Orphan spin operators enable the acquisition of multiple 2D and 3D magic angle spinning solid-state NMR spectra

Gopinath, T.; Veglia, Gianluigi

doi:10.1063/1.4803126

Cited by 36 publications

(50 citation statements)

References 36 publications

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“…The S spins will then evolve under the CS Hamiltonian during the t 2 acquisition period, resulting in a two-dimensional spectrum that correlates the S spin chemical shift with I-S DC. In the SE version, a spin-echo is utilized to recover both sine and cosine modulated dipolar coherences, thereby enhancing the signal by up to 40% (Gopinath et al 2013; Gopinath et al 2010a; Gopinath and Veglia 2009; Gopinath et al 2010b). In the new experiment reported in Figure 1A, we utilize the dual acquisition method to separate sine and cosine coherences to give two separate spectra: 2D PISEMA and PISEMA-mixing.…”

Section: Resultsmentioning

confidence: 99%

“…For these reasons, we propose a new method called DAISY (Dual Acquisition orIented ssNMR spectroScopY) that enables the acquisition of two OS ssNMR spectra, simultaneously. The overall philosophy of this approach impinges on our recent developments in the field of MAS NMR sequences for the dual and multiple acquisitions of 2D and 3D experiments (Gopinath and Veglia 2012a; Gopinath and Veglia 2012b; Gopinath and Veglia 2013). Specifically, we make use of the long living 15 N polarization to acquire two experiments with only one pulse sequence and without the addition of a second receiver.…”

Section: Introductionmentioning

confidence: 99%

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Simultaneous acquisition of 2D and 3D solid-state NMR experiments for sequential assignment of oriented membrane protein samples

2015

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We present a new method called DAISY (Dual Acquisition orIented ssNMR spectroScopY) for the simultaneous acquisition of 2D and 3D oriented solid-state NMR experiments for membrane proteins aligned in mechanically or magnetically lipid bilayers. DAISY utilizes dual acquisition of sine and cosine dipolar or chemical shift coherences and long living 15N longitudinal polarization to obtain two multi-dimensional spectra, simultaneously. In these new experiments, the first acquisition gives the polarization inversion spin exchange at the magic angle (PISEMA) or heteronuclear correlation (HETCOR) spectra, the second acquisition gives PISEMA-mixing or HETCOR-mixing spectra, where the mixing element enables inter-residue correlations through 15N-15N homonuclear polarization transfer. The analysis of the two 2D spectra (first and second acquisitions) enables one to distinguish 15N-15N inter-residue correlations for sequential assignment of membrane proteins. DAISY can be implemented in 3D experiments that include the polarization inversion spin exchange at magic angle via I spin coherence (PISEMAI) sequence, as we show for the simultaneous acquisition of 3D PISEMAI-HETCOR and 3D PISEMAI-HETCOR-mixing experiments.

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Simultaneous acquisition of 2D and 3D solid-state NMR experiments for sequential assignment of oriented membrane protein samples

2015

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“…A similar strategy was previously applied to obtain dual acquisition in the DUMAS and MEIOSIS methods. [9, 10] The t 2 acquisition time was set to 30 and 20 ms for riHSQC and cpHSQC experiments, respectively.…”

Section: Methodsmentioning

confidence: 99%

1 H-detected MAS solid-state NMR experiments enable the simultaneous mapping of rigid and dynamic domains of membrane proteins

Gopinath

Nelson

Veglia

2017

Journal of Magnetic Resonance

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Magic angle spinning (MAS) solid-state NMR (ssNMR) spectroscopy is emerging as a unique method for the atomic resolution structure determination of native membrane proteins in lipid bilayers. Although 13C-detected ssNMR experiments continue to play a major role, recent technological developments have made it possible to carry out 1H-detected experiments, boosting both sensitivity and resolution. Here, we describe a new set of 1H-detected hybrid pulse sequences that combine through-bond and through-space correlation elements into single experiments, enabling the simultaneous detection of rigid and dynamic domains of membrane proteins. As proof-of-principle, we applied these new pulse sequences to the membrane protein phospholamban (PLN) reconstituted in lipid bilayers under moderate MAS conditions. The cross-polarization (CP) based elements enabled the detection of the relatively immobile residues of PLN in the transmembrane domain using through-space correlations; whereas the most dynamic region, which is in equilibrium between folded and unfolded states, was mapped by through-bond INEPT-based elements. These new 1H-detected experiments will enable one to detect not only the most populated (ground) states of biomacromolecules, but also sparsely populated high-energy (excited) states for a complete characterization of protein free energy landscapes.

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“…This was followed by the application of dual acquisition to a separated local field (SLF) spectroscopy [4] version of the experiment [5]. More recently, Gopinath et al and Lamley and Lewandowsky have built on this foundation by employing simultaneous cross-polarization (CP) to 13 C and 15 N to obtain two multi-dimensional spectra in a single experiment [6–9]. …”

Section: Introductionmentioning

confidence: 99%

Multiple acquisition/multiple observation separated local field/chemical shift correlation solid-state magic angle spinning NMR spectroscopy

Das

Opella

2014

Journal of Magnetic Resonance

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Multiple acquisition spectroscopy (MACSY) experiments that enable multiple free induction decays to be recorded during individual experiments are demonstrated. In particular, the experiments incorporate separated local field spectroscopy into homonuclear and heteronuclear correlation spectroscopy. The measured heteronuclear dipolar couplings are valuable in structure determination as well as in enhancing resolution by providing an additional frequency axis. In one example four different three-dimensional spectra are obtained in a single experiment, demonstrating that substantial potential saving in experimental time is available when multiple multi-dimensional spectra are required as part of solid-state NMR studies.

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Orphan spin operators enable the acquisition of multiple 2D and 3D magic angle spinning solid-state NMR spectra

Cited by 36 publications

References 36 publications

Simultaneous acquisition of 2D and 3D solid-state NMR experiments for sequential assignment of oriented membrane protein samples

Simultaneous acquisition of 2D and 3D solid-state NMR experiments for sequential assignment of oriented membrane protein samples

1 H-detected MAS solid-state NMR experiments enable the simultaneous mapping of rigid and dynamic domains of membrane proteins

Multiple acquisition/multiple observation separated local field/chemical shift correlation solid-state magic angle spinning NMR spectroscopy

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