360-MHz proton NMR spectrum

Figure 1 360 MHz Proton NMR spectrum, in CDC13, of protoporphyrin-IX (19) dimethyl ester. Assignments a, methine protons b, vinyl CH c, vinyl CH2 d, propionate CH2CH2CO e, nuclear methyls and methyl esters f, propionate CH2CH2CO g, NH...

Figure 5. 360-MHz proton NMR spectrum of Forrsman hapten in DMSO-ds...

Figure 41. The 360-MHz proton NMR spectrum (4.5 to 9.0 ppm) of the Nuc/D = 10 netropsin poly(dA-dT) complex in 0.1 M cacodylate, 4.4mM EDTA 2H 0, pH 7.08 at 87°C. The tentatively assigned N-methylpyrrole protons of netropsin are...

Figure 8. A, A 360-MHz proton NMR spectrum of camphor, 2 M in deutero-chloroform B and C, A 55-MHz natural-abundance NMR spectrum of the same sample with (B), and without (C) proton broadband decoupling.

Figure 7. The effect of ApA binding upon the photp-CIDNP difference spectrum of the aromatic part of the 360 MHz proton NMR spectrum of gene-5 protein. Ratio ApA/gene-5 pro-telni (A) 0.0 (B) 4.6 (C) 11.4 (0) 17.3.

Figure 17. The 360-MHz proton NMR spectra of the proflavine poly(dA-dT) complex in 1M NaCl, lOmM cacodvlate, JOmM EDTA, zHzO, pH 7. The top spectrum represents the Nuc/D = 24 complex at 78.5°C ( ut of the proflavine resonances in the complex is 80°C), while the bottom spectrum represents the Nuc/D = 8 complex at 8l.4°C ft,/, of proflavine resonances in complex is 84.3°C). The proflavine resonances are designated by asterisks.

Figure 31. Temperature dependence of the aromatic resonances in the 360 MHz H-NMR spectrum of BPTI. For Tyr 35 and Phe 45, the spectra are individually simulated and the flip rates at different temperatures obtained from the best fit with the experimental data are indicated. In the experimental spectrum at 4°C, the resonances of four protons of the Phe 45 (O) and two protons of Tyr 35 (A) are recognized readily, whereas the other lines are masked by resonances of the other aromatics in the protein. Most of the resonance lines of Phe 45 and Tyr 35 are also resolved in the spectra at higher temperatures and the transitions from slow to rapid sign flipping is readily apparent (from [115]).

Fig. 11. Resolution-enhanced 360 MHz IH-NMR spectrum of p-N-acetylneuraminic acid-2-phosphate (pNeu5Ac2P) dissolved in 2H2O, recorded at p H 7.5 and 25 °C. The relative-intensity scale of the 5Ac methyl proton signal differs from that of the other parts of the...

Temuconine (292), C37H42N206, [tt] 5 +68° (c 0.24, MeOH), was isolated from the Chilean species Berberis valdiviana Phil. (Berberidaceae). The structure was established principally by spectral comparison to the known alkaloid, (+)-berbamunine (182), for which the CD spectrum was apparently recorded for the first time. The 200-MHz FT NMR and 360-MHz FT NMR NOE difference spectra (see Section VI,A,2,b) of temuconine were originally interpreted as indicating structure 293 (137) a reinvestigation, which assigned all the protons, particularly the H-T (8 3.78) and H-l (3.61) multiplets, showed that temucocine actually has structure 292 (138). 

Figure 2. 2D J-resolved proton spectrum of the protein bovine pancreatic trypsin inhibitor (BPTI). a. High-field region from 0.4—1.6 ppm, which contains the resonances of 19 methyl groups of the 360-MHz H NMR spectra of a 0.01 M solution of BPTI in D O at pH 4.5, 60°C. Prior to the Fourier transformation, the 2D data set was weighted in the t, and ts directions by weighting functions cos[(t.J 2Tx)ir]exp(tx/0.4Tx), with x = 1,2 Tj = 2.46 s, and Ts = 1.23 s are the maximum acquisition times in the ti and tj domains. The 2D J-resolved spectrum was computed from 64 X SI 92 data points and is presented as a (J, spectrum the top trace shows the conventional ID spectrum the bottom trace shows the projection of the 2D spectrum with 4> = rtl4. b. Presentation of the 2D J-resolved H spectrum (a) by cross sections. The resolved multiplets of 19 methyl protons are shown. The 2D resolved spectrum allows the analysis of otherwise overlapping multiplets, the accurate measurement of coupling constants, and the assignment of the resonances. (Reproduced, with permission, from Ref. 14. Copyright 1978, Academic...

Figure 6. a. Proton NMR spectrum (360 MHz) of glutamate derived from M. ammo-... 

In 73a-f, 13 of the 14 olehnic protons give rise to 111 NMR signals within 0.50 ppm of each other in the spectrum of 73d ah olehnic signals fah within this range. Thus, even at relatively high frequency (360 MHz), extensive overlap occurs (Figures 17-20). 

Figure 10. The 360-MHz correlation proton NMR spectra of poh(dA-dT) in 1M (-H,C),NCl. lOmM phosphate, ImM EDTA, 80% H,0-20% DtO at 37°C. Spectrum A mot recorded at pH 7.5 while Spectrum B wot recorded at pH 9.5. (2H C).NCl was purchased from Merck and used without further purification.

Figure 25. The 360-MHz correlation proton NMR spectra of the daunomycin poly(dA-dT) complex in /M NaCl, lOmNi cacodylate, lOmM EDTA, 80% HaO— 20% 2H 20. Spectrum A corresponds to the Nuc/D = 11.8 complex, pH 6.0 at 67°C and Spectrum B corresponds to the Nuc/D = 5.9 complex, pH 6.05 at 57°C. The strong resonance corresponds to thymidine H-3 proton of the nucleic acid while the weaker resonances (designated hy asterisks) corresponds to hydroxyl protons at Positions 9 and 11 on Ring B of the anthracycline ring of daunomycin...

Liquid crystals can also be used since the temperature-dependent residual static dipole-dipole coupling caused by the anisotropic orientational order produces, in turn, a temperature-dependent static splitting of the proton spectrum. The first study used a 5% v/v solution of benzene in the room temperature mesophase ZLI-1132 liquid crystal in a 5 mm NMR tube. Over 60 lines were present in the spectrum (66 at 360 MHz and 64 at 600 MHz). The authors measured the frequency separation of the outermost lines as a function of temperature at 360 MHz, and fitted this to a third-order polynomial, giving ... 

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