An NMR study of two known his-indole alkaloids is described. In addition to conventional 1D NMR methods, 2D shift-correlated NMR experiments [(1)Hx(1)H-COSY, (1)Hx(13)C-HMQC-(1)J(C,H), (1)Hx(13)C-HMBC-(n)J(C,H) (n = 2 and 3)] and 2D (1)Hx(1)H-NOESY were used for H-1 and C-13 chemical shift assignments of these alkaloids. Copyright (C) 1999 John Wiley & Sons, Ltd.