NMR of large protein systems: Solid state and dynamic nuclear polarization. Sascha Lange, Leibniz-Institut für Molekulare Pharmakologie (FMP)
|
|
- Jocelyn Ryan
- 6 years ago
- Views:
Transcription
1 NMR of large protein systems: Solid state and dynamic nuclear polarization Sascha Lange, Leibniz-Institut für Molekulare Pharmakologie (FMP)
2 The Aim of the Game solution NMR other methods solid state NMR x-ray crystallography electron microscopy % of structures deposited in protein data base (PDB) solution-state NMR requires rapid reorientation of soluble biomolecules X-ray crystallography requires high-quality single crystal solid-state NMR no need for large well-ordered crystals or highly-purified proteins works for immobilised proteins, no inherent limitation on complex size
3 Anisotropic effects in solid state NMR why is anisotropy difficult? liquids: rapid random tumbling averages anisotropic chemical shifts and couplings small lines, high signal! solids: no tumbling, interactions depend on orientation of the single molecules (anisotropic) very broad lines, low signal! anisotropic interactions lead to massive line broadening! 9/26/2014 3
4 Anisotropic effects in solid state NMR why is anisotropy difficult? anisotropy of heteronuclear dipolar interaction homonuclear dipolar interactions chemical shift anisotropy anisotropic interactions lead to massive line broadening! 9/26/2014 4
5 Anisotropic effects in solid state NMR heteronuclear dipolar interaction θ B 0 +B I B 0 +B S B 0 9/26/2014 5
6 Anisotropic effects in solid state NMR homonuclear dipolar interactions θ B 0 +B I B 0 +B I B 0 flip-flop-term 9/26/2014 6
7 Anisotropic effects in solid state NMR Chemical Shift Anisotropy B 0 +B local B 0 spherical symmetry non-axial symmetry axial symmetry 9/26/2014 7
8 Anisotropic effects in solid state NMR Chemical Shift Anisotropy B 0 +B local B 0 9/26/2014 8
9 Anisotropic effects in solid state NMR how to get rid of it? 3cos = = the magic angle! 9/26/2014 9
10 Anisotropic effects in solid state NMR how to get rid of it? 3cos = = the magic angle! 9/26/
11 Anisotropic effects in solid state NMR how to get rid of it? 54.7 = the magic angle! 9/26/
12 Magic Angle Spinning (MAS) how to get rid of it? but the information is NOT LOST FOEVER! (more information at 5pm by Barth-Jan van Rossum) 9/26/
13 Magic Angle Spinning (MAS) Maximum spinning frequency depends on rotor diameter some typical diameters: 4.0 mm 15 khz (1,400,000 x g) 3.2 mm 25 khz (2,700,000 x g) 2.5 mm 35 khz (3,500,000 x g) ( x g) Solid-state NMR is brute force
14 Magic Angle Spinning (MAS) no inherent limitation on complex size : What does it mean? SH3 domain 62 residues (~7 kda) OmpG 281 residues (~34 kda) type III secretion system 80 residues)
15 Dynamic Nuclear Polarization (DNP) low sensitivity is one of the biggest bottlenecks in solid state NMR E hυ0 N β kt kt N α = e = e E = γhb 0 2π sensitivity depends on: gyromagnetic ratio γ of the nuclei the higher the better (e.g. 1 H vs. 13 C) energy difference (i.e. magnetic field strength B 0 ) the stronger the better sample temperature the cooler the better
16 Dynamic Nuclear Polarization (DNP) Why is (solid state) NMR so insensitive Small net magnetic moment (polarization) aligned with B z N 0 N β α = e E kt = e hυ kt ΔE = hv = 5.6 x J 1H T h = Js k b T = 4.1 x J k b = JK -1 E hυ0 N β kt kt 10,000 1 H spins up (I z is aligned with B z ) N α = e = e 9,999 1 H spins down (I z is aligned against B z )
17 Dynamic Nuclear Polarization (DNP) DNP = transfer of the high electron polarization to nearby nuclei CP-Spectrum of SH3 with DNP without DNP 13 C-chemical shift K E hυ0 N β kt kt N α = e = e theoretical enhancement = γ e γ n e.g. for Protons: γ e γ 1H 660 9/26/
18 Dynamic Nuclear Polarization (DNP) The DNP-Spectrometer needed amount 5 nmol / 25 µl (0.2 mm)
19 Dynamic Nuclear Polarization (DNP) The DNP-Spectrometer Gyrotron produces 250 GHz microwaves Standard 400 MHz NMR magnet Cooling Cabinet controls sample temperature ~95K 3 pressurized exchangers within one dewar Gyrotron controller liquid N2 reservoir
20 DNP-Mechanism: 1. The Solid Effect δ < ω n Tritylradical 2ω n δ norm. 1 H-enhancemet DNP (-) microwave frequency
21 DNP-Mechanism: 1. The Solid Effect δ < ω n Tritylradical 2ω n δ norm. 1 H-enhancemet DNP (+) microwave frequency
22 DNP-Mechanism: 2. The Cross Effect ω e1 - ω e2 = ω n
23 DNP-Mechanism: 2. The Cross Effect ω n > ω n > δ δ norm. 1 H-enhancemet DNP (-) microwave frequency Irradiation with ω e1 leads to at the same time:
24 DNP-Mechanism: 2. The Cross Effect ω n > ω n > δ δ DNP (+) norm. 1 H-enhancemet microwave frequency Irradiation with ω e2 leads to at the same time:
25 DNP as a Tool for Structural Biology two main drawbacks of DNP inhomogeneous broadening due to cooling homogeneous broadening due to addition of radicals fast motion cooling
26 DNP as a Tool for Structural Biology Ala55 at low temperatures we can detect different conformers! Pro45 Ala55 Pro K 95 K 293 K 95 K Modell system: SH3 26
27 DNP as a Tool for Structural Biology and we can determine coalescence temperatures! Modell system: SH
28 DNP as a Tool for Structural Biology two main drawbacks of DNP inhomogeneous broadening due to cooling homogeneous broadening due to addition of radicals
29 DNP as a Tool for Structural Biology NP the radical is causing homogeneous line broadening TOTAPOL increases T 2 -Relaxation and therefore (homogeneous) line broadening TOTAPOL increases T 1 -Relaxation line width [ppm] TOTAPOL-conzentration [mm] TOTAPOL-conzentration [mm] e.g. broader lines, causing lower S/N e.g. shorter repetition times are possible (higher S/N per time unit)
30 DNP as a Tool for Structural Biology the radical is shortening effectively CP times NP TOTAPOL causes shorter effective CP times TOTAPOL-conzentration [mm] multi dimensional experiments difficult lower signal intensities
31 DNP as a Tool for Structural Biology NP TOTAPOL leads to a reduction of detectable nuclei: measured, normalized integral modell with r = 10 Å modell with r = 9 Å a i overlapping factor a i = V i V m i 1 j=1 D j V (i V m ) V r = V V bb V e r [TTT] [TOT] = TOTAPOL-concentration
32 DNP as a Tool for Structural Biology NP PRE effect creates holes in the cheese
33 DNP as a Tool for Structural Biology, ACh- Receptor Neurotoxin II (Naja naja oxiana; NOR1) on nachr (Torpedo californica) nicotinic AChR: ionotropic (ligand gated ion-channels) parasympathetic autonomic nervous system, neuromuscular junction
34 DNP as a Tool for Structural Biology, ACh- Receptor inactivation of TOTAPOL in close proximity Linden, Oschkinat et al. J. Am. Chem. Soc. 2011
35 DNP as a Tool for Structural Biology, ACh- Receptor inactivation of TOTAPOL close proximity can help
36 DNP as a Tool for Structural Biology, ACh- Receptor just 6% of the measurement time needed 10 days 10 hours
37 DNP as a Tool for Structural Biology, RNCs ic Nul with DNP we could investigate something small in something very big and nature-like 9/26/
38 DNP as a Tool for Structural Biology, RNCs Auflösung: ca. 7,3Å Bhushan, Beckmann et al. Nature Structural & Molecular Biology (2010) we investigated the folding state of a signal peptide within the ribosomal exit tunnel is there one specific conformation of the nascent chain? what is the helix content? 9/26/
39 DNP as a Tool for Structural Biology, RNCs the ribosome is times bigger compared to the NC 10 nmol nascent chain = ca. 37 µg 10 nmol ribosomes = ca. 25mg 9/26/
40 DNP as a Tool for Structural Biology, RNCs 9/26/
41 DNP as a Tool for Structural Biology, RNCs 9/26/
42 DNP as a Tool for Structural Biology, RNCs 1 MKKIWLALAG LVLAFSASAA FATPVWISQ AQGIRSGP 37 9/26/
43 DNP as a Tool for Structural Biology??? there are lot of barriers - line broadening is a very big issue (DNP is still blobby) - short CP times prevent multi-dimensional experiments - de novo assignements ar nearly impossible - cryo hardware is difficult to maintain and construction sites - new radicals with longer electron relaxation - deuteration of samples - sample preparation (glas matrix) - new systems (more suitable) - coupling of the radical 9/26/
Solid-state NMR and proteins : basic concepts (a pictorial introduction) Barth van Rossum,
Solid-state NMR and proteins : basic concepts (a pictorial introduction) Barth van Rossum, 16.02.2009 Solid-state and solution NMR spectroscopy have many things in common Several concepts have been/will
More informationMagic-Angle Spinning (MAS) drive bearing
Magic-Angle Spinning (MAS) magic-angle spinning is done pneumatically spinning frequency can be stabilized within a few Hz Magic-Angle Spinning (MAS) drive bearing Magic-Angle Spinning (MAS) Maximum spinning
More informationBMB/Bi/Ch 173 Winter 2018
BMB/Bi/Ch 173 Winter 2018 Homework Set 8.1 (100 Points) Assigned 2-27-18, due 3-6-18 by 10:30 a.m. TA: Rachael Kuintzle. Office hours: SFL 220, Friday 3/2 4:00-5:00pm and SFL 229, Monday 3/5 4:00-5:30pm.
More informationNMR in Medicine and Biology
NMR in Medicine and Biology http://en.wikipedia.org/wiki/nmr_spectroscopy MRI- Magnetic Resonance Imaging (water) In-vivo spectroscopy (metabolites) Solid-state t NMR (large structures) t Solution NMR
More informationCross Polarization 53 53
Cross Polarization 53 Why don t we normally detect protons in the solid-state BPTI Strong couplings between protons ( >20kHz) Homogeneous interaction Not readily averaged at moderate spinning speeds Rhodopsin
More informationSlow symmetric exchange
Slow symmetric exchange ϕ A k k B t A B There are three things you should notice compared with the Figure on the previous slide: 1) The lines are broader, 2) the intensities are reduced and 3) the peaks
More informationCenter for Sustainable Environmental Technologies, Iowa State University
NMR Characterization of Biochars By Catherine Brewer Center for Sustainable Environmental Technologies, Iowa State University Introduction Nuclear magnetic resonance spectroscopy (NMR) uses a very strong
More informationNMR in Structural Biology
NMR in Structural Biology Exercise session 2 1. a. List 3 NMR observables that report on structure. b. Also indicate whether the information they give is short/medium or long-range, or perhaps all three?
More informationELECTRON PARAMAGNETIC RESONANCE
ELECTRON PARAMAGNETIC RESONANCE = MAGNETIC RESONANCE TECHNIQUE FOR STUDYING PARAMAGNETIC SYSTEMS i.e. SYSTEMS WITH AT LEAST ONE UNPAIRED ELECTRON Examples of paramagnetic systems Transition-metal complexes
More informationBMB/Bi/Ch 173 Winter 2018
BMB/Bi/Ch 173 Winter 2018 Homework Set 8.1 (100 Points) Assigned 2-27-18, due 3-6-18 by 10:30 a.m. TA: Rachael Kuintzle. Office hours: SFL 220, Friday 3/2 4-5pm and SFL 229, Monday 3/5 4-5:30pm. 1. NMR
More informationBasic principles of multidimensional NMR in solution
Basic principles of multidimensional NMR in solution 19.03.2008 The program 2/93 General aspects Basic principles Parameters in NMR spectroscopy Multidimensional NMR-spectroscopy Protein structures NMR-spectra
More information4 Spin-echo, Spin-echo Double Resonance (SEDOR) and Rotational-echo Double Resonance (REDOR) applied on polymer blends
4 Spin-echo, Spin-echo ouble Resonance (SEOR and Rotational-echo ouble Resonance (REOR applied on polymer blends The next logical step after analyzing and concluding upon the results of proton transversal
More informationPrincipios Básicos de RMN en sólidos destinado a usuarios. Gustavo Monti. Fa.M.A.F. Universidad Nacional de Córdoba Argentina
Principios Básicos de RMN en sólidos destinado a usuarios Gustavo Monti Fa.M.A.F. Universidad Nacional de Córdoba Argentina CONTENIDOS MODULO 2: Alta resolución en sólidos para espines 1/2 Introducción
More informationNMR-spectroscopy of proteins in solution. Peter Schmieder
NMR-spectroscopy of proteins in solution Basic aspects of NMR-Spektroskopie Basic aspects of NMR-spectroscopy 3/84 Prerequisite for NMR-spectroscopy is a nuclear spin that can be thought of as a mixture
More informationDNP enhanced frequency-selective TEDOR experiments in bacteriorhodopsin
DNP enhanced frequency-selective TEDOR experiments in bacteriorhodopsin Journal of Magnetic Resonance 202 (2010) 9-13 Bajaj S. V., Mak-Jurkauskus, A. L., Belenky, M., Herzfeld, J. and Griffin, R. MR Seminar
More informationI690/B680 Structural Bioinformatics Spring Protein Structure Determination by NMR Spectroscopy
I690/B680 Structural Bioinformatics Spring 2006 Protein Structure Determination by NMR Spectroscopy Suggested Reading (1) Van Holde, Johnson, Ho. Principles of Physical Biochemistry, 2 nd Ed., Prentice
More informationIntroduction solution NMR
2 NMR journey Introduction solution NMR Alexandre Bonvin Bijvoet Center for Biomolecular Research with thanks to Dr. Klaartje Houben EMBO Global Exchange course, IHEP, Beijing April 28 - May 5, 20 3 Topics
More informationOptimum levels of exchangeable protons in perdeuterated proteins for proton detection in MAS solid-state NMR spectroscopy
J Biomol NMR (2010) 46:67 73 DOI 10.1007/s10858-009-9369-0 PERSPECTIVE Optimum levels of exchangeable protons in perdeuterated proteins for proton detection in MAS solid-state NMR spectroscopy Ümit Akbey
More informationSupporting Information
Supporting Information Dynamic Nuclear Polarization of Spherical Nanoparticles Ümit Akbey 1 *, Burcu Altin 2, Arne Linden 1, Serdar Özcelik 3, Michael Gradzielski 2, Hartmut Oschkinat 1 1 Leibniz-Institut
More informationInorganic Spectroscopic and Structural Methods
Inorganic Spectroscopic and Structural Methods Electromagnetic spectrum has enormous range of energies. Wide variety of techniques based on absorption of energy e.g. ESR and NMR: radiowaves (MHz) IR vibrations
More informationBasics of protein structure
Today: 1. Projects a. Requirements: i. Critical review of one paper ii. At least one computational result b. Noon, Dec. 3 rd written report and oral presentation are due; submit via email to bphys101@fas.harvard.edu
More informationDynamic Nuclear Polarization Magic Angle Spinning Nuclear Magnetic Resonance: Method Development and Applications
Dynamic Nuclear Polarization Magic Angle Spinning Nuclear Magnetic Resonance: Method Development and Applications Inaugural-Dissertation to obtain the academic degree Doctor rerum naturalium (Dr. rer.
More informationMagnetic Resonance Spectroscopy
INTRODUCTION TO Magnetic Resonance Spectroscopy ESR, NMR, NQR D. N. SATHYANARAYANA Formerly, Chairman Department of Inorganic and Physical Chemistry Indian Institute of Science, Bangalore % I.K. International
More informationChristopher Pavlik Bioanalytical Chemistry March 2, 2011
Nuclear Magnetic Resonance of Proteins Christopher Pavlik Bioanalytical Chemistry March 2, 2011 Nuclear Magnetic Resonance NMR Application of a magnetic field causes absorption of EM energy that induces
More informationNMR course at the FMP: NMR of organic compounds and small biomolecules - II -
NMR course at the FMP: NMR of organic compounds and small biomolecules - II - 16.03.2009 The program 2/76 CW vs. FT NMR What is a pulse? Vectormodel Water-flip-back 3/76 CW vs. FT CW vs. FT 4/76 Two methods
More information16.1 Introduction to NMR Spectroscopy. Spectroscopy. Spectroscopy. Spectroscopy. Spectroscopy. Spectroscopy 4/11/2013
What is spectroscopy? NUCLEAR MAGNETIC RESONANCE (NMR) spectroscopy may be the most powerful method of gaining structural information about organic compounds. NMR involves an interaction between electromagnetic
More informationNMR-spectroscopy in solution - an introduction. Peter Schmieder
NMR-spectroscopy in solution - an introduction 2/92 Advanced Bioanalytics NMR-Spectroscopy Introductory session (11:00 12:30) Basic aspects of NMR-spectroscopy NMR parameter Multidimensional NMR-spectroscopy
More informationNMR-spectroscopy. I: basics. Peter Schmieder
NMR-spectroscopy I: basics Why spectroscopy? 2/102 Why spectroscopy It is well established that all biological relevant processes take place via interactions of molecules, either small ones (metall ions,
More informationDipole Recoupling at High Spinning Frequencies. and. High Magnetic Fields
Dipole Recoupling at High Spinning Frequencies and High Magnetic Fields Stowe, Vermont January 2010 Francis Bitter Magnet Laboratory and Department of Chemistry Massachusetts Institute of Technology Outline
More informationProtein structure determination by solid-state NMR
Protein structure determination by solid-state NMR Birgit Habenstein Supervised by Anja Böckmann Solid state NMR proteinaceous targets Structural studies and structure determination at atomic level Membrane
More informationNMR Studies of Polyethylene: Towards the Organization of Semi Crystalline Polymers
NMR Studies of Polyethylene: Towards the Organization of Semi Crystalline Polymers Yefeng Yao, Robert Graf, Hans Wolfgang Spiess Max-Planck-Institute for Polymer Research, Mainz, Germany Leibniz Institut
More informationChapter 7. Nuclear Magnetic Resonance Spectroscopy
Chapter 7 Nuclear Magnetic Resonance Spectroscopy I. Introduction 1924, W. Pauli proposed that certain atomic nuclei have spin and magnetic moment and exposure to magnetic field would lead to energy level
More informationName: BCMB/CHEM 8190, BIOMOLECULAR NMR FINAL EXAM-5/5/10
Name: BCMB/CHEM 8190, BIOMOLECULAR NMR FINAL EXAM-5/5/10 Instructions: This is an open book, limited time, exam. You may use notes you have from class and any text book you find useful. You may also use
More informationQuantification of Dynamics in the Solid-State
Bernd Reif Quantification of Dynamics in the Solid-State Technische Universität München Helmholtz-Zentrum München Biomolecular Solid-State NMR Winter School Stowe, VT January 0-5, 206 Motivation. Solid
More informationDynamic Nuclear Polarization of Deuterated Proteins
Dynamic Nuclear Polarization of Deuterated Proteins The MIT Faculty has made this article openly available. Please share how this access benefits you. Your story matters. Citation As Published Publisher
More informationSupporting information for. Towards automatic protein backbone assignment using proton-detected 4D solid-state NMR data
Supporting information for Towards automatic protein backbone assignment using proton-detected 4D solid-state NMR data Shengqi Xiang 1, Veniamin Chevelkov 1,2, Stefan Becker 1, Adam Lange 1,2,3 * 1 Max
More informationSpin Relaxation and NOEs BCMB/CHEM 8190
Spin Relaxation and NOEs BCMB/CHEM 8190 T 1, T 2 (reminder), NOE T 1 is the time constant for longitudinal relaxation - the process of re-establishing the Boltzmann distribution of the energy level populations
More informationMagnetic Resonance Spectroscopy EPR and NMR
Magnetic Resonance Spectroscopy EPR and NMR A brief review of the relevant bits of quantum mechanics 1. Electrons have spin, - rotation of the charge about its axis generates a magnetic field at each electron.
More informationTheory and Applications of Residual Dipolar Couplings in Biomolecular NMR
Theory and Applications of Residual Dipolar Couplings in Biomolecular NMR Residual Dipolar Couplings (RDC s) Relatively new technique ~ 1996 Nico Tjandra, Ad Bax- NIH, Jim Prestegard, UGA Combination of
More informationStructurele Biologie NMR
MR journey Structurele Biologie MR 5 /3C 3 /65 MR & Structural biology course setup lectures - Sprangers R & Kay LE ature (27) basics of MR (Klaartje ouben: k.houben@uu.nl; 4/2) from peaks to data (ans
More informationDetermining Protein Structure BIBC 100
Determining Protein Structure BIBC 100 Determining Protein Structure X-Ray Diffraction Interactions of x-rays with electrons in molecules in a crystal NMR- Nuclear Magnetic Resonance Interactions of magnetic
More informationSample Shuttling Bio DNP in Liquids
EU Design Study Bio-DNP Sample Shuttling Bio DNP in Liquids Marcel Reese NMR based Structural Biology Max-Planck-Institute for Biophysical Chemistry, Göttingen Joint NMR-Life and Extend-NMR Meeting 2008,
More informationNMR, the vector model and the relaxation
NMR, the vector model and the relaxation Reading/Books: One and two dimensional NMR spectroscopy, VCH, Friebolin Spin Dynamics, Basics of NMR, Wiley, Levitt Molecular Quantum Mechanics, Oxford Univ. Press,
More information8.2 The Nuclear Overhauser Effect
8.2 The Nuclear Overhauser Effect Copyright Hans J. Reich 2016 All Rights Reserved University of Wisconsin An important consequence of DD relaxation is the Nuclear Overhauser Effect, which can be used
More informationH B. θ = 90 o. Lecture notes Part 4: Spin-Spin Coupling. θ θ
Lecture notes Part 4: Spin-Spin Coupling F. olger Försterling October 4, 2011 So far, spins were regarded spins isolated from each other. owever, the magnetic moment of nuclear spins also have effect on
More informationIntroduction to solution NMR. Alexandre Bonvin. The NMR research group. Bijvoet Center for Biomolecular Research
Introduction to solution NMR 1 Alexandre Bonvin Bijvoet Center for Biomolecular Research with thanks to Dr. Klaartje Houben Bente%Vestergaard% The NMR research group Prof. Marc Baldus Prof. Rolf Boelens
More informationInterpreting and evaluating biological NMR in the literature. Worksheet 1
Interpreting and evaluating biological NMR in the literature Worksheet 1 1D NMR spectra Application of RF pulses of specified lengths and frequencies can make certain nuclei detectable We can selectively
More informationBiochemistry 530 NMR Theory and Practice
Biochemistry 530 NMR Theory and Practice Gabriele Varani Department of Biochemistry and Department of Chemistry University of Washington Lecturer: Gabriele Varani Biochemistry and Chemistry Room J479 and
More informationAn introduction to Solid State NMR and its Interactions
An introduction to Solid State NMR and its Interactions From tensor to NMR spectra CECAM Tutorial September 9 Calculation of Solid-State NMR Parameters Using the GIPAW Method Thibault Charpentier - CEA
More information8 NMR Interactions: Dipolar Coupling
8 NMR Interactions: Dipolar Coupling 8.1 Hamiltonian As discussed in the first lecture, a nucleus with spin I 1/2 has a magnetic moment, µ, associated with it given by µ = γ L. (8.1) If two different nuclear
More informationBiochemistry 530 NMR Theory and Practice
Biochemistry 530 NMR Theory and Practice Gabriele Varani Department of Biochemistry and Department of Chemistry University of Washington 1D spectra contain structural information.. but is hard to extract:
More informationElectron Spin Resonance, Basic principle of NMR, Application of NMR in the study of Biomolecules, NMR imaging and in vivo NMR spectromicroscopy
Electron Spin Resonance, Basic principle of NMR, Application of NMR in the study of Biomolecules, NMR imaging and in vivo NMR spectromicroscopy Mitesh Shrestha Electron Spin Resonance Electron paramagnetic
More informationCopyright Mark Brandt, Ph.D A third method, cryogenic electron microscopy has seen increasing use over the past few years.
Structure Determination and Sequence Analysis The vast majority of the experimentally determined three-dimensional protein structures have been solved by one of two methods: X-ray diffraction and Nuclear
More informationThe Physical Basis of the NMR Experiment
The Physical Basis of the NMR Experiment 1 Interaction of Materials with Magnetic Fields F F S N S N Paramagnetism Diamagnetism 2 Microscopic View: Single Spins an electron has mass and charge in addition
More informationSolid-State NMR Structural Studies of Proteins Using Paramagnetic Probes
Solid-State NMR Structural Studies of Proteins Using Paramagnetic Probes Christopher Jaroniec Department of Chemistry & Biochemistry The Ohio State University Protein Structure by MAS Solid-State NMR D
More informationProtein dynamics from NMR Relaxation data
Protein dynamics from NMR Relaxation data Clubb 3/15/17 (S f2 ) ( e ) Nitrogen-15 relaxation ZZ-exchange R 1 = 1/T 1 Longitudinal relaxation (decay back to z-axis) R 2 = 1/T 2 Spin-spin relaxation (dephasing
More information6 NMR Interactions: Zeeman and CSA
6 NMR Interactions: Zeeman and CSA 6.1 Zeeman Interaction Up to this point, we have mentioned a number of NMR interactions - Zeeman, quadrupolar, dipolar - but we have not looked at the nature of these
More informationUses of Nuclear Magnetic Resonance (NMR) in Metal Hydrides and Deuterides. Mark S. Conradi
Uses of Nuclear Magnetic Resonance (NMR) in Metal Hydrides and Deuterides Mark S. Conradi Washington University Department of Physics St. Louis, MO 63130-4899 USA msc@physics.wustl.edu 1 Uses of Nuclear
More informationEffects of Chemical Exchange on NMR Spectra
Effects of Chemical Exchange on NMR Spectra Chemical exchange refers to any process in which a nucleus exchanges between two or more environments in which its NMR parameters (e.g. chemical shift, scalar
More informationOrientational degeneracy in the presence of one alignment tensor.
Orientational degeneracy in the presence of one alignment tensor. Rotation about the x, y and z axes can be performed in the aligned mode of the program to examine the four degenerate orientations of two
More informationPhysical Background Of Nuclear Magnetic Resonance Spectroscopy
Physical Background Of Nuclear Magnetic Resonance Spectroscopy Michael McClellan Spring 2009 Department of Physics and Physical Oceanography University of North Carolina Wilmington What is Spectroscopy?
More informationSolid-state NMR of spin > 1/2
Solid-state NMR of spin > 1/2 Nuclear spins with I > 1/2 possess an electrical quadrupole moment. Anisotropic Interactions Dipolar Interaction 1 H- 1 H, 1 H- 13 C: typically 50 khz Anisotropy of the chemical
More informationNMR NEWS June To find tutorials, links and more, visit our website
Department of Chemistry NMR Facilities Director: Dr. Carlos A. Steren NMR NEWS June 2014 To find tutorials, links and more, visit our website www.chem.utk.edu/facilities/nmr Computers and software updates
More informationProtein-nucleotide interactions detected by solid-state NMR
190 Å Protein-nucleotide interactions detected by solid-state NMR Dr. Thomas Wiegand CCPN Meeting 2017, Stirling 15/07/2017 120 Å HpDnaB ATP or ATP-analogues + ssdna? Laboratory of Physical Chemistry Group
More informationTimescales of Protein Dynamics
Timescales of Protein Dynamics From Henzler-Wildman and Kern, Nature 2007 Dynamics from NMR Show spies Amide Nitrogen Spies Report On Conformational Dynamics Amide Hydrogen Transverse Relaxation Ensemble
More informationNMR-spectroscopic investigation. of proteins in solution
Practical course Molekulare und zelluläre Signaltransduktion M-spectroscopic investigation of proteins in solution Monika Beerbaum, Peter Schmieder AG M-Spektroskopie Leibniz-Institut für molekulare Pharmakologie
More informationNuclear Magnetic Resonance
Nuclear Magnetic Resonance Lectures for CCB 538 James Aramini, PhD. CABM 014A jma@cabm.rutgers.edu J.A.! 04/21/14! April 21!!!!April 23!! April 28! Outline 1. Introduction / Spectroscopy Overview! 2. NMR
More informationNMR BMB 173 Lecture 16, February
NMR The Structural Biology Continuum Today s lecture: NMR Lots of slides adapted from Levitt, Spin Dynamics; Creighton, Proteins; And Andy Rawlinson There are three types of particles in the universe Quarks
More informationIntroduction to 1D and 2D NMR Spectroscopy (4) Vector Model and Relaxations
Introduction to 1D and 2D NMR Spectroscopy (4) Vector Model and Relaxations Lecturer: Weiguo Hu 7-1428 weiguoh@polysci.umass.edu October 2009 1 Approximate Description 1: Energy level model Magnetic field
More informationNMR = Nuclear Magnetic Resonance
NMR = Nuclear Magnetic Resonance NMR spectroscopy is the most powerful technique available to organic chemists for determining molecular structures. Looks at nuclei with odd mass numbers or odd number
More informationTimescales of Protein Dynamics
Timescales of Protein Dynamics From Henzler-Wildman and Kern, Nature 2007 Summary of 1D Experiment time domain data Fourier Transform (FT) frequency domain data or Transverse Relaxation Ensemble of Nuclear
More informationHigh deuteron polarization in polymer target materials
High deuteron polarization in polymer target materials 1,2 L.Wang, 1 W.Meyer, 1 Ch.Hess, 1 E.Radtke, 1 A.Berlin, 1 J.Herick, 1 G.Reicherz, 1 Institut of Experimental Physics AG I, Ruhr-University Bochum,
More informationIntroduction to Electron Paramagnetic Resonance Spectroscopy
Introduction to Electron Paramagnetic Resonance Spectroscopy Art van der Est, Department of Chemistry, Brock University St. Catharines, Ontario, Canada 1 EPR Spectroscopy EPR is magnetic resonance on unpaired
More informationBayro, 2011, JACS Intermolecular structure determination of amyloid fibrils with magic-angle spinning and dynamic nuclear polarization NMR
Bayro, 2011, JACS Intermolecular structure determination of amyloid fibrils with magic-angle spinning and dynamic nuclear polarization NMR Presented by: Daniel Droste 17.10.2013 Seminar Magnetische Resonanz
More informationProtein Structure Determination using NMR Spectroscopy. Cesar Trinidad
Protein Structure Determination using NMR Spectroscopy Cesar Trinidad Introduction Protein NMR Involves the analysis and calculation of data collected from multiple NMR techniques Utilizes Nuclear Magnetic
More informationChem8028(1314) - Spin Dynamics: Spin Interactions
Chem8028(1314) - Spin Dynamics: Spin Interactions Malcolm Levitt see also IK m106 1 Nuclear spin interactions (diamagnetic materials) 2 Chemical Shift 3 Direct dipole-dipole coupling 4 J-coupling 5 Nuclear
More informatione 2m e c I, (7.1) = g e β B I(I +1), (7.2) = erg/gauss. (7.3)
Chemistry 126 Molecular Spectra & Molecular Structure Week # 7 Electron Spin Resonance Spectroscopy, Supplement Like the hydrogen nucleus, an unpaired electron in a sample has a spin of I=1/2. The magnetic
More informationFerdowsi University of Mashhad
Spectroscopy in Inorganic Chemistry Nuclear Magnetic Resonance Spectroscopy spin deuterium 2 helium 3 The neutron has 2 quarks with a -e/3 charge and one quark with a +2e/3 charge resulting in a total
More information1) NMR is a method of chemical analysis. (Who uses NMR in this way?) 2) NMR is used as a method for medical imaging. (called MRI )
Uses of NMR: 1) NMR is a method of chemical analysis. (Who uses NMR in this way?) 2) NMR is used as a method for medical imaging. (called MRI ) 3) NMR is used as a method for determining of protein, DNA,
More informationLecture #6 (The NOE)
Lecture #6 (The OE) 2/18/15 Clubb Determining Protein tructures by MR: Measure thousands of shorter inter-hydrogen atom distances. Use these to restrain the structure of protein computationally. Distance
More informationSolid state and advanced NMR
Solid state and advanced NMR Dr. Magnus Wolf-Watz Department of Chemistry Umeå University magnus.wolf-watz@chem.umu.se NMR is useful for many things!!! Chemistry Structure of small molecules, chemical
More informationSolid state 13 Cand 1 H MAS NMR investigations of C 60 (ferrocene-d 10 ) 2 complex
Spectroscopy 17 (2003) 39 44 39 IOS Press Solid state 13 Cand 1 H MAS NMR investigations of C 60 (ferrocene-d 10 ) 2 complex E. Shabanova, K. Schaumburg and F.S. Kamounah CISMI, Department of Chemistry,
More informationQuímica Orgânica I. Nuclear Magnetic Resonance Spectroscopy (I) Ciências Farmacêuticas Bioquímica Química AFB QO I 2007/08 1 AFB QO I 2007/08 2
Química Orgânica I Ciências Farmacêuticas Bioquímica Química AFB QO I 2007/08 1 Nuclear Magnetic Resonance Spectroscopy (I) AFB QO I 2007/08 2 1 Adaptado de: Organic Chemistry, 6th Edition; L. G. Wade,
More informationNuclear Magnetic Resonance Spectroscopy Chem 4010/5326: Organic Spectroscopic Analysis Andrew Harned
Nuclear Magnetic Resonance Spectroscopy Chem 4010/5326: Organic Spectroscopic Analysis 2015 Andrew Harned NMR Spectroscopy NMR Spectroscopy All nuclei have a nuclear spin quantum number (I) I = 0, 1/2,
More informationNuclear magnetic resonance spectroscopy
nuclear spin transitions O Nuclear magnetic resonance spectroscopy 1 H, 13 C, 2-dimensional which transitions? wavelength and intensity; ppm what happens if we change the environment of the nucleus? substituent
More informationMeasuring Spin-Lattice Relaxation Time
WJP, PHY381 (2009) Wabash Journal of Physics v4.0, p.1 Measuring Spin-Lattice Relaxation Time L.W. Lupinski, R. Paudel, and M.J. Madsen Department of Physics, Wabash College, Crawfordsville, IN 47933 (Dated:
More information8.1 Relaxation in NMR Spectroscopy
8.1 Relaxation in NMR Spectroscopy Copyright ans J. Reich 2017 All Rights Reserved University of Wisconsin An understanding of relaxation processes is important for the proper measurement and interpretation
More informationTriple Resonance Experiments For Proteins
Triple Resonance Experiments For Proteins Limitations of homonuclear ( 1 H) experiments for proteins -the utility of homonuclear methods drops quickly with mass (~10 kda) -severe spectral degeneracy -decreased
More informationNMR Spectroscopy. Guangjin Hou
NMR Spectroscopy Guangjin Hou 22-04-2009 NMR History 1 H NMR spectra of water H NMR spectra of water (First NMR Spectra on Water, 1946) 1 H NMR spectra ethanol (First bservation of the Chemical Shift,
More informationBiochemistry 530 NMR Theory and Practice
Biochemistry 530 NMR Theory and Practice David Baker Autumn Quarter 2014 Slides Courtesy of Gabriele Varani Recommended NMR Textbooks Derome, A. E. (1987) Modern NMR Techniques for Chemistry Research,
More informationBCMB / CHEM 8190 Biomolecular NMR GRADUATE COURSE OFFERING IN NUCLEAR MAGNETIC RESONANCE
BCMB / CHEM 8190 Biomolecular NMR GRADUATE COURSE OFFERING IN NUCLEAR MAGNETIC RESONANCE "Biomolecular Nuclear Magnetic Resonance" is a course intended for all graduate students with an interest in applications
More informationK ex. Conformational equilibrium. equilibrium K B
Effects of Chemical Exchange on NMR Spectra Chemical exchange refers to any yprocess in which a nucleus exchanges between two or more environments in which its NMR parameters (e.g. chemical shift, scalar
More informationLecture 6: Physical Methods II. UV Vis (electronic spectroscopy) Electron Spin Resonance Mossbauer Spectroscopy
Lecture 6: Physical Methods II UV Vis (electronic spectroscopy) Electron Spin Resonance Mossbauer Spectroscopy Physical Methods used in bioinorganic chemistry X ray crystallography X ray absorption (XAS)
More informationNMR Spectroscopy Laboratory Experiment Introduction. 2. Theory
1. Introduction 64-311 Laboratory Experiment 11 NMR Spectroscopy Nuclear Magnetic Resonance (NMR) spectroscopy is a powerful and theoretically complex analytical tool. This experiment will introduce to
More informationIntroduction to biomolecular NMR spectroscopy
Oct 2002 Introduction to biomolecular NMR spectroscopy Michael Sattler, Structural & Computational Biology EMBL Heidelberg Contents Introduction...2 History... 3 Methodological developments for structure
More informationTo Deuterate Your Proteins or Not to Deuterate? That is the Question. by Bibhuti Das, Paul Ellis, and F. David Doty
To Deuterate Your Proteins or Not to Deuterate? That is the Question. by Bibhuti Das, Paul Ellis, and F. David Doty High-resolution inverse 1 H detection in solid-state (ss) NMR spectroscopy is rapidly
More information16.1 Introduction to NMR. Spectroscopy
16.1 Introduction to NMR What is spectroscopy? Spectroscopy NUCLEAR MAGNETIC RESNANCE (NMR) spectroscopy may be the most powerful method of gaining structural information about organic compounds. NMR involves
More informationNMR journey. Introduction to solution NMR. Alexandre Bonvin. Topics. Why use NMR...? Bijvoet Center for Biomolecular Research
2 NMR journey Introduction to solution NMR Alexandre Bonvin Bijvoet Center for Biomolecular Research with thanks to Dr. Klaartje Houben EMBO Global Exchange course, CCMB, Hyderabad, India November 29th
More informationNMRis the most valuable spectroscopic technique for organic chemists because it maps the carbon-hydrogen framework of a molecule.
Chapter 13: Nuclear magnetic resonance spectroscopy NMRis the most valuable spectroscopic technique for organic chemists because it maps the carbon-hydrogen framework of a molecule. 13.2 The nature of
More informationBiophysical Chemistry: NMR Spectroscopy
Relaxation & Multidimensional Spectrocopy Vrije Universiteit Brussel 9th December 2011 Outline 1 Relaxation 2 Principles 3 Outline 1 Relaxation 2 Principles 3 Establishment of Thermal Equilibrium As previously
More information