Proton NMR study of iron(II)-bleomycin: Assignment of resonances by saturation transfer experiments

R. P. Pillai; R. E. Lenkinski; T. T. Sakai; J. M. Geckle; N. R. Krishna; J. D. Glickson

doi:10.1016/0006-291X(80)91220-6

Proton NMR study of iron(II)-bleomycin: Assignment of resonances by saturation transfer experiments

R. P. Pillai, R. E. Lenkinski, T. T. Sakai, J. M. Geckle, N. R. Krishna, J. D. Glickson

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Abstract

The assignment of the paramagnetically shifted resonances of the Fe(II)-bleomycin complex in D₂O has been accomplished using the transfer of saturation method. A number of additional resonances arising from labile NH protons which are shifted by the metal ion are observed in the ¹H spectrum of the complex in H₂O. The temperature dependence of the chemical shifts is consistent with the formation of an isolated 1:1 complex, but does not obey either the Curie Law or the Curie-Weiss Law. The magnitude of the shifts suggests that the valeric acid hydroxyl (or carbonyl) group, the α-amino group, the imidazole N^π, the carbamoyl oxygen, the pyrimidine N₁ and/or the secondary amino group may be coordinated to the iron(II).

Original language	English (US)
Pages (from-to)	341-349
Number of pages	9
Journal	Topics in Catalysis
Volume	96
Issue number	1
DOIs	https://doi.org/10.1016/0006-291X(80)91220-6
State	Published - 1980

ASJC Scopus subject areas

Catalysis
Chemistry(all)
Biochemistry
Biophysics
Molecular Biology

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10.1016/0006-291X(80)91220-6

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@article{b6a80ff9ec554eeda9e41eddea4f3062,

title = "Proton NMR study of iron(II)-bleomycin: Assignment of resonances by saturation transfer experiments",

abstract = "The assignment of the paramagnetically shifted resonances of the Fe(II)-bleomycin complex in D2O has been accomplished using the transfer of saturation method. A number of additional resonances arising from labile NH protons which are shifted by the metal ion are observed in the 1H spectrum of the complex in H2O. The temperature dependence of the chemical shifts is consistent with the formation of an isolated 1:1 complex, but does not obey either the Curie Law or the Curie-Weiss Law. The magnitude of the shifts suggests that the valeric acid hydroxyl (or carbonyl) group, the α-amino group, the imidazole Nπ, the carbamoyl oxygen, the pyrimidine N1 and/or the secondary amino group may be coordinated to the iron(II).",

author = "Pillai, {R. P.} and Lenkinski, {R. E.} and Sakai, {T. T.} and Geckle, {J. M.} and Krishna, {N. R.} and Glickson, {J. D.}",

note = "Funding Information: Acknowledgement We thank Drs. W.T. Bradner and S.T. Crooke of Bristol Laboratories for the generous gift of Blenoxane. This research was supported by Public Health Service Grants CA-13148 (John R. Durant and JDG), CA-24411 (JDG), GM-27900 (TTS) and by a Faculty Research Award FRA-162 (JDG) from the American Cancer Society.",

year = "1980",

doi = "10.1016/0006-291X(80)91220-6",

language = "English (US)",

volume = "96",

pages = "341--349",

journal = "Topics in Catalysis",

number = "1",

}

TY - JOUR

T1 - Proton NMR study of iron(II)-bleomycin

T2 - Assignment of resonances by saturation transfer experiments

AU - Pillai, R. P.

AU - Lenkinski, R. E.

AU - Sakai, T. T.

AU - Geckle, J. M.

AU - Krishna, N. R.

AU - Glickson, J. D.

N1 - Funding Information: Acknowledgement We thank Drs. W.T. Bradner and S.T. Crooke of Bristol Laboratories for the generous gift of Blenoxane. This research was supported by Public Health Service Grants CA-13148 (John R. Durant and JDG), CA-24411 (JDG), GM-27900 (TTS) and by a Faculty Research Award FRA-162 (JDG) from the American Cancer Society.

PY - 1980

Y1 - 1980

N2 - The assignment of the paramagnetically shifted resonances of the Fe(II)-bleomycin complex in D2O has been accomplished using the transfer of saturation method. A number of additional resonances arising from labile NH protons which are shifted by the metal ion are observed in the 1H spectrum of the complex in H2O. The temperature dependence of the chemical shifts is consistent with the formation of an isolated 1:1 complex, but does not obey either the Curie Law or the Curie-Weiss Law. The magnitude of the shifts suggests that the valeric acid hydroxyl (or carbonyl) group, the α-amino group, the imidazole Nπ, the carbamoyl oxygen, the pyrimidine N1 and/or the secondary amino group may be coordinated to the iron(II).

AB - The assignment of the paramagnetically shifted resonances of the Fe(II)-bleomycin complex in D2O has been accomplished using the transfer of saturation method. A number of additional resonances arising from labile NH protons which are shifted by the metal ion are observed in the 1H spectrum of the complex in H2O. The temperature dependence of the chemical shifts is consistent with the formation of an isolated 1:1 complex, but does not obey either the Curie Law or the Curie-Weiss Law. The magnitude of the shifts suggests that the valeric acid hydroxyl (or carbonyl) group, the α-amino group, the imidazole Nπ, the carbamoyl oxygen, the pyrimidine N1 and/or the secondary amino group may be coordinated to the iron(II).

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DO - 10.1016/0006-291X(80)91220-6

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AN - SCOPUS:0019182473

VL - 96

SP - 341

EP - 349

JO - Topics in Catalysis

JF - Topics in Catalysis

IS - 1

ER -

Proton NMR study of iron(II)-bleomycin: Assignment of resonances by saturation transfer experiments

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