Time‐shared NMR experiments

Abstract

Details on the implementation of the simultaneous evolution of multiple frequencies into the same time period of a NMR pulse sequence are introduced. Timeshared (TS) versions of the most useful inverse 2D NMR experiments (TS-HMBC, TS-HSQC, TS-HSQC-TOCSY, and TS-HSQMBC) are presented and illustrated for simultaneous acquisition of 1 H/ 13 C and 1 H/ 15 N NMR spectra. The major benefits associated to the parallel acquisition of multiple spectra from a single NMR experiment are spectrometer time savings and the achievement of multiple and complementary information with improved sensitivity gains per time unit.

Simultaneous determination of the magnitude and the sign of multiple heteronuclear coupling constants in 19 F or 31 P-containing compounds

“…The proposed methods can also be modified by implementing the time-shared (TS) evolution concept (see pulse sequence details in the Supporting Information). [17] For instance, the simultaneous measurement of small Figure 4 shows a practical example after selection of the H6 proton in 2. Figure 4A shows the pure IP TS-selHSQMBC spectrum where all cross-peaks belonging to spectra are shown superimposed and slightly shifted for the sake of clarity.…”

“…More and detailed information about the general concepts, experimental details, and successful implementation of the TS concepts in conventional NMR experiments are found in the supporting information and Ref. [17].…”

“…[11][12][13][14][15][16] Here, we show how the application of the previously reported 1 H-X selHSQMBC and selHSQMBC-TOSY experiments (X = 13 C or 15 N) to molecules containing passive highly abundant spins (Z = 19 F or 31 P) allows the measurement of the magnitude and the size of multiple heteronuclear coupling constants from complementary in-phase E.COSY and IPAP multiplet patterns. Additionally, time-shared (TS) versions of these selHSQMBC experiments [17] are also proposed for the simultaneous determination of multiple coupling constants for two different heteronuclei, namely X and Y, and examples for the extraction of a complete set of the magnitude and/or the sign of different heteronuclear coupling constants in nitrogen-containing molecules are provided.…”

Spatially Selective Heteronuclear Multiple‐Quantum Coherence Spectroscopy for Biomolecular NMR Studies

“…Here we present HMQC experiments implemented by combining a single SS 90° 1 H pulse with two non-selective 1 H 180° pulses such that 1 H magnetization outside of the selectively excited slice is returned to the z-axis before signal detection. Specifically, we implemented (i) simultaneous [20] 2D [ 13 C methyl / 15 N, 1 H] HMQC (referred to as sim-HMQC in this paper) and (ii) constant time ( ct ) [21] 2D [ 13 C methyl , 1 H] HMQC ( ct -HMQC). Applications of sim-HMQC are presented for U-[ 13 C, 15 N]-labeled 7.6 kDa protein ubiquitin as well as for U-[ 2 H, 13 C, 15 N]-labeled, but isoleucine, leucine, valine (ILV) methyl protonated [22] 7.5 kDa Northeast Structural Genomics Consortium (NESG; http://www.nesg.org) target GmR137.…”

UTOPIA NMR: activating unexploited magnetization using interleaved low-gamma detection

“…Instrumental improvements, isotope labeling schemes (Lundstrom et al 2012) and developments in pulse sequences (Diercks and Orekhov 2005; Farmer 1991; Frueh et al 2009; Kay et al 1990; Kay et al 1992; Kern et al 2008; Lescop et al 2007; Parella and Nolis 2010; Perez-Trujillo et al 2007; Sattler et al 1995; Schanda and Brutscher 2005; Schanda et al 2007; Szyperski et al 1996) can shorten the time for data acquisition and improve the spectral quality, thus partially compensating the growing sample complexity. Several interesting concepts such as time-shared NMR (Farmer 1991; Kay et al 1990; Kay et al 1992; Parella and Nolis 2010; Perez-Trujillo et al 2007; Sattler et al 1995), BEST (Lescop et al 2007) and SOFAST (Kern et al 2008; Schanda and Brutscher 2005; Schanda et al 2007) techniques, have been developed to use the available magnetization more effectively. In addition, the usage of a second receiver allows parallel signal acquisition of different nuclei (Chakraborty et al 2012; Kupce et al 2006; Kupce and Kay 2012; Kupce et al 2010; Moore et al 1991; Reddy and Hosur 2013).…”