Unknown

Dataset Information

0

Direct measurement of the Mn(II) hydration state in metal complexes and metalloproteins through 17O NMR line widths.


ABSTRACT: Here we describe a simple method to estimate the inner-sphere hydration state of the Mn(II) ion in coordination complexes and metalloproteins. The line width of bulk H2(17)O is measured in the presence and absence of Mn(II) as a function of temperature, and transverse (17)O relaxivities are calculated. It is demonstrated that the maximum (17)O relaxivity is directly proportional to the number of inner-sphere water ligands (q). Using a combination of literature data and experimental data for 12 Mn(II) complexes, we show that this method provides accurate estimates of q with an uncertainty of ±0.2 water molecules. The method can be implemented on commercial NMR spectrometers working at fields of 7 T and higher. The hydration number can be obtained for micromolar Mn(II) concentrations. We show that the technique can be extended to metalloproteins or complex:protein interactions. For example, Mn(II) binds to the multimetal binding site A on human serum albumin with two inner-sphere water ligands that undergo rapid exchange (1.06 × 10(8) s(-1) at 37 °C). The possibility of extending this technique to other metal ions such as Gd(III) is discussed.

SUBMITTER: Gale EM 

PROVIDER: S-EPMC3864583 | biostudies-literature | 2013 Dec

REPOSITORIES: biostudies-literature

altmetric image

Publications

Direct measurement of the Mn(II) hydration state in metal complexes and metalloproteins through 17O NMR line widths.

Gale Eric M EM   Zhu Jiang J   Caravan Peter P  

Journal of the American Chemical Society 20131024 49


Here we describe a simple method to estimate the inner-sphere hydration state of the Mn(II) ion in coordination complexes and metalloproteins. The line width of bulk H2(17)O is measured in the presence and absence of Mn(II) as a function of temperature, and transverse (17)O relaxivities are calculated. It is demonstrated that the maximum (17)O relaxivity is directly proportional to the number of inner-sphere water ligands (q). Using a combination of literature data and experimental data for 12 M  ...[more]

Similar Datasets

| S-EPMC5873045 | biostudies-literature
| S-EPMC3222302 | biostudies-literature
| S-EPMC6689193 | biostudies-literature
| S-EPMC5245840 | biostudies-literature
| S-EPMC4118035 | biostudies-literature
| S-EPMC3303200 | biostudies-literature
| S-EPMC3386638 | biostudies-literature
| S-EPMC8223985 | biostudies-literature
| S-EPMC2711274 | biostudies-literature
| S-EPMC3756834 | biostudies-literature