207Pb-1H two-dimensional NMR spectroscopy:: A useful new tool for probing lead(II) coordination chemistry

被引:54
作者
Claudio, ES [1 ]
ter Horst, MA [1 ]
Forde, CE [1 ]
Stern, CL [1 ]
Zart, MK [1 ]
Godwin, HA [1 ]
机构
[1] Northwestern Univ, Dept Chem, Evanston, IL 60208 USA
关键词
D O I
10.1021/ic9909431
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Despite the fact that lead poisoning is the most common disease of environmental origin in the United States, the spectroscopic properties of aqueous Pb(II) coordination compounds have not been extensively investigated. Spectroscopic techniques that can be used to probe the fundamental coordination chemistry of Pb(TI) will aid in both the development of water-soluble ligands that bind lead both tightly and selectively and the characterization of potential biological targets. Here, we report the preparation and characterization of a series of Pb(II) complexes of amido derivatives of EDTA. The Pb-207, chemical shift observed in these complexes (2441, 2189, and 1764 ppm for [Pb(EDTA)](2-) Pb(EDTA-N-2), and [Pb(EDTA-N-4)](2+), respectively) provides an extremely sensitive measure of the local environment and the charge on each complex. These shifts help to map out the lead chemical measure of the local environment shift range that can be expected for biologically relevant sites. In addition, we report the first two-dimensional Pb-207-H-1 heteronuclear multiple-quantum correlation (HMQC) nuclear magnetic resonance spectra and demonstrate that this experiment can provide useful information about the lead coordination environment in aqueous Pb(II) complexes. Because this technique allows Pb-207-H-1 couplings through three bonds to;be identified readily, Pb-207-H-1 NMR spectroscopy should prove useful for the investigation of Pb(II) in more complex systems (e.g., biological and environmental samples).
引用
收藏
页码:1391 / 1397
页数:7
相关论文
共 53 条
[1]   LEAD SEQUESTERING AGENTS .2. SYNTHESIS OF MONO(HYDROXYPYRIDINETHIONE) AND BIS(HYDROXYPYRIDINETHIONE) LIGANDS AND THEIR LEAD COMPLEXES - STRUCTURE OF BIS(6-(DIETHYLCARBAMOYL)-1-HYDROXY-2(1H)-PYRIDINE-2-THIONATO-O,S)LEAD(II) [J].
ABUDARI, K ;
KARPISHIN, TB ;
RAYMOND, KN .
INORGANIC CHEMISTRY, 1993, 32 (14) :3052-3055
[2]   LEAD SEQUESTERING AGENTS .1. SYNTHESIS, PHYSICAL-PROPERTIES, AND STRUCTURES OF LEAD THIOHYDROXAMATO COMPLEXES [J].
ABUDARI, K ;
HAHN, FE ;
RAYMOND, KN .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1990, 112 (04) :1519-1524
[3]  
ALLEN FHB, 1979, ACTA CRYSTALLOGR, P2331
[4]  
[Anonymous], GETTING LEAD OUT COM
[5]   Lead-207 NMR: A novel probe for the study of calcium-binding proteins [J].
Aramini, JM ;
Hiraoki, T ;
Yazawa, M ;
Yuan, T ;
Zhang, MJ ;
Vogel, HJ .
JOURNAL OF BIOLOGICAL INORGANIC CHEMISTRY, 1996, 1 (01) :39-48
[6]   Amide group coordination to the Pb2+ ion [J].
Battistuzzi, G ;
Borsari, M ;
Menabue, L ;
Saladini, M ;
Sola, M .
INORGANIC CHEMISTRY, 1996, 35 (14) :4239-4247
[7]   CORRELATION OF PROTON AND N-15 CHEMICAL-SHIFTS BY MULTIPLE QUANTUM NMR [J].
BAX, A ;
GRIFFEY, RH ;
HAWKINS, BL .
JOURNAL OF MAGNETIC RESONANCE, 1983, 55 (02) :301-315
[8]   VERSATILE CATION COMPLEXATION BY A CALIX[4]ARENE TETRAAMIDE(L) - SYNTHESIS AND CRYSTAL-STRUCTURE OF [ML][CLO4](2)CENTER-DOT-NMECN (M=FE-II, NI-II, CU-II, ZN-II OR PB-II) [J].
BEER, PD ;
DREW, MGB ;
LEESON, PB ;
OGDEN, MI .
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1995, (08) :1273-1283
[9]  
*CIB GEIG, 1969, DIAM TETR BIS, V71
[10]  
COLEMAN JE, 1993, METHOD ENZYMOL, V227, P16