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Tris(pyronato)- and Tris(pyridonato)-ruthenium(III) Complexes and Solution NMR Studies.

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Title: Tris(pyronato)- and Tris(pyridonato)-ruthenium(III) Complexes and Solution NMR Studies.
Authors: Kennedy, David C.1, Wu, Adam1, Patrick, Brian O.1, James, Brian R.1 brj@chem.unc.ca
Source: Inorganic Chemistry. 9/19/2005, Vol. 44 Issue 19, p6529-6535. 8p. 4 Diagrams, 3 Charts, 2 Graphs.
Subjects: Ruthenium compounds, Ruthenium, Breast cancer, Cancer cells, Cell lines, Nuclear magnetic resonance, Electrochemical analysis, Physical & theoretical chemistry
Abstract: The water-soluble RuIII maltolato, ethylmaltolato, and pyridonato complexes, Ru(O-O′)3 (O-O′ = ma (1a), etma (1b), pyd (2a)), were synthesized (Hma = 3-hydroxy-2-methyl-4-pyrone, Hetma = 2-ethyl-3-hydroxy-4-pyrone, Hpyd = 3-hydroxy-1,2-dimethyl-4-pyridone). The complexes were characterized by elemental analysis, NMR and IR spectroscopies, MS, solution conductivity, and cyclic voltammetry, and in the case of Ru(ma)3, by X-ray crystallography, which revealed a met configuration. The paramagnetic 1H NMR resonances of 1a, 1b, and 2a were assigned using 2D methods (¹H COSY and ¹H-13C HMQC) and variable-temperature ¹H NMR data and showed that la and lb exist in aqueous solution predominantly as a mer isomer, while 2a is a mixture of mer and fac isomers. Although a 13C NMR spectrum could not be measured directly for la, a partial 13C spectrum was generated from the ¹H-13C HMQC spectrum. Complexes 1a and 1b were tested for anti-proliferatory activity against the human breast cancer cell line MDA-MB-435S and gave IC50 values of 140 and 90 μM, respectively. [ABSTRACT FROM AUTHOR]
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Abstract:The water-soluble RuIII maltolato, ethylmaltolato, and pyridonato complexes, Ru(O-O′)3 (O-O′ = ma (1a), etma (1b), pyd (2a)), were synthesized (Hma = 3-hydroxy-2-methyl-4-pyrone, Hetma = 2-ethyl-3-hydroxy-4-pyrone, Hpyd = 3-hydroxy-1,2-dimethyl-4-pyridone). The complexes were characterized by elemental analysis, NMR and IR spectroscopies, MS, solution conductivity, and cyclic voltammetry, and in the case of Ru(ma)3, by X-ray crystallography, which revealed a met configuration. The paramagnetic 1H NMR resonances of 1a, 1b, and 2a were assigned using 2D methods (¹H COSY and ¹H-13C HMQC) and variable-temperature ¹H NMR data and showed that la and lb exist in aqueous solution predominantly as a mer isomer, while 2a is a mixture of mer and fac isomers. Although a 13C NMR spectrum could not be measured directly for la, a partial 13C spectrum was generated from the ¹H-13C HMQC spectrum. Complexes 1a and 1b were tested for anti-proliferatory activity against the human breast cancer cell line MDA-MB-435S and gave IC50 values of 140 and 90 μM, respectively. [ABSTRACT FROM AUTHOR]
ISSN:00201669
DOI:10.1021/ic050034d