assignment of tp5 - uzh · assignment of tp5 sequence: arg-lys-asp-val-tyr 1) identify spin systems...
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Assignment of TP5
Sequence: Arg-Lys-Asp-Val-Tyr
1) Identify spin systems in the TOCSY spectrum which region is most suitable for that purpose ? can you recognize unique spin systems ? how many spin systems do you expect to see?
2) Link the spin systems via sequential NOEs in the ROESY spectrum which region is most suitable for that purpose ?
3) Assign the side-chains based upon COSY correlations be careful, you do not know whether methylene protons will give one or two peaks TIP: You may start from both ends of the side-chain be careful to not mix different spin-system, if two protons from different spin systems have the same chemical shift (check against TOCSY)
4) Assign the aromatic ring spin system find it in the COSY or TOCSY spectrum how can you distinguish between delta and epsilon protons?
Some peak assignments are annotated in the spectra. In the end, you need a complete, fully consistentassignment!
DQF-COSY of TP5 Arg-Lys-Asp-Val-Tyr
2.004.006.008.00
1.0
2.0
3.0
4.0
5.0
6.0
7.0
8.0
1.00
2.00
3.00
4.00
COSY of TP5
QG1/QD1
QG1/HB3 1
TOCSY of TP5COSY of TP5
7.007.508.008.50 7.007.508.008.50
1.00
1.50
2.00
2.50
3.00
3.50
4.00
4.50
QD1/HE1
QE2/HN2
2.004.006.008.00
1.0
2.0
3.0
4.0
5.0
6.0
7.0
8.0
ROESY of TP5 Arg-Lys-Asp-Val-Tyr
ROESY of TP5
7.007.508.008.50 7.007.508.008.50
3.80
3.90
4.00
4.10
4.20
4.30
4.40
4.50
4.60
4.70
COSY of TP5
HA2/HN3
HA3/HN4