ligand-bridged diruthenium polypyridyl species
AU - Fletcher, Nicholas C.
AU - Junk, Peter C.
AU - Reitsma, David A.
AU - Keene, F. Richard
PY - 1998/1/7
Y1 - 1998/1/7
N2 - Cation-exchange chromatographic techniques have been developed to separate stereoisomers of polymetallic complexes, using SP Sephadex C-25 as support. Through the example of the ligand-bridged dinuclear cation [{Ru(dmbpy)2}2(μ-bipym)]4+ (dmbpy = 4,4′-dimethyl-2,2′-bipyridine, bipym = 2,2′-bipyrimidine), the isolation and characterisation of the meso and rac diastereoisomers by elution with aqueous sodium toluene-4-sulfonate solution are demonstrated. The effects of variation in salt concentration and temperature on the efficacy of the separation are discussed. The enantiomeric pair of the rac diastereoisomer (ΔΔ and ΛΛ) was subsequently chromatographically resolved on SP Sephadex C-25, relying upon the inherent chirality of the support. Optical resolutions using eluents with chiral anions [aquecus sodium (+)-O,O′-dibenzoyl-D-tartrate and sodium (-)-O,O′-dibenzoyl-L-tartrate] were investigated, with the (-)-enantiomer demonstrating a positive [the (+)-enantiomer a negative] synergistic effect in combination with the Sephadex support. Crystals of the meso form were isolated, allowing an X-ray structural determination.
AB - Cation-exchange chromatographic techniques have been developed to separate stereoisomers of polymetallic complexes, using SP Sephadex C-25 as support. Through the example of the ligand-bridged dinuclear cation [{Ru(dmbpy)2}2(μ-bipym)]4+ (dmbpy = 4,4′-dimethyl-2,2′-bipyridine, bipym = 2,2′-bipyrimidine), the isolation and characterisation of the meso and rac diastereoisomers by elution with aqueous sodium toluene-4-sulfonate solution are demonstrated. The effects of variation in salt concentration and temperature on the efficacy of the separation are discussed. The enantiomeric pair of the rac diastereoisomer (ΔΔ and ΛΛ) was subsequently chromatographically resolved on SP Sephadex C-25, relying upon the inherent chirality of the support. Optical resolutions using eluents with chiral anions [aquecus sodium (+)-O,O′-dibenzoyl-D-tartrate and sodium (-)-O,O′-dibenzoyl-L-tartrate] were investigated, with the (-)-enantiomer demonstrating a positive [the (+)-enantiomer a negative] synergistic effect in combination with the Sephadex support. Crystals of the meso form were isolated, allowing an X-ray structural determination.
U2 - 10.1039/a705947g
DO - 10.1039/a705947g
M3 - Journal article
AN - SCOPUS:0343004213
VL - 1998
SP - 133
EP - 138
JO - Journal of the Chemical Society - Dalton Transactions
JF - Journal of the Chemical Society - Dalton Transactions
SN - 0300-9246
IS - 1
ER -