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_COSY, UCSD_13C_HSQC and UCSD_13C_HMBC to start with. Other spectra that may be useful can be run using UCSD_TOCSY, UCSD_NOESY UCSD_ROESY and UCSD_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_TOCSY_1D_sel npa600, bma600 1D 1H TOCSY
with selective excitation
UCSD_NOESY_1D_sel 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_DEPT135 npa600 1D 15N, direct detect 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 Homonuclear Experiments

Parameter Set Spectrometer Notes
UCSD_COSY npa600, bma600 2D 1H-1H COSY
UCSD_DQF-COSY npa600, bma600 2D 1H-1H DQF-COSY
not as sensitive as UCSD_COSY but better 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_TOCSY_BSHD_PRESAT npa600, bma600 Pure shift 2D 1H-1H TOCSY
with DIPSI2 spinlock and presaturation
UCSD_NOESY npa600, bma600 2D 1H-1H NOESY
UCSD_NOESY_PRESAT npa600, bma600 2D 1H-1H NOESY
with presaturation
UCSD_NOESY_ES npa600, bma600 2D 1H-1H NOESY
with 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_INADEQUATE bma600 2D 13C-13C INADEQUATE
13C-13C double quantum correlation,
very insensitive

2D Heteronuclear 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, adaibatic pulses, matched sweep pulse
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_PRESAT npa600, bma600 Pure shift 2D 1H-13C HSQC with presaturation
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_LR-HSQMBC npa600, bma600 2D 1H-13C long range HSQMBC
2-6 bond correlation via nJHC
reference
UCSD_13C_HSQMBC-TOCSY npa600 2D 1H-13C HSQMBC-TOCSY
2-6 bond nJHC correlation followed by TOCSY
UCSD_13C_HSQMBC_IPAP npa600, bma600 IPAP 2D 1H-13C HSQMBC
measurement of nJHC via IPAP
reference
UCSD_13C_HSQMBC_TOCSY_IPAP npa600, bma600 IPAP 2D 1H-13C HSQMBC-TOCSY
measurement of nJHC via IPAP
reference
UCSD_HMBC-J npa600 2D 1H-13C J-HMBC
for measurement of nJHC
reference
UCSD_HETLOC npa600, bma600 2D 1H-1H HETLOC
for measurement of nJHC
reference
UCSD_HECADE npa600 2D 1H-13C HECADE
for measurement of JHC
reference
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 2017-May-15

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