Correlating fast and slow chemical shift spinning sideband patterns in solid-state NMR

Orr, Robin M.; Duer, Melinda J.; Ashbrook, Sharon E.

doi:10.1016/j.jmr.2005.03.001

Cited by 31 publications

(55 citation statements)

References 26 publications

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“…Dipolar dephasing experiments were also carried out with similar parameters and a dephasing interval of 1 ms. Two-dimensional CP CSA-amplified PASS experiments were performed using the pulse sequence of Orr et al [28,29] The total scaling factor is given by N T ¼ (n PASS þ 1)N, where N is the scaling factor determined by the timing of the five π pulses and n PASS is the number of additional five π pulse blocks. Cogwheel phase cycling was employed to reduce the length of the phase cycle required [39].…”

Section: Solid-state Nmr Spectroscopymentioning

confidence: 99%

“…For nuclear sites that possess high local symmetry, resulting in small anisotropies, "amplification" experiments have also recently been developed [27], increasing the apparent magnitude of the interaction (by a user-defined scaling factor) and enabling more accurate measurement. The experiment used in this work, the CSA-amplified PASS approach [28,29], has been used successfully to investigate 1 H, 13 C, 31 P and 89 Y local environments in a range of materials, and correlations with local structural parameters, e.g., bond distances or point symmetry, demonstrated [29][30][31][32][33]. For ZIFs, solid-state NMR spectroscopy can provide information on the type and relative proportions of linkers present, and the number of crystallographically-distinct molecules present in the asymmetric unit.…”

Section: Introductionmentioning

confidence: 99%

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Investigation of zeolitic imidazolate frameworks using 13 C and 15 N solid-state NMR spectroscopy

Sneddon

Kahr

Orsi

et al. 2017

Solid State Nuclear Magnetic Resonance

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Zeolitic imidazolate frameworks (ZIFs) are a subclass of metal-organic frameworks (MOFs) with extended threedimensional networks of transition metal nodes (bridged by rigid imidazolate linkers), with potential applications in gas storage and separation, sensing and controlled delivery of drug molecules. Here, we investigate the use of 13 C and 15 N solid-state NMR spectroscopy to characterise the local structure and disorder in a variety of singleand dual-linker ZIFs. In most cases, a combination of a basic knowledge of chemical shifts typically observed in solution-state NMR spectroscopy and the use of dipolar dephasing NMR experiments to reveal information about quaternary carbon species are combined to enable spectral assignment. Accurate measurement of the anisotropic components of the chemical shift provided additional information to characterise the local environment and the possibility of trying to understand the relationships between NMR parameters and both local and long-range structure. First-principles calculations on some of the simpler, ordered ZIFs were possible, and provided support for the spectral assignments, while comparison of these model systems to more disordered ZIFs aided interpretation of the more complex spectra obtained. It is shown that 13 C and 15 N NMR are sufficiently sensitive to detect small changes in the local environment, e.g., functionalisation of the linker, crystallographic inequivalence and changes to the framework topology, while the relative proportion of each linker present can be obtained by comparing relative intensities of resonances corresponding to chemically-similar species in cross polarisation experiments with short contact times. Therefore, multinuclear NMR spectroscopy, and in particular the measurement of both isotropic and anisotropic parameters, offers a useful tool for the structural study of ordered and, in particular, disordered ZIFs.

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Section: Solid-state Nmr Spectroscopymentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Investigation of zeolitic imidazolate frameworks using 13 C and 15 N solid-state NMR spectroscopy

Sneddon

Kahr

Orsi

et al. 2017

Solid State Nuclear Magnetic Resonance

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“…With respect to the anisotropy of the shift interaction, methods have been introduced that are not only capable of recoupling the inhomogeneity averaged out by the fast mechanical rotation, but also amplifying it, as if the experiment was performed at a slower and fictitious spinning rate. [37][38][39][40][41][42] This allows for more precise measurements of the full shielding tensor than those that one can achieve under static conditions or by spinning the sample at lower rates. [38] With respect to the chemical shift interaction, the following convention of NMR parameters is adopted in this study: [43] …”

Section: Introductionmentioning

confidence: 99%

Columnar self-assembly of N,N′,N′′-trihexylbenzene-1,3,5-tricarboxamides investigated by means of NMR spectroscopy and computational methods in solution and the solid state

Banach

Invernizzi

Baudin

et al. 2017

Phys. Chem. Chem. Phys.

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“…2). We have determined the chemical shift parameters using both a sideband-sideband correlation experiment, using CSA-amplified 2D-PASS, [16] and a powder-sideband correlation experiment, MAS-CSA. [10,11] Inspection of the powder-sideband correlation pattern, shows clearly that there are two components to this signal, which cannot be seen by eye in the sideband-sideband correlation pattern.…”

Section: Resultsmentioning

confidence: 99%

“…The 31 P CSA-amplified (2D-PASS) [16] spectrum was recorded at an actual spinning rate of 8 kHz, with a scaling factor of N = 3.4, www.interscience.wiley.com/journal/mrc giving an effective indirect dimension spinning rate of 2353 Hz. There were 32 t 1 data points collected, with 64 scans per point using a cogwheel phase cycling scheme.…”

Section: Methodsmentioning

confidence: 99%

Correlating sideband patterns with powder patterns for accurate determination of chemical shift parameters in solid‐state NMR

Ironside¹,

Reid²,

Duer³

2008

Magnetic Reson in Chemistry

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Powder patterns and sideband patterns have different strengths when it comes to using them to determine chemical shift parameters. Here, we show that chemical shift parameters can be determined with high accuracy by analysing the correlation pattern from a 2D experiment which correlates a powder pattern in the indirect dimension with a sideband pattern in the direct dimension. The chemical shift parameters so determined have greater accuracy than those obtained by analysing a sideband or powder pattern alone, for the same signal-to-noise ratio. This method can be applied for both resolved correlation patterns and to cases where two components share similar isotropic chemical shifts. The methodology is demonstrated in this paper, both theoretically and experimentally, on the (31)P signals of the bis-phosphonate drug, pamidronate.

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Correlating fast and slow chemical shift spinning sideband patterns in solid-state NMR

Cited by 31 publications

References 26 publications

Investigation of zeolitic imidazolate frameworks using 13 C and 15 N solid-state NMR spectroscopy

Investigation of zeolitic imidazolate frameworks using 13 C and 15 N solid-state NMR spectroscopy

Columnar self-assembly of N,N′,N′′-trihexylbenzene-1,3,5-tricarboxamides investigated by means of NMR spectroscopy and computational methods in solution and the solid state

Correlating sideband patterns with powder patterns for accurate determination of chemical shift parameters in solid‐state NMR

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