Accurate and Precise Measurement of Heteronuclear Long-Range Couplings by a Gradient-Enhanced Two-Dimensional Multiple-Bond Correlation Experiment

Sheng, Shuqun; Halbeek, Herman van

doi:10.1006/jmre.1997.1318

Cited by 36 publications

(12 citation statements)

References 13 publications

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“…Finally, there is also the PS-GHMBC experiment proposed by Sheng and van Hallbeek . The extraction of heteronuclear long-range coupling information from this experiment is considerably more cumbersome than the examination of a slice from the data matrix and the measurement of the antiphase limbs of a multiplet.…”

Section: Methods For Direct and Long-range 1h−15n Heteronuclear Shift...mentioning

confidence: 99%

“…Their experiment, which has been given the acronym GSQMBC, offers improved F 1 resolution relative to the multiple quantum-based sequences in the same sense that GHSQC differs from GHMQC. 32 Sheng and van Halbeek 43 have also reported a phase-sensitive long-range experiment, which they have labeled PS-GHMBC. In mid-1998, Wagner and Berger 44 reported a different approach to a more uniform long-range coupling excitation in an experiment they called ACCORD-HMBC.…”

Section: Pep-ghsqc-tocsymentioning

confidence: 99%

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Long-Range ¹H−¹⁵N Heteronuclear Shift Correlation at Natural Abundance

Martin¹,

Hadden²

2000

J. Nat. Prod.

193

187

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Despite the inherently low sensitivity of (15)N NMR because of its low gyromagnetic ratio (gamma(N)) and its relatively low natural abundance (0.37%), this important nuclide still has useful potential as a structural probe even at natural abundance. Inverse-detected NMR methods coupled with major advances in NMR probe designs have made it possible to acquire long-range (1)H-(15)N heteronuclear shift correlation data on samples as small as a micromole overnight. Chemical shift referencing schemes for (15)N and the range of (15)N shifts are discussed, followed by a discussion of the currently available pulse sequences, pulse calibration, parametrization and processing of long-range (1)H-(15)N data, and the implications of probe selection. These topics are followed by a review of the applications contained in the literature that have utilized (1)H-(15)N heteronuclear shift correlation experiments at natural abundance, with emphasis placed on the observed long-range coupling pathways.

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Section: Methods For Direct and Long-range 1h−15n Heteronuclear Shift...mentioning

confidence: 99%

Section: Pep-ghsqc-tocsymentioning

confidence: 99%

Long-Range ¹H−¹⁵N Heteronuclear Shift Correlation at Natural Abundance

Martin¹,

Hadden²

2000

J. Nat. Prod.

193

187

View full text Add to dashboard Cite

show abstract

“…A modified WATERGATE pulse sequence (54, 55) was used for one‐dimensional NMR with 16 000 complex data points. DPFGSE‐TOCSY (mixing time, 40–90ms) (56, 57) and DPFGSE‐ROESY (mixing time, 30–400 ms) (58) were used for two‐dimensional NMR at 5°C. Complex data points of 2048 in the t 2 dimension, 300–600 t 1 increments and 64 scans for each t 1 increment were used.…”

Section: Methodsmentioning

confidence: 99%

Peptide analogs from E‐cadherin with different calcium‐binding affinities

Yang

Tsai

Kats

et al. 2000

The Journal of Peptide Research

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Cadherins are a family of calcium-dependent cell-surface proteins that are fundamental in controlling the development and maintenance of tissues. Motif B of E-cadherin seems to be a crucial calcium-binding site as single point mutations (D134A and D134K) completely inactivate its adhesion activity. We analyzed peptide models corresponding to motif B (amino acids 128-144) as well as selected mutations of this motif. Our NMR studies showed that this motif B sequence is actually an active calcium-binding region, even in the absence of the rest of the cadherin molecule. We found that the binding affinity of this motif is very sensitive to mutations. For example, our peptide P128-144 with the native calcium-binding sequence has an affinity of Kd 0.4 mM, whereas the mutants P128-144/ D134A and P128-144/D134K containing the replacement of Asp134 by Ala and Lys, have Kd values of only 1.5 and 11 mM, respectively. Removing Asp at position 134, which correlates with the loss of adhesion activity, decreases calcium-binding affinity 20-fold. Ala132, along with residues Asp134, Asp136 and Asn143, is involved in calcium binding in solution. We also demonstrated that the calcium-binding affinity can be increased 3-fold when an additional Asp is introduced at position 132. In 50% organic solvent, this binding affinity of peptide P128-144/A132D (17-mer) from E-cadherin is similar to that of peptide P72-100/C73-77-91A (29-mer) from alpha-lactalbumin.

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“…Transients (128) were recorded for each t 1 increment. Long range 1 H- 13 C couplings were detected by choosing dephasing±phasing delay times (t) of 30 and 40 ms (37). BASHD-TOCSY ( 38) experiments were recorded with a mixing time of 80 ms and 128 transients.…”

Section: Nmr Experimentsmentioning

confidence: 99%

Synthesis, characterization and solution structure of tethered oligonucleotides containing an internal 3'-phosphoglycolate, 5'-phosphate gapped lesion

Junker

Hoehn²,

Bunt³

et al. 2002

Nucleic Acids Research

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Bleomycins (BLMs) are antitumor antibiotics that in the presence of iron and oxygen mediate DNA damage by 4'-hydrogen atom abstraction of pyrimidines 3' to guanines. The resulting 4'-deoxyribose radicals can be trapped by O2 and ultimately result in the formation of base-propenal and gapped DNA with 3'-phosphoglycolate (3'-PG) and 5'-phosphate (5'-P) ends. The role of this lesion in triggering double-strand cleavage of duplex DNA by a single BLM molecule and the mechanism by which this lesion is repaired in vivo remain unsolved problems. The structure of these lesions is an essential step in addressing both of these problems. Duplex DNAs (13mers containing tethered hexaethylene glycol linkers) with GTAC and GGCC cleavage sites have been synthesized in which gaps containing 3'-PG and 5'-P ends at the sites of BLM cleavage have been inserted. The former sequence represents a hot spot for double-strand cleavage, while the latter is a hot spot for single-strand cleavage. Analytical methods to characterize the lesioned products have been developed. These oligonucleotides have been examined using 2D NMR methods and molecular modeling. The studies reveal that the lesioned DNAs are B-form and the 3'-PG and 5'-P are extrahelical. The base opposite the gap and the base pairs adjacent to the gap remain well stacked in the DNA duplex. Titrations of the lesioned GGCC oligomer with HOO-CoBLM leads to a mixture of complexes, in contrast to results of a similar titration with the lesioned GTAC oligomer.

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Accurate and Precise Measurement of Heteronuclear Long-Range Couplings by a Gradient-Enhanced Two-Dimensional Multiple-Bond Correlation Experiment

Cited by 36 publications

References 13 publications

Long-Range ¹H−¹⁵N Heteronuclear Shift Correlation at Natural Abundance

Long-Range ¹H−¹⁵N Heteronuclear Shift Correlation at Natural Abundance

Peptide analogs from E‐cadherin with different calcium‐binding affinities

Synthesis, characterization and solution structure of tethered oligonucleotides containing an internal 3'-phosphoglycolate, 5'-phosphate gapped lesion

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Accurate and Precise Measurement of Heteronuclear Long-Range Couplings by a Gradient-Enhanced Two-Dimensional Multiple-Bond Correlation Experiment

Cited by 36 publications

References 13 publications

Long-Range 1H−15N Heteronuclear Shift Correlation at Natural Abundance

Long-Range 1H−15N Heteronuclear Shift Correlation at Natural Abundance

Peptide analogs from E‐cadherin with different calcium‐binding affinities

Synthesis, characterization and solution structure of tethered oligonucleotides containing an internal 3'-phosphoglycolate, 5'-phosphate gapped lesion

Contact Info

Product

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Long-Range ¹H−¹⁵N Heteronuclear Shift Correlation at Natural Abundance

Long-Range ¹H−¹⁵N Heteronuclear Shift Correlation at Natural Abundance