<sup>67</sup>Zn QCPMG Solid-State NMR Studies of Zinc Complexes as Models for Metalloproteins

Larsen, Flemming H.; Lipton, Andrew S.; Jakobsen, Hans J.; Nielsen, Niels Chr.; Ellis, Paul D.

doi:10.1021/ja9839623

Cited by 70 publications

(83 citation statements)

References 26 publications

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“…We may, however, compare the span of 47 ppm in L-cysteine ethyl ester hydrochloride to two known chlorine chemical shift tensor spans of oxychloro anions, both determined from single-crystal 35 Cl studies: Ω ) 32.0 ( 1.2 ppm for NH 4 ClO 4 , 9 and Ω ) 40 ( 7 ppm for NaClO 3 . 6 The 35 Cl spectra acquired at 18.8 T. b Parameters determined from MAS, Hahn-echo, and QCPMG 35 Cl spectra acquired at 18.8 T. c Parameters determined from Hahn-echo 35 Cl spectra acquired at 18.8 and 9.4 T, and Hahn-echo 37 Cl spectra acquired at 9.4 T.…”

Section: Resultsmentioning

confidence: 99%

“…All of the spectra acquired at 9.4 T suffer to a certain extent from nonuniform rf excitation; nevertheless, fitting of the discontinuities in the spectra allows for the determination of C Q and η. NMR of the 37 Cl nucleus affords narrower line shapes due to its smaller quadrupole moment relative to 35 Cl; however, the lower natural abundance of 37 Cl results in spectra with lower signal-to-noise ratios relative to 35 Cl. Analyses of both 37 Cl and 35 Cl NMR spectra allow for more accurate and precise determinations of the EFG tensor parameters (Table 1). In Figure 4c, the QCPMG sidebands were deliberately spaced at relatively small (1 kHz) intervals about the transmitter frequency to faithfully mimic the envelope of the powder pattern obtained using a simple Hahn echo pulse sequence.…”

Section: Figurementioning

confidence: 99%

“…Experimental chlorine NMR static echo spectra of quinuclidine hydrochloride acquired for (a) 37 Cl at 9.4 T, (b) 35 Cl at 9.4 T, and (c) 35 Cl at 18.8 T, along with the best-fit simulations. Also shown in part (c) is the experimental 35 Cl QCPMG spectrum acquired at 18.8 T.…”

Section: Figurementioning

confidence: 99%

“…Figure 5. Experimental chlorine NMR static echo spectra of tris sarcosine calcium chloride acquired for (a) 37 Cl at 9.4 T, (b) 35 Cl at 9.4 T, and (c) 35 Cl at 18.8 T, along with the best-fit simulations. The experimental spectra shown in parts (a) and (b) suffer from nonuniform excitation across the ∼80 kHz breadth.…”

Section: Figurementioning

confidence: 99%

“…Chlorine has two NMR-active isotopes, 35 Cl (I ) 3/2; N. A. ) 75.53%; γ ) 2.6242 × 10 7 rad T -1 s -1 ; Q ) -82 mb 4 ) and 37 Cl (I ) 3/2; N. A. ) 24.47%; γ ) 2.1844 × 10 7 rad T -1 s -1 ; Q ) -64.6 mb 4c,5 ).…”

Section: Introductionmentioning

confidence: 99%

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High-Field Chlorine NMR Spectroscopy of Solid Organic Hydrochloride Salts: A Sensitive Probe of Hydrogen Bonding Environment

2001

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A series of organic hydrochloride salts has been investigated using solid-state 35 Cl and 37 Cl NMR spectroscopy at applied magnetic field strengths of 9.4 and 18.8 T. Magic-angle spinning, static Hahn-echo, and quadrupolar Carr-Purcell Meiboom-Gill (QCPMG) echo experiments have been applied to investigate the chlorine electric field gradient (EFG) and chemical shift (CS) tensors for L-tyrosine hydrochloride, L-cysteine methyl ester hydrochloride, L-cysteine ethyl ester hydrochloride, quinuclidine hydrochloride, and tris sarcosine calcium chloride. Chlorine-35 nuclear quadrupolar coupling constants for these compounds range from 2.23 to 5.25 MHz, and isotropic chemical shifts range from approximately 9 to 53 ppm relative to the chloride ion in aqueous solution. The results demonstrate the feasibility and benefits of high-field 35/37 Cl NMR studies of organic chloride salts. A discussion of the data in the context of the known X-ray or neutron diffraction structures for these compounds suggests that the chlorine EFG tensor is a valuable probe of hydrogen bonding to the chloride ion. Because the anisotropies of the CS tensors are rather small, precise determination of the chlorine CS tensors proved to be challenging and was only feasible for L-cysteine ethyl ester hydrochloride, where the span, Ω, was found to be 47 ( 4 ppm. This represents the first determination of Ω(Cl) from a powder sample. Results of ab initio calculations of the chlorine EFG and CS tensors in L-tyrosine hydrochloride are presented and compared with the experimental data.

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Section: Resultsmentioning

confidence: 99%

Section: Figurementioning

confidence: 99%

Section: Figurementioning

confidence: 99%

Section: Figurementioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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High-Field Chlorine NMR Spectroscopy of Solid Organic Hydrochloride Salts: A Sensitive Probe of Hydrogen Bonding Environment

2001

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Methoden der Festk��rper-NMR-Spektroskopie in der Chemie

2002

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A. Jerschow et al. und 29 Si. Wir behandeln daher zun‰chst die Spinwechselwirkungen, die bei solchen Kernen eine Rolle spielen, und stellen spektroskopische Methoden vor, mit denen sich diese Wechselwirkungen zur Vereinfachung der Spektren beeinflussen oder gar ausschalten lassen.In einem einfachen Beispiel wird eine w‰ssrige Lˆsung von 1-13 C-markiertem (10 %) Glycin mit einem p/2-Einzelpuls der Resonanzfrequenz von 13 C-Kernen bestrahlt. In dem resultierenden Spektrum (Abbildung 1) beobachtet man zwei gut aufgelˆste Signale, die den 13 C-angereicherten Carbonyl-C-Atomen und den in nat¸rlicher Isotopenverteilung (ca. 1 % 13

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Solid-State NMR Spectroscopic Methods in Chemistry

Laws

Bitter

Jerschow

2002

Angew. Chem. Int. Ed.

313

247

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Over the last decades, NMR spectroscopy has grown into an indispensable tool for chemical analysis, structure determination, and the study of dynamics in organic, inorganic, and biological systems. It is commonly used for a wide range of applications from the characterization of synthetic products to the study of molecular structures of systems such as catalysts, polymers, and proteins. Although most NMR experiments are performed on liquid-state samples, solid-state NMR is rapidly emerging as a powerful method for the study of solid samples and materials. This Review outlines some of the developments of solid-state NMR spectroscopy, including techniques such as cross-polarization, magic-angle spinning, multiple-pulse sequences, homo- and heteronuclear decoupling and recoupling techniques, multiple-quantum spectroscopy, and dynamic angle spinning, as well as their applications to structure determination. Modern solid-state NMR spectroscopic techniques not only produce spectra with a resolution close to that of liquid-state spectra, but also capitalize on anisotropic interactions, which are often unavailable for liquid samples. With this background, the future of solid-state NMR spectroscopy in chemistry appears to be promising, indeed.

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⁶⁷Zn QCPMG Solid-State NMR Studies of Zinc Complexes as Models for Metalloproteins

Cited by 70 publications

References 26 publications

High-Field Chlorine NMR Spectroscopy of Solid Organic Hydrochloride Salts: A Sensitive Probe of Hydrogen Bonding Environment

High-Field Chlorine NMR Spectroscopy of Solid Organic Hydrochloride Salts: A Sensitive Probe of Hydrogen Bonding Environment

Methoden der Festk��rper-NMR-Spektroskopie in der Chemie

Solid-State NMR Spectroscopic Methods in Chemistry

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67Zn QCPMG Solid-State NMR Studies of Zinc Complexes as Models for Metalloproteins

Cited by 70 publications

References 26 publications

High-Field Chlorine NMR Spectroscopy of Solid Organic Hydrochloride Salts: A Sensitive Probe of Hydrogen Bonding Environment

High-Field Chlorine NMR Spectroscopy of Solid Organic Hydrochloride Salts: A Sensitive Probe of Hydrogen Bonding Environment

Methoden der Festk��rper-NMR-Spektroskopie in der Chemie

Solid-State NMR Spectroscopic Methods in Chemistry

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Product

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⁶⁷Zn QCPMG Solid-State NMR Studies of Zinc Complexes as Models for Metalloproteins