Spin pair geometry revealed by high-field DEER in the presence of conformational distributions

Orientation selection on two nitroxide-labelled shape-persistent molecules is demonstrated by high-field pulsed electron–electron double resonance experiments at a frequency of 95 GHz with a commercial spectrometer. The experiments are performed with fixed observer and pump frequencies by variation...

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Published in:Journal of magnetic resonance (1997) Vol. 185; no. 1; pp. 118 - 129
Main Authors: Polyhach, Ye, Godt, A., Bauer, C., Jeschke, G.
Format: Journal Article
Language:English
Published: United States Elsevier Inc 01.03.2007
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ISSN:1090-7807, 1096-0856
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Abstract Orientation selection on two nitroxide-labelled shape-persistent molecules is demonstrated by high-field pulsed electron–electron double resonance experiments at a frequency of 95 GHz with a commercial spectrometer. The experiments are performed with fixed observer and pump frequencies by variation of the magnetic field, so that the variation of both the dipolar frequencies and the modulation depths can be analyzed. By applying the deadtime-free four-pulse double electron–electron resonance (DEER) sequence, the lineshapes of the dipolar spectra are obtained. In the investigated linear biradical and equilateral triradical the nitroxide labels undergo restricted dynamics, so that their relative orientations are not fixed, but are correlated to some extent. In this situation, the general dependence of the dipolar spectra on the observer field can be satisfyingly modelled by simple geometrical models that involve only one rotational degree of freedom for the biradical and two rotational degrees of freedom for the triradical. A somewhat better agreement of the dipolar lineshapes for the biradical is obtained by simulations based on a molecular dynamics trajectory. For the triradical, small but significant deviations of the lineshape are observed with both models, indicating that the technique can reveal deficiencies in modelling of the conformational ensemble of a macromolecule.
AbstractList Orientation selection on two nitroxide-labelled shape-persistent molecules is demonstrated by high-field pulsed electron-electron double resonance experiments at a frequency of 95 GHz with a commercial spectrometer. The experiments are performed with fixed observer and pump frequencies by variation of the magnetic field, so that the variation of both the dipolar frequencies and the modulation depths can be analyzed. By applying the deadtime-free four-pulse double electron-electron resonance (DEER) sequence, the lineshapes of the dipolar spectra are obtained. In the investigated linear biradical and equilateral triradical the nitroxide labels undergo restricted dynamics, so that their relative orientations are not fixed, but are correlated to some extent. In this situation, the general dependence of the dipolar spectra on the observer field can be satisfyingly modelled by simple geometrical models that involve only one rotational degree of freedom for the biradical and two rotational degrees of freedom for the triradical. A somewhat better agreement of the dipolar lineshapes for the biradical is obtained by simulations based on a molecular dynamics trajectory. For the triradical, small but significant deviations of the lineshape are observed with both models, indicating that the technique can reveal deficiencies in modelling of the conformational ensemble of a macromolecule.Orientation selection on two nitroxide-labelled shape-persistent molecules is demonstrated by high-field pulsed electron-electron double resonance experiments at a frequency of 95 GHz with a commercial spectrometer. The experiments are performed with fixed observer and pump frequencies by variation of the magnetic field, so that the variation of both the dipolar frequencies and the modulation depths can be analyzed. By applying the deadtime-free four-pulse double electron-electron resonance (DEER) sequence, the lineshapes of the dipolar spectra are obtained. In the investigated linear biradical and equilateral triradical the nitroxide labels undergo restricted dynamics, so that their relative orientations are not fixed, but are correlated to some extent. In this situation, the general dependence of the dipolar spectra on the observer field can be satisfyingly modelled by simple geometrical models that involve only one rotational degree of freedom for the biradical and two rotational degrees of freedom for the triradical. A somewhat better agreement of the dipolar lineshapes for the biradical is obtained by simulations based on a molecular dynamics trajectory. For the triradical, small but significant deviations of the lineshape are observed with both models, indicating that the technique can reveal deficiencies in modelling of the conformational ensemble of a macromolecule.
Orientation selection on two nitroxide-labelled shape-persistent molecules is demonstrated by high-field pulsed electron–electron double resonance experiments at a frequency of 95 GHz with a commercial spectrometer. The experiments are performed with fixed observer and pump frequencies by variation of the magnetic field, so that the variation of both the dipolar frequencies and the modulation depths can be analyzed. By applying the deadtime-free four-pulse double electron–electron resonance (DEER) sequence, the lineshapes of the dipolar spectra are obtained. In the investigated linear biradical and equilateral triradical the nitroxide labels undergo restricted dynamics, so that their relative orientations are not fixed, but are correlated to some extent. In this situation, the general dependence of the dipolar spectra on the observer field can be satisfyingly modelled by simple geometrical models that involve only one rotational degree of freedom for the biradical and two rotational degrees of freedom for the triradical. A somewhat better agreement of the dipolar lineshapes for the biradical is obtained by simulations based on a molecular dynamics trajectory. For the triradical, small but significant deviations of the lineshape are observed with both models, indicating that the technique can reveal deficiencies in modelling of the conformational ensemble of a macromolecule.
Orientation selection on two nitroxide-labelled shape-persistent molecules is demonstrated by high-field pulsed electron-electron double resonance experiments at a frequency of 95 GHz with a commercial spectrometer. The experiments are performed with fixed observer and pump frequencies by variation of the magnetic field, so that the variation of both the dipolar frequencies and the modulation depths can be analyzed. By applying the deadtime-free four-pulse double electron-electron resonance (DEER) sequence, the lineshapes of the dipolar spectra are obtained. In the investigated linear biradical and equilateral triradical the nitroxide labels undergo restricted dynamics, so that their relative orientations are not fixed, but are correlated to some extent. In this situation, the general dependence of the dipolar spectra on the observer field can be satisfyingly modelled by simple geometrical models that involve only one rotational degree of freedom for the biradical and two rotational degrees of freedom for the triradical. A somewhat better agreement of the dipolar lineshapes for the biradical is obtained by simulations based on a molecular dynamics trajectory. For the triradical, small but significant deviations of the lineshape are observed with both models, indicating that the technique can reveal deficiencies in modelling of the conformational ensemble of a macromolecule.
Author Godt, A.
Jeschke, G.
Bauer, C.
Polyhach, Ye
Author_xml – sequence: 1
  givenname: Ye
  surname: Polyhach
  fullname: Polyhach, Ye
  organization: Max Planck Institute for Polymer Research, Postfach 3148, 55021 Mainz, Germany
– sequence: 2
  givenname: A.
  surname: Godt
  fullname: Godt, A.
  organization: Bielefeld University, Department uf Chemistry, Universitätsstraße 25, 33615 Bielefeld, Germany
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  fullname: Bauer, C.
  organization: Max Planck Institute for Polymer Research, Postfach 3148, 55021 Mainz, Germany
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  givenname: G.
  surname: Jeschke
  fullname: Jeschke, G.
  email: Gunnar.Jeschke@uni-konstanz.de
  organization: Max Planck Institute for Polymer Research, Postfach 3148, 55021 Mainz, Germany
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Issue 1
Keywords Orientation selection
Spin labeling
High-field EPR
EPR
ELDOR
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  article-title: Assessing oligomerization of membrane proteins by four-pulse DEER: pH-dependent dimerization of NhaA Na+/H+ antiporter of E. coli
  publication-title: Biophys. J.
  doi: 10.1529/biophysj.105.062232
– volume: 180
  start-page: 178
  year: 2006
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  article-title: Distance between a native cofactor and a spin label in the reaction centre of Rhodobacter sphaeroides by a two-frequency pulsed electron paramagnetic resonance method and molecular dynamics simulations
  publication-title: J. Magn. Reson.
  doi: 10.1016/j.jmr.2006.02.008
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Snippet Orientation selection on two nitroxide-labelled shape-persistent molecules is demonstrated by high-field pulsed electron–electron double resonance experiments...
Orientation selection on two nitroxide-labelled shape-persistent molecules is demonstrated by high-field pulsed electron-electron double resonance experiments...
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StartPage 118
SubjectTerms Algorithms
Biopolymers - chemistry
Computer Simulation
ELDOR
EPR
High-field EPR
Magnetic Resonance Spectroscopy - methods
Models, Chemical
Models, Molecular
Molecular Conformation
Orientation selection
Spin labeling
Spin Labels
Title Spin pair geometry revealed by high-field DEER in the presence of conformational distributions
URI https://dx.doi.org/10.1016/j.jmr.2006.11.012
https://www.ncbi.nlm.nih.gov/pubmed/17188008
https://www.proquest.com/docview/70327255
Volume 185
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