Identification of the internal axial ligand of HO2-cobalt(III)-bleomycin:: 1H{15N} HSQC NMR investigation of bleomycin, deglycobleomycin, and their hydroperoxide-cobalt(III) complexes

被引:15
|
作者
Xia, CW [1 ]
Försterling, FH [1 ]
Petering, DH [1 ]
机构
[1] Univ Wisconsin, Dept Chem, Milwaukee, WI 53201 USA
关键词
D O I
10.1021/bi030016c
中图分类号
Q5 [生物化学]; Q7 [分子生物学];
学科分类号
071010 ; 081704 ;
摘要
The identity of the axial ligand contributed by the drug in hydroperoxide-Co(III)-bleomycin and hydroperoxide-Co(III)-deglycobleomycin has been in doubt. With each structure, a combination of H-1{N-15} HSQC and HMBC and H-1 COSY and NOESY NMR spectroscopy was used to observe and completely assign the nonaromatic N-15 chemical shifts of natural abundance bleomycin in the two hydroperoxide-Co(III) structures. Together with the N-15 assignments from a published ID N-15 spectrum, the results permitted the assignment of the primary amine nitrogen to an axial ligand position in both structures.
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页码:6559 / 6564
页数:6
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