Standard Parameter Sets
The tables below list the names of standard parameter sets, the spectrometer they are currently available on, and some notes about the experiments. These parameters can be read in either with "rpar", or by selecting the parameter set when creating a new dataset with "edc". After reading the desired parameters, executing "gpro" to set the appropriate pulse lengths and attenuations and "rga" to optimise the receiver gain should be all that is needed before starting acquisition. Parameters you may consider optimising are the number of scans (NS), the number of increments (TD), the carrier frequencies (O1/O2/O3) and the sweep widths (SW).
For longer experiments, particularly those in aqueous solvents, pulse calibration is recommended.
The basic experiments
For a full structure determination of an unknown compound I recommend running UCSD_1H, UCSD_CLIP_COSY, UCSD_13C_HSQC_ASAP and UCSD_13C_HMBC to start with. Other spectra that may be useful can be run using UCSD_TOCSY, UCSD_NOESY UCSD_ROESY, UCSD_13C_HSQC_TOCSY and UCSD_13C_H2BC. For measuring 3JHH coupling constants use UCSD_1H and for nJHC coupling constants use UCSD_HSQMBC_IPAP and UCSD_HSQMBC_TOCSY_IPAP.
1D Proton Experiments
| Parameter Set | Spectrometer | Notes |
|---|---|---|
| UCSD_1H | npa600, bma600 |
1D 1H, with 30o pulse and short relaxation delay for rapid pulsing |
| UCSD_1H_PRESAT | npa600, bma600 | 1D 1H with presaturation |
| UCSD_1H_ES | npa600, bma600 |
1D 1H with excitation sculpting, allows suppression of two resonances, reference |
| UCSD_1H_JR | npa600, bma600 |
1D 1H with jump-return solvent suppression good for nucleic acids reference |
| UCSD_1H_PSYCHE | npa600, bma600 |
1D 1H pure shift spectrum homo-decoupling via PSYCHE reference |
| UCSD_1H_HOMODEC | npa600, bma600 |
1D 1H with selective homodecoupling |
| UCSD_TOCSY_1D | npa600, bma600 |
1D 1H TOCSY with selective excitation |
| UCSD_NOESY_1D | npa600, bma600 |
1D 1H NOESY with selective excitation |
| UCSD_NOESY_1D_PRESAT | npa600, bma600 |
1D 1H NOESY with presaturation, good for metabolomics |
1D Deuterium Experiments
| Parameter Set | Spectrometer | Notes |
|---|---|---|
| UCSD_2H | npa600, bma600 |
1D 2H for tuning 2H channel |
1D Carbon Experiments
| Parameter Set | Spectrometer | Notes |
|---|---|---|
| UCSD_13C | npa600, bma600 |
1D 13C, direct detect with 1H decoupling with 30o pulse and short relaxation delay for rapid pulsing |
| UCSD_13C_DEPT45 | npa600, bma600 |
1D 13C DEPT, with 45o pulse, all peaks positive reference |
| UCSD_13C_DEPT90 | npa600, bma600 |
1D 13C DEPT, with 90o pulse, shows only CH resonances reference |
| UCSD_13C_DEPT135 | npa600, bma600 |
1D 13C DEPT, with 135o pulse, shows CH and CH3 peaks positive and CH2 peaks negative reference |
| UCSD_13C_APT | npa600, bma600 |
1D 13C APT CH and CH3 peaks positive and C and CH2 peaks negative |
| UCSD_13C_INEPT | npa600 |
1D 13C INEPT CH and CH3 peaks positive and CH2 peaks negative |
| UCSD_13C_DEPTQ | npa600 |
1D 13C DEPTQ CH and CH3 peaks positive and and C and CH2 peaks negative reference |
| UCSD_13C_SELINQUATE | bma600 |
1D 13C selective INADEQUATE good for measuring specific 1JCC coupling constants reference |
1D Nitrogen Experiments
| Parameter Set | Spectrometer | Notes |
|---|---|---|
| UCSD_15N | npa600 |
1D 15N, direct detect with 1H decoupling with 30o pulse and short relaxation delay for rapid pulsing |
| UCSD_15N_APT | npa600 |
1D 15N with 1H decoupling shows NH peaks positive and NH2 peaks negative |
| UCSD_15N_DEPT135 | npa600 |
1D 15N with 1H decoupling shows NH peaks positive and NH2 peaks negative |
| UCSD_15N_DEPTQ | npa600 |
1D 15N with 1H decoupling shows NH peaks positive and NH2 peaks negative |
| UCSD_15N_INEPT | npa600 |
1D 15N INEPT shows NH peaks positive and NH2 peaks negative |
2D 1H-1H Experiments
| Parameter Set | Spectrometer | Notes |
|---|---|---|
| UCSD_COSY | npa600, bma600 |
2D 1H-1H COSY not phase sensitive, requires magnitude processing |
| UCSD_COSY_PRESAT | npa600, bma600 |
2D 1H-1H COSY with presaturation not phase sensitive, requires magnitude processing |
| UCSD_COSY_CLIP | npa600, bma600 |
2D 1H-1H CLIP-COSY gives cleaner spectra than UCSD_COSY but slightly less sensitive, phase sensitive reference |
| UCSD_DQF-COSY | npa600, bma600 |
2D 1H-1H DQF-COSY least sensitive COSY but best diagonal suppression reference |
| UCSD_DQF-COSY_PRESAT | npa600, bma600 |
2D 1H-1H DQF-COSY with presaturation reference |
| UCSD_DQF-COSY_ES | npa600, bma600 |
2D 1H-1H DQF-COSY with multiple solvent suppression reference |
| UCSD_TOCSY | npa600, bma600 | 2D 1H-1H TOCSY with DIPSI2 spinlock |
| UCSD_TOCSY_PRESAT | npa600, bma600 |
2D 1H-1H TOCSY with DIPSI2 spinlock and presaturation |
| UCSD_TOCSY_ES | npa600, bma600 |
2D 1H-1H TOCSY with DIPSI2 spinlock and multiple solvent suppression |
| UCSD_TOCSY_BSHD | npa600, bma600 |
Pure shift 2D 1H-1H TOCSY with DIPSI2 spinlock |
| UCSD_NOESY | npa600, bma600 |
2D 1H-1H NOESY with zero quantum suppression reference |
| UCSD_NOESY_PRESAT | npa600, bma600 |
2D 1H-1H NOESY with zero quantum suppression and presaturation |
| UCSD_NOESY_ES | npa600, bma600 |
2D 1H-1H NOESY with zero quantum suppression and multiple solvent suppression |
| UCSD_ROESY | npa600, bma600 |
2D 1H-1H ROESY with two pulse spinlock reference |
| UCSD_ROESY_PRESAT | npa600, bma600 |
2D 1H-1H ROESY with two pulse spinlock and presaturation reference |
| UCSD_ROESY_ES | npa600, bma600 |
2D 1H-1H ROESY with two pulse spinlock and excitation sculpting reference |
| UCSD_INADEQUATE | bma600 |
2D 13C-13C INADEQUATE 13C-13C double quantum correlation, very insensitive |
2D 1H-13C Experiments
| Parameter Set | Spectrometer | Notes |
|---|---|---|
| UCSD_13C_HETCOR | bma600 |
2D 13C-1H HETCOR not as sensitive as HSQC |
| UCSD_13C_HSQC | npa600, bma600 |
2D 1H-13C HSQC with multiplicity editing, adiabatic pulses, matched sweep pulse |
| UCSD_13C_HSQC_ASAP | npa600, bma600 |
2D 1H-13C HSQC with multiplicity editing, adiabatic pulses, matched sweep pulse, ASAP |
| UCSD_13C_HSQC_PRESAT | npa6000 |
2D 1H-13C HSQC with multiplicity editing and solvent suppression via presaturation |
| UCSD_13C_HSQC_BBHD | npa600, bma600 | Pure shift 2D 1H-13C HSQC |
| UCSD_13C_HSQC_BBHD_ASAP | npa600, bma600 | Pure shift 2D 1H-13C HSQC with ASAP |
| UCSD_13C_HSQC_BBHD_PRESAT | npa600, bma600 | Pure shift 2D 1H-13C HSQC with presaturation |
| UCSD_13C_HSQC_JRES | npa600, bma600 |
Perfect 2D 1H-13C HSQC for measurement of
1JCH reference |
| UCSD_13C_HSQC-TOCSY | npa600 | 2D 1H-13C HSQC-TOCSY |
| UCSD_13C_H2BC | npa600, bma600 |
2D 1H-13C H2BC two bond 1H-13C correlation via 1JHC and 3JHH reference |
| UCSD_13C_H2BC_PRESAT | npa600 |
2D 1H-13C H2BC two bond 1H-13C correlation via 1JHC and 3JHH with solvent suppression via presaturation |
| UCSD_13C_11ADEQUATE | npa600, bma600 |
2D 1H-13C 1,1-ADEQUATE, two bond 1H-13C correlation via 1JHC and 1JCC reference |
| UCSD_13C_1nADEQUATE | bma600 |
2D 1H-13C 1,n-ADEQUATE, three to four bond 1H-13C correlation via 1JHC and nJCC reference |
| UCSD_13C_HMBC | npa600, bma600 |
2D 1H-13C IMPACT-HMBC reference |
| UCSD_13C_HMBC_PRESAT | npa600 |
2D 1H-13C HMBC with solvent suppression via presaturation |
| UCSD_13C_HMBC_sel | npa600 |
2D band selective 1H-13C HMBC reduced 13C sweep width for increased resolution good for aromatic or carbonyl resonances reference |
| UCSD_13C_HMBC-J | npa600 | 2D 1H-13C J-HMBC for measurement of nJHC reference |
| UCSD_13C_HETLOC | npa600, bma600 |
2D 1H-1H HETLOC for measurement of nJHC reference |
| UCSD_13C_HSQMBC | npa600 |
2D 1H-13C HSQMBC selective measurement of nJHC |
| UCSD_13C_HSQMBC_IPAP | npa600, bma600 |
IPAP 2D 1H-13C HSQMBC selective measurement of nJHC via IPAP reference |
| UCSD_13C_HSQMBC-TOCSY | npa600 |
2D 1H-13C HSQMBC-TOCSY selective 2-6 bond nJHC correlation followed by TOCSY |
| UCSD_13C_HSQMBC_TOCSY_IPAP | npa600, bma600 |
IPAP 2D 1H-13C HSQMBC-TOCSY selective measurement of nJHC via IPAP reference |
| UCSD_13C_LR-HSQMBC | npa600, bma600 |
2D 1H-13C long range HSQMBC 2-6 bond correlation via nJHC reference |
2D 1H-15N Experiments
| Parameter Set | Spectrometer | Notes |
|---|---|---|
| UCSD_15N_HSQC | npa600, bma600 | 2D 1H-15N HSQC |
| UCSD_15N_HSQC_TOCSY | bma600 |
2D 1H-15N HSQC-TOCSY sensitivity enhanced, good for peptides reference |
| UCSD_15N_HMQC_SF | npa600, bma600 |
2D 1H-15N SOFAST-HMQC rapid H-N correlation for 15N labelled biomolecules reference |
| UCSD_15N_HMBC | npa600, bma600 | 2D 1H-15N HMBC |
| UCSD_15N_TROSY | bma600 |
2D 1H-15N TROSY for large 15N labelled biomolecules reference |
| UCSD_TROSY_13Caro | bma600 |
2D 1H-13C TROSY for aromatic resonances in 13C labelled biomolecules referience |
| UCSD_hbCBcgcdHD | bma600 |
2D 1H-13C hbCBcgcdHD for aromatic resonances in 13C labelled biomolecules reference |
| UCSD_hbCBcgcdceHE | bma600 |
2D 1H-13C hbCBcgcdceHE for aromatic resonances in 13C labelled biomolecules reference |
3D Experiments
| Parameter Set | Spectrometer | Notes |
|---|---|---|
| UCSD_TOCSY_HSQC_HNH | bma600 |
3D 1H-15N-1H TOCSY-HSQC with DIPSI2 spinlock, for 15N labelled biomolecules |
| UCSD_NOESY_HSQC_HNH | npa600, bma600 |
3D 1H-15N-1H NOESY-HSQC for 15N labelled biomolecules |
| UCSD_NOESY_HSQC_NNH | bma600 |
3D 15N-15N-1H HSQC-NOESY-HSQC for 15N labelled biomolecules |
| UCSD_NOESY_HSQC_HCH | bma600 |
3D 1H-13C-1H NOESY-HSQC for 13C labelled biomolecules |
| UCSD_HNHA | npa600, bma600 |
3D 1H-15N-1H HNHA for 15N labelled biomolecules correlates HN and Hα, measures φ |
| UCSD_HNHB | npa600, bma600 |
3D 1H-15N-1H HNHB for 15N labelled biomolecules correlates HN and Hβ, measures ψ |
| UCSD_HNCO | bma600 |
3D 1H-13C-15N HNCO with watergate, for 13C-15N labelled proteins |
| UCSD_HNcaCO | bma600 |
3D 1H-13C-15N HN(CA)CO with watergate, for 13C-15N labelled proteins |
| UCSD_HNCA | bma600 |
3D 1H-13C-15N HNCA with watergate, for 13C-15N labelled proteins |
| UCSD_HNcoCA | bma600 |
3D 1H-13C-15N HN(CO)CA with watergate, for 13C-15N labelled proteins |
| UCSD_HNCACB | bma600 |
3D 1H-13C-15N HNCACB with watergate, for 13C-15N labelled proteins |
| UCSD_CBCAcoNH | bma600 |
3D 1H-13C-15N CBCA(CO)NH with watergate, for 13C-15N labelled proteins |
| UCSD_HBHAcoNH | bma600 |
3D 1H-13C-15N HBHA(CO)NH with watergate, for 13C-15N labelled proteins |
Relaxation Experiments
| Parameter Set | Spectrometer | Notes |
|---|---|---|
| UCSD_1H_T1 | npa600, bma600 | 1D 1H T1 relaxation rate measurement |
| UCSD_13C_T1 | npa600 | 2D 13C T1 relaxation rate measurement |
| UCSD_13C_T2 | npa600 | 2D 13C T2 relaxation rate measurement |
| UCSD_15N_T1 | npa600, bma600 |
2D 15N T1 relaxation rate measurement for 15N labelled proteins interleaved acquisistion as pseudo 3D |
| UCSD_15N_T2 | npa600, bma600 |
2D 15N T2 relaxation rate measurement for 15N labelled proteins interleaved acquisistion as pseudo 3D temperature compensation |
| UCSD_15N_HETNOE | npa600, bma600 |
2D 15N heteronuclear NOE measurement for 15N labelled proteins interleaved acquisisition |
Diffusion Experiments
| Parameter Set | Spectrometer | Notes |
|---|---|---|
| UCSD_DOSY | npa600,bma600 | 2D diffusion measurement |
| UCSD_DOSY_PRESAT | npa600,bma600 |
2D diffusion measurement with solvent suppression via presaturation |
| UCSD_XSTE | bma600 |
1D diffusion measurement of large 15N labelled molecules acquired as pseudo 2D reference |
| UCSD_XSTE-H-TROSY | bma600 |
1D diffusion measurement of large 15N labelled molecules acquired as pseudo 2D reference |
| UCSD_XSTE-N-TROSY | bma600 |
1D diffusion measurement of large 15N labelled molecules acquired as pseudo 2D reference |
Calibration Experiments
| Parameter Set | Spectrometer | Notes |
|---|---|---|
| UCSD_CAL_1H_TRANS | npa600, bma600 | Calibrate 1H 90o transmitter pulse |
| UCSD_CAL_C13_TRANS | npa600, bma600 | Calibrate 13C 90o transmitter pulse |
| UCSD_CAL_C13_DEC | npa600, bma600 | Calibrate 13C 90odecoupler pulse |
| UCSD_CAL_N15_DEC | bma600 | Calibrate 15N 90odecoupler pulse |
Written by Brendan Duggan. Last modified 2022-Jul-22
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