Assignment of complex proton NMR spectra via two-dimensional homonuclear Hartmann-Hahn spectroscopy

Abstract

We propose the use of a new type of two-dimensional NMR experiment for the determination of homonuclear scalar connectivity in complex molecules. The method relies on the principle of cross polarization, first introduced by Hartmann and Hahn1 and commonly used for sensitivity enhancement in solid-state 13C

Native Corrinoids fromClostridium cochleariumAre Adeninylcobamides: Spectroscopic Analysis and Identification of Pseudovitamin B12and Factor A

“…The solvents included 90% 10 mM phosphate buffer (pH 5.2) and 10% D 2 O. 1 H, 13 C, and 15 N signal assignments were from 1 H NMR spectra with water presaturation; 1 H-broad-band-decoupled 13 C NMR spectra; 1 H, 13 C gradient-enhanced heteronuclear single-quantum coherence experiments (PFG-HSQC) (19,38); 1 H, 15 N gradient-enhanced heteronuclear single-quantum coherence experiments (PFG-HSQC) (19,38), 2D gradient-enhanced heteronuclear multiple-bond coherence experiments (PFG-HMBC) (5, 38), 2D total correlation spectroscopy (watergate-TOCSY) (3,14,18,56), and 2D rotating frame Overhauser enhancement spectroscopy (watergate-ROESY) (4,11,56). All 2D NMR experiments were parametrized as described earlier (42).…”

The 3D structure of a cyclosporin analogue in water is nearly identical to the cyclophilin‐bound cyclosporin conformation

“…Sample conditions are given in the figure legends. Resonance assignments were obtained from 2QF-COSY [23], TOCSY [24,25], and NOESY [26] experiments. The data used for structure determination of [D-Me&r'-D-Ser(O-Gly)*]CS in (D,)DMSO (4 mM) were obtained from a NOESY spectrum with a mixing time z, of 50 ms recorded at 500 MHz.…”

Quantification of the calcium‐induced secondary structural changes in the regulatory domain of troponin‐C

“…All experiments were carried out on a Varian Unity-600 NMR spectrometer operating at a temperature of 30 "C. Assignments of 'H-and "N-resonances of NTnC-apo were carried out by acquiring the following sets of 2D-and 3D-NMR data: (1) DQF-COSY in H 2 0 (Rance et al, 1983); (2) TOCSY (50 ms) in H 2 0 (Braunschweiler & Ernst, 1983;Davis & Bax, 1985); (3) NOESY (40, 80, 120, 160, 200, 250 ms) in H 2 0 (Jeener et al, 1979;Macura & Ernst, 1980); (4) DQF-COSY in DzO; (5) TOCSY (50 ms) in DzO; (6) NOESY (150 ms) in DzO; (7) 2D( 15N-'HJ HMQC (Bax et al, 1983); (8) 3D-I5N-edited NOESY (150ms) in H,O (Kay et al, 1989); and (9) 3D-I'N-edited TOCSY (75 ms) in H 2 0 (Marion et al, 1989a). The following experiments were used for the study of NTnC.2Ca: (10) 2D(I5N-IH] HMQC; (1 1) 3D-HNCA (Grzesiek & Bax, 1992); (12) 3D-HNCO (Grzesiek & Bax, 1992); (13) 3D-HNCOCA (Grzesiek & Bax, 1992); (14) 3D-HCACO ; (15) 3D-15N-edited NOESY (150 ms); and (16) 3D-I5N-edited TOCSY (70 ms).…”