Triplet NOAH supersequences optimised for small molecule structure characterisation
Corresponding Author
Tim D.W. Claridge
Department of Chemistry, University of Oxford, Chemistry Research Laboratory, Oxford, UK
Correspondence
Tim D. W. Claridge, Department of Chemistry, University of Oxford, Chemistry Research Laboratory, Mansfield Road, Oxford OX1 3TA, UK.
Email: [email protected]
Search for more papers by this authorMaksim Mayzel
Application Science CH, MRS Division, Bruker BioSpin AG, Fällanden, Switzerland
Search for more papers by this authorĒriks Kupče
Advanced Applications Development, Bruker UK Ltd., Coventry, UK
Search for more papers by this authorCorresponding Author
Tim D.W. Claridge
Department of Chemistry, University of Oxford, Chemistry Research Laboratory, Oxford, UK
Correspondence
Tim D. W. Claridge, Department of Chemistry, University of Oxford, Chemistry Research Laboratory, Mansfield Road, Oxford OX1 3TA, UK.
Email: [email protected]
Search for more papers by this authorMaksim Mayzel
Application Science CH, MRS Division, Bruker BioSpin AG, Fällanden, Switzerland
Search for more papers by this authorĒriks Kupče
Advanced Applications Development, Bruker UK Ltd., Coventry, UK
Search for more papers by this authorAbstract
A series of NMR supersequences are presented for the time-efficient structure characterisation of small molecules in the solution state. These triplet sequences provide HMBC, HSQC, and one homonuclear correlation experiment of choice according to the NMR by Ordered Acquisition using 1H detection principle. The experiments are demonstrated to be compatible with non-uniform sampling schemes and may be acquired and processed under full automation.
Supporting Information
| Filename | Description |
|---|---|
| mrc4887-sup-0001-Sup_Info.pdfPDF document, 1.4 MB |
Figure S1. Comparison of NOAH3-BSX spectra versus conventional data sets of andrographolide recorded with similar acquisition parameters. Left-hand traces derive from individual experiments and right-hand traces from NOAH modules. The corresponding spectra contain comparable information. The conventional DQF-COSY experiment shows artefacts typically associated with “rapid pulsing” (marked by dashed line) which are attenuated in the NOAH module at the expense of some residual artefacts arising from the intense methyl singlets (boxed). Figure S2. Andrographolide NOAH-3 BSN and BSRo data: NOESY (left) versus ROESY (right) data at 700 MHz (upper) and 500 MHz (lower). Table S1. Comparison of the time requirements for NOAH-2 experiments and NOAH-3 BSX experiments versus the total time for the separate correlation experiments. All data sets were collected as 1K*256 points (per individual module) across 7 ppm (1H) and 170 ppm (13C) windows, acquiring 2 transients per increment with a recovery delay (d1) of 1.5 s. Coupling constants were assumed to be 145 Hz (1JCH) and 8 Hz (2/3JCH) with mixing times as indicated in the table. For CLIP-COSY, JHH was set to a compromise value of 30 Hz. Fig S3. A comparison of ROESY spectra from NOAH-3 BSR experiments employing with either the phase-alternating spin-lock (left) or the off-resonance adiabatic sweeps (right) for ROE generation. The corresponding NOAH module is shown above each spectrum. Positive cross peaks (black) arise from exchange between hydroxyl protons and water. Data were collected at 500 MHz using a room temperature TBO probe for andrographolide (38 mM, DMSO). Both NOAH data sets were collected with 2 transients per increment with mixing times of 300 ms. The phase-alternating sequence comprised 694 cycles of pairs of 216 μs 180o pulses, whilst the high and low offset off-resonance pulses were each 150 ms amplitude-modulated WURST sweeps with B1(max) of 5 kHz applied at 9.5 and -0.5 ppm respectively. Fig S4. A comparison of signal intensities in spectrum projections extracted from conventional spectra (lower traces) vs the NOAH BSX modules (upper traces) of andrographolide (38 mM, DMSO, 700 MHz TXI probe). All spectra were collected with 2 transients per increment. |
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