HETCOR (C, H Correlation by Polarization Transfer) SOLUTION APPLICATION
1. Introduction
A two dimensional HETeronuclear COrrelation experiment (HETCOR) is described here as 13C-1H
Correlation by Polarization Transfer. The experiment encodes the proton chemical shift information into
13C signals that are observed, and yields cross signals for all protons and 13C nuclei that are connected by
a 13C-1H coupling over one bond. The assignment of one member of a spin-coupled pair immediately leads
to the assignment of the other. The HETCOR experiment described here uses a phase cycling for magnitude
processing. This example demonstrates the basic principle of 2D NMR data acquisition and processing on
Tecmag spectrometers.
2. Pulse sequence
1H π t1/2 t1/2 d1 π d2
2 2 WALTZ-16 d1 = 1/2JCH
(a) P1 P2 d2 = 1/3JCH
13C π π WALTZ-16 = RRRR RRRR RRRR RRRR,
2 R = 90x180-x270x
P3 P4
(b) 1D phase tables:
(P1): 0.
ph1(P2): 0, 2, 1, 3.
ph0(P3): 0, 0, 0, 0,
2, 2, 2, 2.
ph1(P4): 0, 0, 0, 0,
1, 1, 1, 1,
2, 2, 2, 2.
3, 3, 3, 3.
phrx: (0, 2, 1, 3)2,
(1, 3, 2, 0)2,
(2, 0, 3, 1)2,
(3, 1, 0, 2)2.
(All tables are in 4 step mode.)
2D delay table:
de1:2 (t1/2):
Auto, Every Pass.
Increment value: 200 µs,
Fig. 1. (a) The pulse sequence for the HETCOR experiment. (b) The sequence in the NTNMR sequence
editor with phase tables set for magnitude processing.
3. Experiment
Sample: 20 % ethyl crotonate in CDCl3
Spectrometer: 7 Tesla magnet with Tecmag HF3 Discovery
Probe: Nalorac D300-5 OWB 5mm 1H/13C Switchable probe
13C 90o pulse:
10.5 µs
1H 90o pulse:
42.5 µs
HETCOR (C, H Correlation by Polarization Transfer) SOLUTION APPLICATION
3. Experiment (continued)
SW +/- (1D, 13C) : 8.3 kHz (110.5 ppm)
SW 2D (+/-, 1H): 1.25 kHz (4.15 ppm) O
1
Dwell time (1D): 60 µs H 3 2 C 5 6
Dwell_2D: 400 µs C C O CH 2 CH 3
Acq. points (and Points 1D): 1024 H 3 C H
4
Points 2D: 256
Scans 1D: 32 Ethyl crotonate
Notes:
1. The sample is locked but not spun. The magnet is shimmed to ~0.8 Hz line width.
2. First, calibrate the 90o pulse widths of 1H and 13C using the nutation experiment (see note, "One Pulse
Experiment and Pulse Calibration").
3. Set up the WALTZ sequence according to the note, "13C NMR Spectra with 1H WALTZ Decoupling".
4. The center of pulses P2 and P4 should be aligned. Since P2 > P4, P2 have to split into 3 pulses. The delay
of P2's middle pulse equals to P4, and the delay of both sides is (P2 - P4)/2 . The middle pulse of P2 falls
on the same event as P4 (and P5).
2 3 5 46
1
4. Results
Data processing:
In the NDFT window, 0
click the "1D" tab and select:
"Use 1D settings", 1
"Fourier Transform",
2
"Sine Bell, SB Shift: 90,
SB Skew: 5, SB width: 1024";
δH(ppm)
3
click the "2D" tab and select:
"Use 2D settings",
4
"Zero fill, 1",
"Sine Bell, SB Shift: 90,
5
SB Skew: 5, SB width: 512";
"Fourier Transform", 6
"Transpose: complex",
click "Do it". 7
The data processing procedure is
automated in an NMRScript. To use the
150 100 50 0
script, click "Scripts|Processing scripts|
δC(ppm)
Process 2D (Magnitude)".
Fig. 2. Magnitude plot of the HETCOR spectrum of
ethyl crotonate.
5. References
1. R. Freman, G. A. Morris, J. Chem. Soc. Chem. Commun., 1978, 684-686.
2. S. Braun, H.-O. Kalinowski, S. Berger, "150 and More Basic NMR Experiments", Wiley-VCH, 1999,
375-377. QWZ 11/15/2002
