|
authors |
Coelho, C; Rocha, J; Madhu, PK; Mafra, L |
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nationality |
International |
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journal |
JOURNAL OF MAGNETIC RESONANCE |
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author keywords |
(1)H; Homonuclear techniques; 2D homonuclear correlation; Solid-state NMR; Lee-Goldburg; High-resolution proton decoupling; LG decoupling; CRAMPS techniques; Inorganic-organic hybrids materials; FSLG; PMLG |
|
keywords |
STATE NMR-SPECTROSCOPY; NUCLEAR-MAGNETIC-RESONANCE; ANGLE-SPINNING NMR; DIPOLAR-CORRELATION SPECTROSCOPY; MULTIPLE PULSE NMR; MAS C-13 NMR; CHEMICAL-SHIFT; THROUGH-BOND; HETERONUCLEAR DIPOLAR; POLARIZATION TRANSFER |
|
abstract |
Elucidating the local environment of the hydrogen atoms is an important problem in materials science. Because (1)H spectra in solid-state nuclear magnetic resonance (NMR) suffer from low resolution due to homogeneous broadening, even under magic-angle spinning (MAS), information of chemical interest may only be obtained using certain high-resolution (1)H MAS techniques. (1)H Lee-Goldburg (LG) CRAMPS (Combined Rotation And Multiple-Pulse Spectroscopy) methods are particularly well suited for studying inorganic-organic hybrid materials, rich in (1)H nuclei. However, setting up CRAMPS experiments is time-consuming and not entirely trivial, facts that have discouraged their widespread use by materials scientists. To change this status quo, here we describe and discuss some important aspects of the experimental implementation of CRAMPS techniques based on LG decoupling schemes, such as FSLG (Frequency Switched), and windowed and windowless PMLG (Phase Modulated). In particular, we discuss the influence on the quality of the (1)H NMR spectra of the different parameters at play, for example LG (Lee-Goldburg) pulses, radio-frequency (rf) phase, frequency switching, and pulse imperfections, using glycine and adamantane as model compounds. The efficiency and robustness of the different LG-decoupling schemes is then illustrated on the following materials: organo-phosphorus ligand, N-(phosphonomethyl)iminodiacetic acid [H(4)pmida] [1], and inorganic-organic hybrid materials (C(4)H(12)N(2))[Ge(2)(pmida)(2)OH(2)].4H(2)O [II] and (C(2)H(5)NH(3))[Ti(H(1.5)PO(4))(PO(4))](2) H(2)O [111]. (C) 2008 Elsevier Inc. All rights reserved. |
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publisher |
ACADEMIC PRESS INC ELSEVIER SCIENCE |
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issn |
1090-7807 |
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year published |
2008 |
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volume |
194 |
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issue |
2 |
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beginning page |
264 |
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ending page |
282 |
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digital object identifier (doi) |
10.1016/j.jmr.2008.07.019 |
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web of science category |
Biochemical Research Methods; Physics, Atomic, Molecular & Chemical; Spectroscopy |
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subject category |
Biochemistry & Molecular Biology; Physics; Spectroscopy |
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unique article identifier |
WOS:000259952000013
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