Practical aspects of Lee-Goldburg based CRAMPS techniques for high-resolution 1H NMR spectroscopy in solids: implementation and applications.
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] [I], and inorganic-organic hybrid materials (C(4)H(12)N(2))[Ge(2)(pmida)(2)OH(2)] x 4H(2)O [II] and (C(2)H(5)NH(3))[Ti(H(1.5)PO(4))(PO(4))](2) x H(2)O [III].
Coelho
Cristina
C
Department of Chemistry, CICECO, University of Aveiro, Aveiro, Portugal.
Rocha
João
J
Madhu
P K
PK
Mafra
Luís
L
D000465:Algorithms; D003198:Computer Simulation; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008422:Materials Testing / Q000379:methods*; D008956:Models, Chemical; D011522:Protons; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
D011522:Protons