Figure 3.

The pulse sequence of the 2D (H2C)N(CC)H-TOCSY experiment. This experiment provides correlation between Lys side-chain 15Nζ and 1H resonances, and corresponds to a hybrid of the H2CN (Andre et al. 2007) and HCCH-TOCSY (Kay et al. 1993) experiments for H2O samples. 13C shaped pulses are Lys 13Cε-selective r-SNOB pulses (980 us). Length of the 13C- spin lock (SL) was 1 ms. 13C carrier position was 43 ppm. The rf strength of the DIPSI-3 scheme (the total length, 16.9 ms) was 9.6 kHz and that of hard 13C pulses was 20.8 kHz. 15N shaped pulses are Lys 15Nζ-selective r-SNOB pulses (1.0 ms). 15N carrier position was 32 ppm. Delays: τ1 = 1.6 ms; τ2 = 1.1 ms; δ = 1.7 ms; and Tc = 20 ms. Phase cycles: ϕ1 = [x, −x]; ϕ2 = [2x, 2(−x)], ϕ3 = [4x, 4y]; ϕ4 = [4x, 4(−x)]; and receiver = [x, −x, −x, x, −y, y, y, −y]. Quadrature detections for indirect 15N dimensions was achieved using States-TPPI for ϕ1.