BMRB Entry 53341

Chem Shift validation: AVS_full
BMRB Entry DOI: doi:10.13018/BMR53341

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Title:
2-dimensional and 3-dimensional [1H,13C] spectra for Ile delta1-13CH3 labeled caspase-6
Deposition date:
2025-09-04
Original release date:
2026-08-03
Authors:
Kuzio, Nathanael; Tonelli, Marco; Fejzo, Jasna; Hardy, Jeanne
Citation:

Citation: Kuzio, Nathanael; Tonelli, Marco; Fejzo, Jasna; Hardy, Jeanne. "An NMR sample preparation case study: Considerations for the self-destructive protease caspase-6 "  PLoS One 20, e0337291-e0337291 (2025).
PubMed: 41270077

Assembly members:

Assembly members:
entity_1, polymer, 263 residues, Formula weight is not available

Natural source:

Natural source:   Common Name: E. coli   Taxonomy ID: 562   Superkingdom: Bacteria   Kingdom: not available   Genus/species: Escherichia coli

Experimental source:

Experimental source:   Production method: recombinant technology   Host organism: Escherichia coli   Vector: pET11a

Entity Sequences (FASTA):

Entity Sequences (FASTA):
entity_1: AFYKREMFDPAEKYKMDHRR RGIALIFNHERFFWHLTLPE RRGTCADRDNLTRRFSDLGF EVKCFNDLKAEELLLKIHEV STVSHADADCFVCVFLSHGE GNHIYAYDAKIEIQTLTGLF KGDKCHSLVGKPKIFIIQAC RGNQHDVPVIPLDVVD-AAS VYTLPAGADFLMCYSVAEGY YSHRETVNGSWYIQDLCEML GKYGSSLEFTELLTLVNRKV SQRRVDFCKDPSAIGKKQVP CFASMLTKKLHFFPKSNHHH HHH

Data typeCount

Additional metadata:

  • Assembly
  • Samples and Experiments
  • Software
  • Spectrometers
  • Hide all

Assembly:

Entity Assembly IDEntity NameEntity ID
1Unliganded caspase-6, chain 11
2Unliganded caspase-6, chain 21

Entities:

Entity 1, Unliganded caspase-6, chain 1 263 residues - Formula weight is not available

1   ALAPHETYRLYSARGGLUMETPHEASPPRO
2   ALAGLULYSTYRLYSMETASPHISARGARG
3   ARGGLYILEALALEUILEPHEASNHISGLU
4   ARGPHEPHETRPHISLEUTHRLEUPROGLU
5   ARGARGGLYTHRCYSALAASPARGASPASN
6   LEUTHRARGARGPHESERASPLEUGLYPHE
7   GLUVALLYSCYSPHEASNASPLEULYSALA
8   GLUGLULEULEULEULYSILEHISGLUVAL
9   SERTHRVALSERHISALAASPALAASPCYS
10   PHEVALCYSVALPHELEUSERHISGLYGLU
11   GLYASNHISILETYRALATYRASPALALYS
12   ILEGLUILEGLNTHRLEUTHRGLYLEUPHE
13   LYSGLYASPLYSCYSHISSERLEUVALGLY
14   LYSPROLYSILEPHEILEILEGLNALACYS
15   ARGGLYASNGLNHISASPVALPROVALILE
16   PROLEUASPVALVALASPXALAALASER
17   VALTYRTHRLEUPROALAGLYALAASPPHE
18   LEUMETCYSTYRSERVALALAGLUGLYTYR
19   TYRSERHISARGGLUTHRVALASNGLYSER
20   TRPTYRILEGLNASPLEUCYSGLUMETLEU
21   GLYLYSTYRGLYSERSERLEUGLUPHETHR
22   GLULEULEUTHRLEUVALASNARGLYSVAL
23   SERGLNARGARGVALASPPHECYSLYSASP
24   PROSERALAILEGLYLYSLYSGLNVALPRO
25   CYSPHEALASERMETLEUTHRLYSLYSLEU
26   HISPHEPHEPROLYSSERASNHISHISHIS
27   HISHISHIS

Samples:

sample_1: mature caspase-6 homodimer, [U-13C]-Ile, 140 uM; TRIS, [U-99% 2H], 20 mM; NaCl 200 mM; glycerol, [U-99% 2H], 5%; DTT, [U-99% 2H], 10 mM

sample_2: mature caspase-6 S257D homodimer, [U-13C]-Ile, 140 uM; TRIS, [U-99% 2H], 20 mM; NaCl 200 mM; glycerol, [U-99% 2H], 5%; DTT, [U-99% 2H], 10 mM

sample_3: mature caspase-6 homodimer, [U-13C]-Ile, 140 uM; TRIS, [U-99% 2H], 20 mM; NaCl 200 mM; glycerol, [U-99% 2H], 5%; DTT, [U-99% 2H], 10 mM; VEID-CHO 200 uM

sample_4: mature caspase-6 homodimer, [U-13C]-Ile, 90 uM; TRIS, [U-99% 2H], 20 mM; NaCl 200 mM; glycerol, [U-99% 2H], 5%

sample_5: mature caspase-6 homodimer, [U-13C]-Ile, 90 uM; TRIS, [U-99% 2H], 20 mM; NaCl 200 mM; glycerol, [U-99% 2H], 5%; ZnCl2 500 uM; DTT, [U-99% 2H], 10 mM

sample_6: mature caspase-6 homodimer, [U-13C]-Ile, 50 uM; sodium acetate 50 mM; NaCl 180 mM; glycerol, [U-99% 2H], 5%; DTT, [U-99% 2H], 10 mM; VEID-CHO 100 uM

sample_7: mature caspase-6 homodimer, [U-13C]-Ile, 50 uM; sodium acetate 50 mM; NaCl 180 mM; glycerol, [U-99% 2H], 5%; DTT, [U-99% 2H], 10 mM

sample_conditions_1: pH: 8.5; pressure: 1 atm; temperature: 308 K

sample_conditions_2: pH: 8.5; pressure: 1 atm; temperature: 298 K

sample_conditions_3: pH: 8.5; pressure: 1 atm; temperature: 288 K

sample_conditions_4: pH: 8.5; pressure: 1 atm; temperature: 293 K

sample_conditions_5: pH: 6; pressure: 1 atm; temperature: 298 K

Experiments:

NameSampleSample stateSample conditions
2D 1H-13C HMQCsample_1isotropicsample_conditions_1
2D 1H-13C HMQCsample_1isotropicsample_conditions_2
2D 1H-13C HMQCsample_1isotropicsample_conditions_3
2D 1H-13C HMQCsample_1isotropicsample_conditions_1
2D 1H-13C HMQCsample_1isotropicsample_conditions_2
2D 1H-13C HMQCsample_1isotropicsample_conditions_3
2D 1H-13C HMQCsample_1isotropicsample_conditions_1
2D 1H-13C HMQCsample_1isotropicsample_conditions_2
2D 1H-13C HMQCsample_1isotropicsample_conditions_3
2D 1H-13C HMQCsample_3isotropicsample_conditions_1
2D 1H-13C HMQCsample_4isotropicsample_conditions_2
2D 1H-13C HMQCsample_5isotropicsample_conditions_2
2D 1H-13C HMQCsample_7isotropicsample_conditions_2
2D 1H-13C HMQCsample_6isotropicsample_conditions_2
2D 1H-13C HMQCsample_2isotropicsample_conditions_2
3D 13C-separated NOESYsample_1isotropicsample_conditions_4
3D 13C-separated NOESYsample_3isotropicsample_conditions_4
3D 13C-separated NOESYsample_3isotropicsample_conditions_1
pseudo 3D 1H single-quantum CPMG relaxation dispersionsample_1isotropicsample_conditions_1
pseudo 3D 1H single-quantum CPMG relaxation dispersionsample_1isotropicsample_conditions_1
3D [13C,1H,13C] ZZ-exchangesample_1isotropicsample_conditions_2
3D [13C,1H,13C] ZZ-exchangesample_2isotropicsample_conditions_2

Software:

TOPSPIN - collection, processing

NMRPipe - processing

NMRFAM-SPARKY - peak picking

NMR spectrometers:

  • Bruker AVANCE III 900 MHz
  • Bruker AVANCE III 600 MHz
  • Bruker AVANCE NEO 900 MHz
  • Bruker AVANCE NEO 1100 MHz