Quantification of Dynamics in the Solid-State

Size: px
Start display at page:

Download "Quantification of Dynamics in the Solid-State"

Transcription

1 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 samples are more susceptible to local structural fluctuations Is there dynamics in the solid-state? How does local dynamics compare between solution- and solid-state? How can we quantify dynamics in the solid-state? Solution-state: Relaxation is due to molecular tumbling τ c Solid-state: Relaxation is due to local structural fluctuations R ( 5 N) = d 2 [ ( ) + 3J ( ω N ) + 6J 2 ( ω H + ω N )] J 0 ω H ω N J(ω) = S 2 τ R + ω 2 τ + S 2 2 ( F ) R + ω 2 τ + S F ( S S ) F + ω 2 2 τ S τ F τ S ( ) 5 c 2 J ω N In solids In solution

2 Measurement of 5 N-T Solid-State Solution Chevelkov et al. JCP (2008) Motivation 2. Temperature dependence of H, 5 N correlations in α-sh3 RT loop N-Src loop distal loop N- and C- terminus

3 In solution, things get worse with larger molecular weight τ c Observables for the quantification of dynamics - INEPT vs CP based experiments - T Spin-Lattice Relaxation - T2 Spin-Spin Relaxation - Order Parameter measurements - CPMG / Rρ Relaxation Dispersion - Heteronuclear NOE - off- magic angle spinning trivial, but very useful spin density? affected by spin density classical observable similar to CP/INEPT, quantitative rotating methyl groups act as sinks for relaxation low resolution! " "!!? "

4 What determines T 2 in the solid-state? In solution-state: Overall tumbling, τ C (local fluctuations, chemical exchange) τ c In the solid-state: LW( H, 3 24 khz, 600 MHz) > 7 Hz, 4 Hz ) Acquisition time - Insufficient decoupling power - Insufficient MAS frequencies - Probe design Not an issue in deuterated samples 2) Shimming 3) Crystal imperfections LW (adamantane) 2 Hz T 2 * = T 2 4) Local dynamics? Quantification of Dynamics Relaxation of longitudinal 5 N magnetization: R ( 5 N) = d 2 [ ( ) + 3J ( ω N ) + 6J 2 ( ω H + ω N )] J 0 ω H ω N ( ) 5 c 2 J ω N Definition of the spectral density function J(ω): J m # ( ) = dτ m ω m ω m # t 0 [ Y α 2,m ( Ω(0) ), Y β 2, m $ ( Ω(τ) )] [ ] (m, m # C ) α,β (τ) exp i( ω m ω m # )τ τ C In solution: (m, m # C ) α,α (τ) = exp( τ /τ C ) In general: ( ) τ F ( ) 2 J(ω) = S F + ω 2 τ + S F S S F + ω 2 2 τ S τ S S: order parameter τ: correlation time τ S /τ F : Slow and fast motional time scale

5 Quantification of Dynamics in the Solid-State In Solution-State NMR, relaxation is determined by the tumbling of the molecule in water τ S R ( 5 N) = d 2 [ ( ) + 3J ( ω N ) + 6J 2 ( ω H + ω N )] J 0 ω H ω N ( ) 5 c 2 J ω N ( ) τ F ( ) 2 J(ω) = S F + ω 2 τ + S F S S F + ω 2 2 τ S τ S In solution In solids In Solid-State NMR, relaxation is determined by local structural fluctuations only τ F. Measurement of 5 N-T in the solid-state R ( 5 N) = d 2 [ ( ) + 3J ( ω N ) + 6J 2 ( ω H + ω N )] J 0 ω H ω N ( ) 5 c 2 J ω N Chevelkov et al. J Chem Phys (2008)

6 2. Can we learn something on J(0) in the solid-state? ) Coherent, Static effect (CSA-dipole correlation) [MAS dependent] 2) Incoherent, Dynamic effect due to Dipole-CSA cross-correlated relaxation [MAS independent] Chevelkov et al. JACS (2007) Composition of Multiplet Intensities ) Static effect (CSA-dipole correlation) [MAS dependent] 0 *# δ N N z + D HN H z N z = δ N + D HN % 2 + H & # z ( % $ ' 2 H &- 3, z (/ $ '. 5 N z [ ] [ ] 0 8 = δ N + D HN H α 28 δ N D HN H β H β Center band J NH st spinning side band H α

7 Composition of Multiplet Intensities ) Static effect (CSA-dipole correlation) [MAS dependent] 0 *# δ N N z + D HN H z N z = δ N + D HN % 2 + H & z $ ' ( # % $ 2 H &- 3, ( + z / 4 2 '. 5 N z [ ] [ ] 0 8 = δ N + D HN H α 28 δ N D HN H β H β Center band J NH st spinning side band H α Composition of Multiplet Intensities ) Static effect (CSA-dipole correlation) [MAS dependent] 0 *# δ N N z + D HN H z N z = δ N + D HN % 2 + H & # z ( % $ ' 2 H &- 3, z (/ $ '. 5 N z [ ] [ ] 0 8 = δ N + D HN H α 28 δ N D HN H β H β Center band J NH st spinning side band H α

8 Composition of Multiplet Intensities ) Static effect (CSA-dipole correlation) [MAS dependent] 0 *# δ N N z + D HN H z N z = δ N + D HN % 2 + H & z $ ' ( # % $ 2 H &- 3, ( + z / 4 2 '. 5 N z [ ] [ ] 0 8 = δ N + D HN H α 28 δ N D HN H β H β Center band J NH st spinning side band H α Composition of Multiplet Intensities 2) Dynamic effect due to Dipole-CSA cross-correlated relaxation [MAS independent] c Γ NH,N γ Hγ N γ 3 N B 0 δ N (3cos 2 β )*τ c r NH J NH 5 N Is there a contribution due to dynamics? Chevelkov et al. Mag Res Chem 45 S56-60 (2007) Skrynnikov Mag Res Chem 45 S6-73 (2007)

9 N-H α /N-H β Differential Line Broadening due to Dynamics MAS = 3 khz = const J NH Columns along 5 N Broad Lines in traditional solid-state NMR experiments T 2 decay of 5 N-Hα/β allows to access the timescale of local dynamics η CSA / DD = & 2Δ ln I β ) ( ' I α + = dc { * 5 4J (0) + 3J (ω ) 0 N }P 2 (cosθ) Chevelkov et al. MRC 45 S56-60 (2007)

10 Differential T 2 decay of α/β multiplet components T eff = 2 C; MAS = 24 khz η CSA / DD = & 2Δ ln I β ) ( ' I α + = dc { * 5 4J 0(0) + 3J (ω N )}P 2 (cosθ) Chevelkov et al. MRC 45 S56 (2007) 3. H- 5 N dipolar coupling measurements yield Order Parameters Simulation Parameters: MAS = 20 khz Ideal condition: ω RF ( H)/2π = 56 khz ω RF ( 5 N)/2π = 76 khz Δω RF ( 5 N)/2π = -6 khz Wu and Zilm, JMR A 04, 54 (993) Dvinskikh, Zimmermann, Maliniak and Sandstrøm, JCP 22, (2005) Chevelkov, Fink, Reif, J Am Chem Soc 3, 408 (2009)

11 Experimental CPPI spectra for α-spectrin SH3 khz Error estimation in the determination of H, 5 N dipolar couplings (K8) LB = Line Broadening of the Exponential Apodization; D app = apparent dipolar splitting; D HN = true dipolar coupling (without scaling factor of the pulse sequence)

12 H, 5 N dipolar couplings in α-spectrin SH3 H-bond acceptor γ D NH = µ H γ N! 0 3 r NH.035 Å = Hz.045 Å = Hz.055 Å = Hz Are variations in the size of the H N - 5 N dipolar coupling due to a variation in the H N -N bond length or due to dynamics? Correlation between the scalar coupling across a hydrogen bond 3h J NC and the H N isotropic chemical shift from Cordier and Grzesiek, JACS 2 60 (999)

13 Correlation between the H N, 5 N dipolar couplings and the H N isotropic chemical shift γ D NH = µ H γ N! 0 3 r NH However: N-H bond length should be increased in a H-Bond Mobility Increased dynamics for weak hydrogen bonds No effect of H-bonding on the N-H bond length Alternatively: Order Parameters via REDOR type experiments Schanda P, Meier BH, Ernst M Accurate measurement of one-bond H-X heteronuclear dipolar couplings in MAS solid-state NMR. J. Magn. Reson. 20: (20).

14 Order Parameters via REDOR type experiments Schanda P, Huber M, Boisbouvier J, Meier BH, Ernst M. Solid-State NMR Measurements of Asymmetric Dipolar Couplings Provide Insight into Protein Side-Chain Motion. Angew. Chem. Int. Ed. 50: (202) Model-free Analysis to decribe Motion in the Solid-State Let's assume that you have slow and fast motions in your protein ( ) J(ω ) = S F 2 τ F ( ) τ S +ω 2 τ + S F S S F +ω 2 2 τ S There are 4 unknown parameters S 2 S, S2 F, τ S and τ F What can we measure? H, 5 N dipole 5 N CSA cross-correlated relaxation " 5 N-T 2 " H, 5 N dipolar couplings S 2 F S2 S 5 N 2 fields

15 Rmsd minimization of S 2 S, S2 F, τ F and τ S Q # & # rmsd =, % R theo exp (,i R exp,i )( + % $ R.- i,i ' $ % 2 / 2 & ( η exp ηtheo η exp )( / - 0 '( - Data used for fitting: 5 N-T (900 MHz) 5 N-T (600 MHz) Data used for fitting: 5 N-T (900 MHz) 5 N-T (600 MHz) η ( 5 N-CSA / H- 5 N) S 2 S S2 F = 0.776; S2 S = 0.92 τ F = 26 ps Rmsd minimization of S 2 S, S2 F, τ F and τ S D # & # rmsd =, % R theo exp (,i R exp,i )( + % $ R.- i,i ' $ % 2 / 2 & ( η exp ηtheo η exp )( / - 0 '( - Data used for fitting: 5 N-T (900 MHz) 5 N-T (600 MHz) Data used for fitting: 5 N-T (900 MHz) 5 N-T (600 MHz) η ( 5 N-CSA / H- 5 N) S 2 S S2 F = 0.349; S2 S = τ F = 3.9 ns

16 Order Parameter and τ S in α-spectrin SH3 τ S and τ F in α-spectrin SH3

17 τ S and τ F in α-spectrin SH3 Is TROSY beneficial for solid-state NMR?

18 Observation : INEPT based experiments allow to detect residues in mobile regions Linser et al., J. Am. Chem. Soc. (200) Observation 2: Regions which are not detectable in CP experiments undergo a ns-µs time scale dynamics Quantification of η CSA/DD using INEPT based experiments Linser et al., J. Am. Chem. Soc. (200)

19 TROSY experiments are beneficial in the solid-state for regions undergoing slow dynamics Linser et al., J. Am. Chem. Soc. (200) Intensities in 2D-HSQC/TROSY and 3D-HNCO/TROSY-HNCO Using TROSY experiments, the S/N in dynamic regions of the protein can be increased by x2-5

20 4. heteronuclear NOE measurements: Additional dynamics information in the solid-state Lopez et al. JBNMR (204) H, 3 C heteronuclear NOE measurements

21 H, 5 N heteronuclear NOE measurements Deuteration is required to avoid spin diffusion 5 N R rates in a protonated and deuterated SH3 sample 2 H R rates in Solids and Solution J. Am. Chem. Soc (2006) J. Chem. Phys (2008)

22 Aliphatic protons (RAP, Reduction of Adjoining Protonation) 5 NH 4 Cl [ 2 H, 3 C]-glucose 5-30 % H 2 O (95-70 % D 2 O) Asami et al., J. Am. Chem. Soc. 200; Asami et al., Acc. Chem. Res. 203 Experimental 3C T decay curves are bi-exponential (25% SH3 RAP sample, 24 khz MAS). Orientation dependence yields frequency dependent R rates Mono-exponential initial-rate approximation (Torchia) 2. Spin Diffusion: efficient magnetization transfer to methyls which act as relaxation sinks

23 Dilution of the proton AND carbon spin system H, 3 C correlations of α-sh3: RAP-glucose vs. RAP 2-glycerol 25% RAP-glucose (25 % H2O / 75 % D2O, 2 H, 3 C glucose in M9) 0% RAP-glycerol (0 % H2O / 90 % D2O, [u- 2 H, 2-3 C]-glycerole in M9) improved resolution (no evolution of J couplings) simplified spectra: e.g. no Cα labeling for R, Q, E, L, P no methyl labeling for A, I-γ2, V, L, M 3 Cα T Decay Curves 25% RAP-glucose, 24 khz MAS 0% RAP-glycerol, 24 khz MAS 0% RAP-glycerol, 50 khz MAS (mono-exponential)

24 3 Cα T in α-spectrin SH3 and MD derived order parameters 5. Protein Side Chain Dynamics 3D 2 H- 3 C- 3 C correlation using 3 C- 3 C RFDR mixing and 2 H- 3 C CP applied to α-spectrin SH3 Hologne et al. (2005) JACS 27, 208

25 3D- 2 H, 3 C, 3 C Correlation of α-spectrin SH3 2 H Pake Pattern for Valine-CD 3 in α-spectrin SH3 Conformational exchange is directly reflected in the anisotropy δ and the asymmetry η of the 2 H pake pattern (τ c < / 52 khz)

26 Motional Model for the Side Chain Dynamics of Val-23 Best fit: 2-site jump, jump angle 40 (Center band intensities are not well reproduced in the simulations) 2 H β Pake Pattern for different Valines in α-spectrin SH3 Lower intensities for V23 indicates motion (τ c < /60 khz )

27 But,... there are many methyls indicating motion and no second conformation is visible in the X-ray structure η=0 η= δ η=0 Comparison of X-Ray Analysis at 00K and RT Ile-30, 00K Ile-30, RT Resolution RT:.90 Å; 00 K:.49 Å Crystal dimensions: RT: 34.5 Å, 42.5 Å, 50.8 Å 00 K: 33.6 Å, 42.3 Å, 49.6 Å B-factors (Å 2 ) main chain RT: 26.9 ; 00K: 3.9 side chain RT: 29.6 ; 00K: 7. whole RT: 28.3 ; 00K: 5.6

28 Acknowledgement Vipin Agarwal Sam Asami Veniamin Chevelkov Rasmus Linser Purdue University Nikolai Skrynnikov

Labelling strategies in the NMR structure determination of larger proteins

Labelling strategies in the NMR structure determination of larger proteins Labelling strategies in the NMR structure determination of larger proteins - Difficulties of studying larger proteins - The effect of deuteration on spectral complexity and relaxation rates - NMR expts

More information

Model-Free Approach to Internal Motions in Proteins

Model-Free Approach to Internal Motions in Proteins Model-Free Approach to Internal Motions in Proteins Lipari & Szabo, JACS 104, 4546 (1982) Palmer AG. Ann. Rev. Biophys. Biomol. Struc., 30, 129-155 (2001) Palmer AG, Kroenke CD, Loria JP, Meth. Enzymol.

More information

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, 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 information

T 1, T 2, NOE (reminder)

T 1, T 2, NOE (reminder) T 1, T 2, NOE (reminder) T 1 is the time constant for longitudinal relaxation - the process of re-establishing the Boltzmann distribution of the energy level populations of the system following perturbation

More information

Triple Resonance Experiments For Proteins

Triple 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 information

Introduction to Relaxation Theory James Keeler

Introduction to Relaxation Theory James Keeler EUROMAR Zürich, 24 Introduction to Relaxation Theory James Keeler University of Cambridge Department of Chemistry What is relaxation? Why might it be interesting? relaxation is the process which drives

More information

Protein dynamics from NMR Relaxation data

Protein 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 information

Timescales of Protein Dynamics

Timescales 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 information

Supplementary Information Access to side- chain carbon information in deuterated solids under ultra- fast MAS through non- rotor- synchronized mixing

Supplementary Information Access to side- chain carbon information in deuterated solids under ultra- fast MAS through non- rotor- synchronized mixing Electronic Supplementary Material (ESI) for ChemComm. This journal is The Royal Society of Chemistry Supplementary Information Access to side- chain carbon information in deuterated solids under ultra-

More information

Topics in SSNMR and Dynamics of Proteins: Consequences of Intermediate Exchange

Topics in SSNMR and Dynamics of Proteins: Consequences of Intermediate Exchange Topics in SSNMR and Dynamics of Proteins: Consequences of Intermediate Exchange A McDermott, Columbia University Winter School in Biomolecular NMR, Stowe VT January 20-23 2008 Effects on NMR Spectra: Local,

More information

Cross Polarization 53 53

Cross 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 information

NMR journey. Introduction to solution NMR. Alexandre Bonvin. Topics. Why use NMR...? Bijvoet Center for Biomolecular Research

NMR 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 information

Timescales of Protein Dynamics

Timescales 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 information

NMR in Structural Biology

NMR 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 information

Spin Relaxation and NOEs BCMB/CHEM 8190

Spin 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 information

Dipole Recoupling at High Spinning Frequencies. and. High Magnetic Fields

Dipole 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 information

PROTEIN NMR SPECTROSCOPY

PROTEIN NMR SPECTROSCOPY List of Figures List of Tables xvii xxvi 1. NMR SPECTROSCOPY 1 1.1 Introduction to NMR Spectroscopy 2 1.2 One Dimensional NMR Spectroscopy 3 1.2.1 Classical Description of NMR Spectroscopy 3 1.2.2 Nuclear

More information

Biophysical Chemistry: NMR Spectroscopy

Biophysical 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

PRACTICAL ASPECTS OF NMR RELAXATION STUDIES OF BIOMOLECULAR DYNAMICS

PRACTICAL ASPECTS OF NMR RELAXATION STUDIES OF BIOMOLECULAR DYNAMICS PRACTICAL ASPECTS OF MR RELAXATIO STUDIES OF BIOMOLECULAR DYAMICS Further reading: Can be downloaded from my web page Korzhnev D.E., Billeter M., Arseniev A.S., and Orekhov V. Y., MR Studies of Brownian

More information

Longitudinal-relaxation enhanced fast-pulsing techniques: New tools for biomolecular NMR spectroscopy

Longitudinal-relaxation enhanced fast-pulsing techniques: New tools for biomolecular NMR spectroscopy Longitudinal-relaxation enhanced fast-pulsing techniques: New tools for biomolecular NMR spectroscopy Bernhard Brutscher Laboratoire de Résonance Magnétique Nucléaire Institut de Biologie Structurale -

More information

Optimum levels of exchangeable protons in perdeuterated proteins for proton detection in MAS solid-state NMR spectroscopy

Optimum 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 information

NMR Relaxation and Molecular Dynamics

NMR Relaxation and Molecular Dynamics Ecole RMN Cargese Mars 2008 NMR Relaxation and Molecular Dynamics Martin Blackledge IBS Grenoble Carine van Heijenoort ICSN, CNRS Gif-sur-Yvette Solution NMR Timescales for Biomolecular Motion ps ns µs

More information

Spin-spin coupling I Ravinder Reddy

Spin-spin coupling I Ravinder Reddy Spin-spin coupling I Ravinder Reddy Spin-interactions External interactions Magnetic field Bo, RF field B1 Internal Interactions Molecular motions Exchange Chemical shifts J-coupling Spin Diffusion Dipolar

More information

Introduction solution NMR

Introduction 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 information

NMR-spectroscopy of proteins in solution. Peter Schmieder

NMR-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 information

Slow symmetric exchange

Slow 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 information

Deuteration: Structural Studies of Larger Proteins

Deuteration: Structural Studies of Larger Proteins Deuteration: Structural Studies of Larger Proteins Problems with larger proteins Impact of deuteration on relaxation rates Approaches to structure determination Practical aspects of producing deuterated

More information

Magic-Angle Spinning (MAS) drive bearing

Magic-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 information

PRACTICAL ASPECTS OF NMR RELAXATION STUDIES OF BIOMOLECULAR DYNAMICS

PRACTICAL ASPECTS OF NMR RELAXATION STUDIES OF BIOMOLECULAR DYNAMICS PRACTICAL ASPECTS OF MR RELAXATIO STUDIES OF BIOMOLECULAR DYAMICS Further reading: (Can be downloaded from my web page Korzhnev D.E., Billeter M., Arseniev A.S., and Orekhov V. Y., MR Studies of Brownian

More information

Supporting 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 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 information

Spectroscopy of Polymers

Spectroscopy of Polymers Spectroscopy of Polymers Jack L. Koenig Case Western Reserve University WOMACS Professional Reference Book American Chemical Society, Washington, DC 1992 Contents Preface m xiii Theory of Polymer Characterization

More information

8.2 The Nuclear Overhauser Effect

8.2 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 information

Advanced Quadrupolar NMR. Sharon Ashbrook School of Chemistry, University of St Andrews

Advanced Quadrupolar NMR. Sharon Ashbrook School of Chemistry, University of St Andrews Advanced Quadrupolar NMR Sharon Ashbrook School of Chemistry, University of St Andrews Quadrupolar nuclei: revision single crystal powder ST 500 khz ST ω 0 MAS 1 khz 5 khz second-order broadening Example:

More information

BMB/Bi/Ch 173 Winter 2018

BMB/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 information

Effects of Chemical Exchange on NMR Spectra

Effects 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 information

NMR Studies of Polyethylene: Towards the Organization of Semi Crystalline Polymers

NMR 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 information

Errors in the Measurement of Cross-Correlated Relaxation Rates and How to Avoid Them

Errors in the Measurement of Cross-Correlated Relaxation Rates and How to Avoid Them Journal of Magnetic Resonance 44, 8 87 () doi:.6/jmre..56, available online at http://www.idealibrary.com on Errors in the Measurement of Cross-Correlated Relaxation Rates and How to Avoid Them T. Carlomagno

More information

Introduction to solution NMR. Alexandre Bonvin. The NMR research group. Bijvoet Center for Biomolecular Research

Introduction 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 information

K ex. Conformational equilibrium. equilibrium K B

K 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 information

Effects of Chemical Exchange on NMR Spectra

Effects 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 information

Probing Hydrogen Bonding by Solid-State NMR. Steven P. Brown

Probing Hydrogen Bonding by Solid-State NMR. Steven P. Brown Probing ydrogen Bonding by Solid-State M Steven P. Brown Solution-State M: Isotropic Interactions Fast isotropic tumbling of the molecules averages to zero all anisotropic broadening Chemical Shift Differentiation

More information

Supporting Information

Supporting Information Supporting Information Boehr et al. 10.1073/pnas.0914163107 SI Text Materials and Methods. R 2 relaxation dispersion experiments. 15 NR 2 relaxation dispersion data measured at 1 H Larmor frequencies of

More information

Biochemistry 530 NMR Theory and Practice. Gabriele Varani Department of Biochemistry and Department of Chemistry University of Washington

Biochemistry 530 NMR Theory and Practice. Gabriele Varani Department of Biochemistry and Department of Chemistry University of Washington 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 information

Lecture #6 Chemical Exchange

Lecture #6 Chemical Exchange Lecture #6 Chemical Exchange Topics Introduction Effects on longitudinal magnetization Effects on transverse magnetization Examples Handouts and Reading assignments Kowalewski, Chapter 13 Levitt, sections

More information

Name: BCMB/CHEM 8190, BIOMOLECULAR NMR FINAL EXAM-5/5/10

Name: 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 information

Chem8028(1314) - Spin Dynamics: Spin Interactions

Chem8028(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 information

SUPPLEMENTARY INFORMATION

SUPPLEMENTARY INFORMATION DOI: 10.1038/NCHEM.1299 Protein fold determined by paramagnetic magic-angle spinning solid-state NMR spectroscopy Ishita Sengupta 1, Philippe S. Nadaud 1, Jonathan J. Helmus 1, Charles D. Schwieters 2

More information

NMR Spectroscopy: A Quantum Phenomena

NMR Spectroscopy: A Quantum Phenomena NMR Spectroscopy: A Quantum Phenomena Pascale Legault Département de Biochimie Université de Montréal Outline 1) Energy Diagrams and Vector Diagrams 2) Simple 1D Spectra 3) Beyond Simple 1D Spectra 4)

More information

8 NMR Interactions: Dipolar Coupling

8 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 information

General NMR basics. Solid State NMR workshop 2011: An introduction to Solid State NMR spectroscopy. # nuclei

General NMR basics. Solid State NMR workshop 2011: An introduction to Solid State NMR spectroscopy. # nuclei : An introduction to Solid State NMR spectroscopy Dr. Susanne Causemann (Solid State NMR specialist/ researcher) Interaction between nuclear spins and applied magnetic fields B 0 application of a static

More information

Topics in SSNMR and Conformational Dynamics of Biopolymers: Consequences of Intermediate Exchange

Topics in SSNMR and Conformational Dynamics of Biopolymers: Consequences of Intermediate Exchange Topics in SSNMR and Conformational Dynamics of Biopolymers: Consequences of Intermediate Exchange A McDermott US Canada Winter School in Biomolecular SSNMR Stowe, VT January 24-29 2010 Effects on NMR Spectra:

More information

Introduction to 1D and 2D NMR Spectroscopy (4) Vector Model and Relaxations

Introduction 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 information

Spin Dynamics Basics of Nuclear Magnetic Resonance. Malcolm H. Levitt

Spin Dynamics Basics of Nuclear Magnetic Resonance. Malcolm H. Levitt Spin Dynamics Basics of Nuclear Magnetic Resonance Second edition Malcolm H. Levitt The University of Southampton, UK John Wiley &. Sons, Ltd Preface xxi Preface to the First Edition xxiii Introduction

More information

Concepts on protein triple resonance experiments

Concepts on protein triple resonance experiments 2005 NMR User Training Course National Program for Genomic Medicine igh-field NMR Core Facility, The Genomic Research Center, Academia Sinica 03/30/2005 Course andout Concepts on protein triple resonance

More information

Magnetic Resonance Spectroscopy

Magnetic 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 information

- Basic understandings: - Mapping interactions:

- Basic understandings: - Mapping interactions: NMR-lecture April 6th, 2009, FMP Berlin Outline: Christian Freund - Basic understandings: Relaxation Chemical exchange - Mapping interactions: -Chemical shift mapping (fast exchange) Linewidth analysis

More information

Chapter 7. Nuclear Magnetic Resonance Spectroscopy

Chapter 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 information

NMR Dynamics and Relaxation

NMR Dynamics and Relaxation NMR Dynamics and Relaxation Günter Hempel MLU Halle, Institut für Physik, FG Festkörper-NMR 1 Introduction: Relaxation Two basic magnetic relaxation processes: Longitudinal relaxation: T 1 Relaxation Return

More information

Polarised Nucleon Targets for Europe, 2nd meeting, Bochum 2005

Polarised Nucleon Targets for Europe, 2nd meeting, Bochum 2005 Polarised Nucleon Targets for Europe, nd meeting, Bochum Temperature dependence of nuclear spin-lattice relaxations in liquid ethanol with dissolved TEMPO radicals H. Štěpánková, J. Englich, J. Kohout,

More information

BMB/Bi/Ch 173 Winter 2018

BMB/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 information

Biophysical Journal, Volume 96. Supporting Material

Biophysical Journal, Volume 96. Supporting Material Biophysical Journal, Volume 96 Supporting Material NMR dynamics of PSE-4 β-lactamase: an interplay of ps-ns order and μs-ms motions in the active site Sébastien Morin and Stéphane M. Gagné NMR dynamics

More information

Practical Manual. General outline to use the structural information obtained from molecular alignment

Practical Manual. General outline to use the structural information obtained from molecular alignment Practical Manual General outline to use the structural information obtained from molecular alignment 1. In order to use the information one needs to know the direction and the size of the tensor (susceptibility,

More information

4 Spin-echo, Spin-echo Double Resonance (SEDOR) and Rotational-echo Double Resonance (REDOR) applied on polymer blends

4 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 information

QENS in the Energy Domain: Backscattering and Time-of

QENS in the Energy Domain: Backscattering and Time-of QENS in the Energy Domain: Backscattering and Time-of of-flight Alexei Sokolov Department of Polymer Science, The University of Akron Outline Soft Matter and Neutron Spectroscopy Using elastic scattering

More information

Uses 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 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 information

Magnetic Resonance Lectures for Chem 341 James Aramini, PhD. CABM 014A

Magnetic Resonance Lectures for Chem 341 James Aramini, PhD. CABM 014A Magnetic Resonance Lectures for Chem 341 James Aramini, PhD. CABM 014A jma@cabm.rutgers.edu " J.A. 12/11/13 Dec. 4 Dec. 9 Dec. 11" " Outline" " 1. Introduction / Spectroscopy Overview 2. NMR Spectroscopy

More information

Principios 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 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 information

Supporting Information

Supporting Information upporting Information Comparison of olid-tate Dipolar Couplings and olution Relaxation Data Provides Insight into Protein Backbone Dynamics. Veniamin Chevelkov, Yi Xue, Rasmus Linser, Nikolai R. krynnikov,

More information

Supporting Information Elucidating Lithium-Ion and Proton Dynamics in Anti- Perovskite Solid Electrolytes

Supporting Information Elucidating Lithium-Ion and Proton Dynamics in Anti- Perovskite Solid Electrolytes Electronic Supplementary Material (ESI) for Energy & Environmental Science. This journal is The Royal Society of Chemistry 2018 Supporting Information Elucidating Lithium-Ion and Proton Dynamics in Anti-

More information

Center for Sustainable Environmental Technologies, Iowa State University

Center 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 information

Lecture #7 In Vivo Water

Lecture #7 In Vivo Water Lecture #7 In Vivo Water Topics Hydration layers Tissue relaxation times Magic angle effects Magnetization Transfer Contrast (MTC) CEST Handouts and Reading assignments Mathur-De Vre, R., The NMR studies

More information

Christopher Pavlik Bioanalytical Chemistry March 2, 2011

Christopher 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 information

DNP enhanced frequency-selective TEDOR experiments in bacteriorhodopsin

DNP 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 information

Solid-state NMR studies of protein dynamics: New approaches and applications to crystalline proteins and large molecular assemblies

Solid-state NMR studies of protein dynamics: New approaches and applications to crystalline proteins and large molecular assemblies Solid-state NMR studies of protein dynamics: New approaches and applications to crystalline proteins and large molecular assemblies Paul Schanda To cite this version: Paul Schanda. Solid-state NMR studies

More information

An introduction to Solid State NMR and its Interactions

An 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 information

Introduction to NMR for measuring structure and dynamics + = UCSF Macromolecular Interactions. John Gross, Ph.D.

Introduction to NMR for measuring structure and dynamics + = UCSF Macromolecular Interactions. John Gross, Ph.D. Introduction to NMR for measuring structure and dynamics + = UCSF Macromolecular Interactions John Gross, Ph.D. Nuclear Spins: Microscopic Bar Magnets H µ S N N + Protein Fragment Magnetic Moment Bar Magnet

More information

HSQC spectra for three proteins

HSQC spectra for three proteins HSQC spectra for three proteins SH3 domain from Abp1p Kinase domain from EphB2 apo Calmodulin What do the spectra tell you about the three proteins? HSQC spectra for three proteins Small protein Big protein

More information

I690/B680 Structural Bioinformatics Spring Protein Structure Determination by NMR Spectroscopy

I690/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 information

Solid-State NMR Structural Studies of Proteins Using Paramagnetic Probes

Solid-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 information

Solid state 13 Cand 1 H MAS NMR investigations of C 60 (ferrocene-d 10 ) 2 complex

Solid 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 information

Introduction to NMR Product Operators. C. Griesinger. Max Planck Institute for Biophysical Chemistry. Am Faßberg 11. D Göttingen.

Introduction to NMR Product Operators. C. Griesinger. Max Planck Institute for Biophysical Chemistry. Am Faßberg 11. D Göttingen. ntroduction to NMR Product Operato C. Griesinger Max Planck nstitute for Biophysical Chemistry Am Faßberg 11 D-3777 Göttingen Germany cigr@nmr.mpibpc.mpg.de http://goenmr.de EMBO Coue Heidelberg Sept.

More information

NMR in Medicine and Biology

NMR 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 information

UNIVERSITY OF CINCINNATI

UNIVERSITY OF CINCINNATI UNIVERSITY OF CINCINNATI Date: I,, hereby submit this work as part of the requirements for the degree of: in: It is entitled: This work and its defense approved by: Chair: Nuclear Magnetic Resonance Studies

More information

NMR of large protein systems: Solid state and dynamic nuclear polarization. Sascha Lange, Leibniz-Institut für Molekulare Pharmakologie (FMP)

NMR of large protein systems: Solid state and dynamic nuclear polarization. Sascha Lange, Leibniz-Institut für Molekulare Pharmakologie (FMP) NMR of large protein systems: Solid state and dynamic nuclear polarization Sascha Lange, Leibniz-Institut für Molekulare Pharmakologie (FMP) The Aim of the Game solution NMR other methods solid state NMR

More information

Protein structure determination by solid-state NMR

Protein 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 information

Interactions and Dynamics within the Troponin Complex

Interactions and Dynamics within the Troponin Complex Interactions and Dynamics within the Troponin Complex Tharin Blumenschein Steve Matthews Lab - Imperial College London (formerly Brian Sykes Lab, Canada) Striated muscle Thin filament proteins - regulation

More information

H B. θ = 90 o. Lecture notes Part 4: Spin-Spin Coupling. θ θ

H 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 information

NMR 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 - 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 information

Millisecond Time-scale Protein Dynamics by Relaxation Dispersion NMR. Dmitry M. Korzhnev

Millisecond Time-scale Protein Dynamics by Relaxation Dispersion NMR. Dmitry M. Korzhnev Millisecond Time-scale Protein Dynamics by Relaxation Dispersion NMR Dmitry M. Korzhnev Department of Molecular, Microbial and Structural Biology University of Connecticut Health Center 263 Farmington

More information

Biochemistry 530 NMR Theory and Practice

Biochemistry 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 information

Nuclear Magnetic Resonance

Nuclear 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 information

SUPPLEMENTARY NOTE 1: ADDITIONAL CHARACTERIZATION OF NANODIAMOND SOLUTIONS AND THE OVERHAUSER EFFECT

SUPPLEMENTARY NOTE 1: ADDITIONAL CHARACTERIZATION OF NANODIAMOND SOLUTIONS AND THE OVERHAUSER EFFECT 1 SUPPLEMENTARY NOTE 1: ADDITIONAL CHARACTERIZATION OF NANODIAMOND SOLUTIONS AND THE OVERHAUSER EFFECT Nanodiamond (ND) solutions were prepared using high power probe sonication and analyzed by dynamic

More information

Coupling of Functional Hydrogen Bonds in Pyridoxal-5 -phosphate- Enzyme Model Systems Observed by Solid State NMR

Coupling of Functional Hydrogen Bonds in Pyridoxal-5 -phosphate- Enzyme Model Systems Observed by Solid State NMR Supporting Information for Coupling of Functional ydrogen Bonds in Pyridoxal-5 -phosphate- Enzyme Model Systems bserved by Solid State NMR Shasad Sharif, David Schagen, Michael D. Toney, and ans-einrich

More information

Measuring Spin-Lattice Relaxation Time

Measuring 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 information

Biochemistry 530 NMR Theory and Practice

Biochemistry 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 information

NMR-spectroscopy. I: basics. Peter Schmieder

NMR-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 information

6 NMR Interactions: Zeeman and CSA

6 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 information

Protein Dynamics Relaxation techniques

Protein Dynamics Relaxation techniques Protein Dynamics Relaxation techniques Daniel Mathieu Bruker Users Meeting 2016, Karlsruhe Innovation with Integrity Proteins aren t exactly rock solid 10.11.2016 Users meeting 2016 2 Characterizing Dynamic

More information

Direct dipolar interaction - utilization

Direct dipolar interaction - utilization Direct dipolar interaction - utilization Two main uses: I: magnetization transfer II: probing internuclear distances Direct dipolar interaction - utilization Probing internuclear distances ˆ hetero D d

More information

Supplemental Information for. Quaternary dynamics of B crystallin as a direct consequence of localised tertiary fluctuations in the C terminus

Supplemental Information for. Quaternary dynamics of B crystallin as a direct consequence of localised tertiary fluctuations in the C terminus Supplemental Information for Quaternary dynamics of B crystallin as a direct consequence of localised tertiary fluctuations in the C terminus Andrew J. Baldwin 1, Gillian R. Hilton 2, Hadi Lioe 2, Claire

More information