A broadband ADEQUATE pulse sequence using chirp pulses

Köck, Matthias; Kerssebaum, Rainer; Bermel, Wolfgang

doi:10.1002/mrc.1097

Cited by 64 publications

(67 citation statements)

References 36 publications

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“…Contiguous non-protonated carbon resonances can be spanned by either a variant of the HMBC [19] experiment or an experiment such as 1,n-ADEQUATE. [16] The structure of strychnine shown below summarizes the carbon-carbon bond connectivities derived from HSQC-ADEQUATE data. Solid lines in either red or blue indicate adjacent protonated carbon pairs.…”

Section: Resultsmentioning

confidence: 99%

HSQC‐ADEQUATE: an investigation of data requirements

Martin¹,

Hilton²,

Willcott³

et al. 2011

Magnetic Reson in Chemistry

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Utilizing (13)C-(13)C connectivity networks for the assembly of carbon skeletons from HSQC-ADEQUATE spectra was recently reported. HSQC-ADEQUATE data retain the resonance multiplicity information of the multiplicity-edited GHSQC spectrum and afford a significant improvement in the signal-to-noise (s/n) ratio relative to the 1,1-ADEQUATE data used in the calculation of the HSQC-ADEQUATE spectrum by unsymmetrical indirect covariance (UIC) processing methods. The initial investigation into the computation of HSQC-ADEQUATE correlation plots utilized overnight acquisition of the 1,1-ADEQUATE data used for the calculation. In this communication, we report the results of an investigation of the reduction in acquisition time for the 1,1-ADEQUATE data to take advantage of the s/n gain during the UIC processing to afford the final HSQC-ADEQUATE correlation plot. Data acquisition times for the 1,1-ADEQUATE spectrum can be reduced to as little as a few hours, while retaining excellent s/n ratios and all responses contained in spectra computed from overnight data acquisitions. Concatenation of multiplicity-edited GHSQC and 1,1-ADEQUATE data also allows the interrogation of submilligram samples with 1,1-ADEQUATE data when using spectrometers equipped with 1.7-mm Micro CryoProbes ™.

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Section: Resultsmentioning

confidence: 99%

HSQC‐ADEQUATE: an investigation of data requirements

Martin¹,

Hilton²,

Willcott³

et al. 2011

Magnetic Reson in Chemistry

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“…We use, wherever possible, broad-band excitation and inversion pulses 17,18 -an approach proposed previously for inversion pulses. 19 The determination of 1 J CC values from the nonrefocused INADEQUATE spectra is trivial because of large separation of the two components of the one-bond antiphase doublets. Prior to peak picking, it maybe beneficial to add or subtract the two spectra, providing both contain one-bond cross peaks with sufficient intensity.…”

Section: Resultsmentioning

confidence: 99%

¹³C‐detected IPAP‐INADEQUATE for simultaneous measurement of one‐bond and long‐range scalar or residual dipolar coupling constants

Jin

Uhrı́n

2007

Magnetic Reson in Chemistry

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The sensitivity of cryoprobes, which are rapidly becoming available, means that the measurement of coupling constants involving 13C, 13C pairs at the natural abundance of 13C can now, in principle, be done by using tens rather then hundreds of milligrams of compounds. However, a robust method that would yield reliable values of small long-range carbon--carbon coupling constants is still missing. In this Communication, we describe a novel 13C-detected incredible natural-abundance double-quantum transfer experiment (INADEQUATE) experiment for simultaneous correlation of one-bond and long-range 13C- 13C pairs and the measurement of both types of coupling constants in 13C natural abundance samples. This method yields accurate values of one-bond and long-range coupling constants by manipulation of pure phase in-phase (IP) and antiphase (AP) doublets, and is referred to as 13C-detected IPAP-INADEQUATE. It is illustrated by the measurement of interglycosidic (3)J(CCOC) coupling constants in a disaccharide molecule providing important information about the conformation of the glycosidic linkage. Owing to the simplicity of INADEQUATE spectra the carbon-carbon coupling constants are particularly suitable for studies of partially oriented molecules through the measurement of carbon-carbon residual dipolar couplings (RDCs). An example of this approach is presented. We expect the method to find a variety of applications in the conformational analysis of small molecules, determination of diastereoisomers and enantiomers, and studies of molecules in aligned media.

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“…The performance of these pulses is compared with the composite adiabatic pulse scheme [19] implemented as a smoothed Chirp pulse [44,45] in standard Bruker software .…”

Section: Burbop Compared To Refocusing With Pp Pulsesmentioning

confidence: 99%

“…The best broadband refocusing performance available in the standard Bruker pulse library satisfying the required conservative pulse power limits is obtained using the pulse designated Chirp80 [45]. This pulse is constructed from three adiabatic inversion pulses with pulse lengths in the ratio 1:2:1 [19].…”

Section: Three Adiabatic Inversion Pulsesmentioning

confidence: 99%

New strategies for designing robust universal rotation pulses: Application to broadband refocusing at low power

Skinner

Gershenzon

Nimbalkar

et al. 2012

Journal of Magnetic Resonance

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Broadband inversion pulses that rotate all magnetization components 180• about a given fixed axis are necessary for refocusing and mixing in highresolution NMR spectroscopy. The relative merits of various methodologies for generating pulses suitable for broadband refocusing are considered. The de novo design of 180• universal rotation pulses (180 • U R ) using optimal control can provide improved performance compared to schemes which construct refocusing pulses as composites of existing pulses. The advantages of broadband universal rotation by optimized pulses (BURBOP) are most evident for pulse design that includes tolerance to RF inhomogeneity or miscalibration. We present new modifications of the optimal control algorithm that incorporate symmetry principles and relax conservative limits on peak RF pulse amplitude for short time periods that pose no threat to the probe. We apply them to generate a set of 180• BU RBOP pulses suitable for widespread use in 13 C spectroscopy on the majority of available probes.

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A broadband ADEQUATE pulse sequence using chirp pulses

Cited by 64 publications

References 36 publications

HSQC‐ADEQUATE: an investigation of data requirements

HSQC‐ADEQUATE: an investigation of data requirements

¹³C‐detected IPAP‐INADEQUATE for simultaneous measurement of one‐bond and long‐range scalar or residual dipolar coupling constants

New strategies for designing robust universal rotation pulses: Application to broadband refocusing at low power

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A broadband ADEQUATE pulse sequence using chirp pulses

Cited by 64 publications

References 36 publications

HSQC‐ADEQUATE: an investigation of data requirements

HSQC‐ADEQUATE: an investigation of data requirements

13C‐detected IPAP‐INADEQUATE for simultaneous measurement of one‐bond and long‐range scalar or residual dipolar coupling constants

New strategies for designing robust universal rotation pulses: Application to broadband refocusing at low power

Contact Info

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¹³C‐detected IPAP‐INADEQUATE for simultaneous measurement of one‐bond and long‐range scalar or residual dipolar coupling constants