Two-dimensional heteronuclear spectroscopy with methanol. (A) Setup. (B) 1H-only 1D spectrum. (C) HSQC spectrum. A four-phase cycling to select the particular coherence pathway uses ϕ1∈{0,π,0,π}, ϕ2∈{0,0,π,π}, and ϕ3∈{0,π,π,0}. HSQC spectrum takes 17 min to obtain (168 scans including phase cycling with a single scan/wait time of 6 s). (D) HMQC spectrum. An eight-phase cycling to select the particular coherence pathway uses ϕ1∈{0,π,0,π,0,π,0,π}, ϕ2∈{0,0,π/2, π/2,π,π,3π/2,3π/2}, and ϕ3∈{0,π,π,0,0,π,π,0}. HMQC spectrum takes 34 min to acquire (336 scans including phase cycling with a single scan/wait time of 6 s). For C and D, the 13C π/2-pulse duration is obtained separately (Materials and Methods), and τ = 1/(4JC-H).