Directly and indirectly detected through-bond heteronuclear correlation solid-state NMR spectroscopy under fast MAS

Mao, Kanmi; Pruski, Marek

doi:10.1016/j.jmr.2009.09.004

Cited by 70 publications

(87 citation statements)

References 44 publications

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“…As we shown, the transfer of magnetization realized by cross polarization from abundant spin (mainly 1 H) to rare spin (e.g.,: 13 C, 15 N, or 29 Si) is an approach that greatly improves the sensitivity. More recently, another method, referred to as dynamic nuclear polarization (DNP), [24] has become one of the most promising NMR tools for structural studies of condensed matter, as a result of incredible progress in hardware development during the last few years.…”

Section: Dynamic Nuclear Polarization Solid State Nuclear Magnetic Rementioning

confidence: 99%

“…This problem is in particular painful when rare spins are under investigation. To this group belong 13 C, 15 N, and 29 Si, which are very often building units of polymers. The natural abundance for 13 C is 1.1%, for 15 N is 0.37% while for 29 Si is 4.7%.…”

Section: Very Fast Magic Angle Spinning Solid State Nuclear Magnetic mentioning

confidence: 99%

“…To this group belong 13 C, 15 N, and 29 Si, which are very often building units of polymers. The natural abundance for 13 C is 1.1%, for 15 N is 0.37% while for 29 Si is 4.7%. In order to overcome the sensitivity problem, the SSNMR spectra of rare spins are typically obtained using CP (cross polarization) sequence [6] (Fig.…”

Section: Very Fast Magic Angle Spinning Solid State Nuclear Magnetic mentioning

confidence: 99%

“…Especially, the amine and amide groups in CNC-RhB conjugates could be detected, by 13 C and 15 N NMR, in order to illustrate the structural change during the switching process: CNC-RhB-close containing close-ring spiroamide and CNC-RhB-open containing open-ring spirolactam. Additionally, due to extraordinary sensitivity, it was possible to identify another structural form of CNC-RhB conjugates, which was revealed after the heat-treatment at 130°C (CNC-RhB-130°C), which was stabilized through an electrostatic interaction.…”

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Modern solid state NMR techniques and concepts in structural studies of synthetic polymers

Kaźmierski

Pawlak

Jeziorna

et al. 2016

Polym. Adv. Technol.

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In this mini-review, we present the solid state nuclear magnetic resonance (NMR) methods which trace the new tendency in structural studies of synthetic polymers. The review is organized into three sections. In the first part, short theoretical background and introduction to very fast magic angle spinning NMR technique with sample rotation 60 kHz are shown. The second part presents method for enhancing the sensitivity of NMR experiments by application of dynamic nuclear polarization magic angle spinning technique. In the third section, the power of the NMR crystallography approach which can be used for fine refinement of polymers structure on the atomic level is discussed.

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Section: Dynamic Nuclear Polarization Solid State Nuclear Magnetic Rementioning

confidence: 99%

Section: Very Fast Magic Angle Spinning Solid State Nuclear Magnetic mentioning

confidence: 99%

Section: Very Fast Magic Angle Spinning Solid State Nuclear Magnetic mentioning

confidence: 99%

mentioning

confidence: 99%

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Modern solid state NMR techniques and concepts in structural studies of synthetic polymers

Kaźmierski

Pawlak

Jeziorna

et al. 2016

Polym. Adv. Technol.

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“…7,8 Therefore, a combination of through-bond and through-space correlation experiments could be used to determine molecular structures and inter-molecular assemblies. Inspite of the development of a diverse set of dipolar-coupling driven experiments and their application to determine heteronuclear/homonuclear connectivity and distances, [9][10][11][12][13][14][15][16][17][18][19][20][21][22][23] relatively few experiments [24][25][26][27][28][29][30][31][32] make use of scalar coupling for structural studies due to its smaller magnitude, when compared to dipolar coupling, in solids. For example, the dipolar coupling between single bonded 13 C− 13 C pair is around 2 kHz, whereas the scalar coupling is only around 55 Hz.…”

Section: Introductionmentioning

confidence: 99%

Constant-time 2D and 3D through-bond correlation NMR spectroscopy of solids under 60 kHz MAS

Zhang

Ramamoorthy

2016

The Journal of Chemical Physics

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Establishing connectivity and proximity of nuclei is an important step in elucidating the structure and dynamics of molecules in solids using magic angle spinning (MAS) NMR spectroscopy. Although recent studies have successfully demonstrated the feasibility of proton-detected multidimensional solid-state NMR experiments under ultrafast-MAS frequencies and obtaining high-resolution spectral lines of protons, assignment of proton resonances is a major challenge. In this study, we first re-visit and demonstrate the feasibility of 2D constant-time uniform-sign cross-peak correlation (CTUC-COSY) NMR experiment on rigid solids under ultrafast-MAS conditions, where the sensitivity of the experiment is enhanced by the reduced spin-spin relaxation rate and the use of low radio-frequency power for heteronuclear decoupling during the evolution intervals of the pulse sequence. In addition, we experimentally demonstrate the performance of a proton-detected pulse sequence to obtain a 3D 1 H/ 13 C/ 1 H chemical shift correlation spectrum by incorporating an additional cross-polarization period in the CTUC-COSY pulse sequence to enable proton chemical shift evolution and proton detection in the incrementable t 1 and t 3 periods, respectively. In addition to through-space and through-bond 13 C/ 1 H and 13 C/ 13 C chemical shift correlations, the 3D 1 H/ 13 C/ 1 H experiment also provides a COSY-type 1 H/ 1 H chemical shift correlation spectrum, where only the chemical shifts of those protons, which are bonded to two neighboring carbons, are correlated. By extracting 2D F1/F3 slices ( 1 H/ 1 H chemical shift correlation spectrum) at different 13 C chemical shift frequencies from the 3D 1 H/ 13 C/ 1 H spectrum, resonances of proton atoms located close to a specific carbon atom can be identified. Overall, the through-bond and through-space homonuclear/heteronuclear proximities determined from the 3D 1 H/ 13 C/ 1 H experiment would be useful to study the structure and dynamics of a variety of chemical and biological solids. C 2016 AIP Publishing LLC. [http://dx

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Study of Intermolecular Interactions in the Corrole Matrix by Solid‐State NMR under 100 kHz MAS and Theoretical Calculations

et al. 2013

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Directly and indirectly detected through-bond heteronuclear correlation solid-state NMR spectroscopy under fast MAS

Cited by 70 publications

References 44 publications

Modern solid state NMR techniques and concepts in structural studies of synthetic polymers

Modern solid state NMR techniques and concepts in structural studies of synthetic polymers

Constant-time 2D and 3D through-bond correlation NMR spectroscopy of solids under 60 kHz MAS

Study of Intermolecular Interactions in the Corrole Matrix by Solid‐State NMR under 100 kHz MAS and Theoretical Calculations

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