4. Acquisition

Time requirement: 5h Sample: 0.5 ml salicylaldehyde with 0.2 ml [DgJDMSO.

Record normal ¹H and ¹³C NMR spectra of the sample, note the required spectral widths and note the offset of the middle of each spectrum. Change to the 2D mode of the spectrometer and load the 2Q-HMBC pulse program. You have to set:

td2: 1 k data points in F2 td1: 128 data points in F;

sw2: 5.2 ppm sw1: 206 ppm (C,C double-quantum frequency, enter in Hz) offset of ¹H frequency: center of ¹H NMR spectrum offset of ¹³C frequency: center of ¹³C NMR spectrum p!: 90° ¹H transmitter pulse p2: 180° ¹H transmitter pulse p3, p4, p5, p7: 90° ¹³C decoupler pulse p6: 180° ¹³C decoupler pulse dl:4s 1 d2: – effecti dient duration = 1.936 - 2. +0.146I 4, ~Join effective gradient duration ms, cal culated from 'J(C,Hmax) = 179 Hz and '(C,Hmin) = 159 Hz 1 d3: – effecti dient duration = 1. - Dra, ~0.146 oa, Soin effective gradient duration = 1.689 ms, cal culated from 'J(C,Hmax) = 179 Hz and '(C,Hmin) = 159 Hz d4: 2(CH) – effective gradient duration = 57.6 ms, calculated from °J(C,H) initial value for ¢, evolution: 3 μs increment for ¢, evolution: 1/[2-sw1] g1–g5: sinusoidal-shaped field gradients with 5% truncation, 1 ms duration and ca. 0.2 T/m strength, with gradient loop counters, ring-down delays (100 μs), lock blanking and gradient coil blanking switches according to actual instrumentation used. Gradient strength ratio: 3 : -2 : -1 :3:-l (echo) and 3 : -2 : -1 : -3 : 1 (anti-echo) For the phase-sensitive echo/anti-echo scheme in F, use simultaneous data mode in F.