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2D w1-X-edited NOESY

DESCRIPTION
The 2D w1-X-edited (filtered or selected) NOESY experiment affords a 2D NOESY spectrum in which 1H directly-attached to X nuclei are efficiently filtered or selected before evolution during the variable t1 period. This experiment is widely used to study protein-ligand complexes, where the protein is usually 13C and/or 15N-labeled and the ligand is at natural abundance .

REQUIREMENTS
Easy implementation on any AVANCE spectrometer equipped with an inverse probehead.
VERSIONS
The basic sequence of the 2D w1-X-edited NOESY experiment is easily designed by replacing the initial 90º 1H pulse of a conventional 2D NOESY pulse scheme by an X half-filter ( 91ANG1329 ) or an X-filter element ( 96JB492-8 ). If required, a BIRD-recovery cluster can be used as a preparation period in order to reduce the large unwanted 1H-X (typically, 12C or 14N) magnetization. Carbon decoupling is optionally applied during proton acquisition. Because there is no heteronuclear decoupling during t1, all relay peaks appear as doublets in F1 dimension due to 1J(CH), reducing the sensitivity of the method.

Modified approaches have been reported using 13C/15N double half filters (w1-13C/15N-doubly edited NOESY experiments) and time-shared 13C-filters ( 00JMR168-144 )

Other closely related experiments are:

EXPERIMENTAL DETAILS
The 2D w1-X-edited NOESY experiment can be recorded in routine/automation modes. The experiment is basically optimized as described for the 2D NOESY experiment. The X half-filter is optimized as described in a regular HMQC experiment and the phase cycle is selected in order to select or to filter the desired isotope.
  • Tutorials: 2D inverse experiments
  • Tutorials: 2D gradient-based inverse experiments
  • SPECTRA
    The 2D w1-X-edited NOESY spectrum shows a typical 2D NOESY map in which cross-peaks show E.COSY pattern. The nJ(CH) values are measured from signal displacement in two F1 slices through each signal of the cross-peak doublet split by 1J(CH) in the F1 dimension. Thus, coupling constants smaller than the linewidth can be determined accurately. In addition, the pulse sequence contains no delays to evolve nJ(CH) as in HMBC-like experiments, which simultaneous allows evolution of J(HH). Therefore, the  spectrum is free from J(HH) modulation and it can be phased to pure absorption.
    RELATED TOPICS
    Analogs 3D NOESY-HMQC, 3D NOESY-HSQC, 3D HMQC-NOESY, and 3D HSQC-NOESY experiments can easily designed by incorporating a second variable evolution period in the HMQC/HSQC block as usual. On the other hand, a very similar pulse sequence is used for the 2D HMQC-NOESY and 2D HSQC-NOESY experiments by using a single variable evolution period in the HMQC/HSQC block .

    Related experiments:

  • 2D Inverse experiments
  • 2D Inverse gradient-enhanced experiments