Table 1.
TSP4-N data collection and refinement statistics.
| Protein Precipitant |
TSP4-N335 SeMet LiSO4 | TSP4-N335 tartrate | TSP4-N250 PEG8000 |
|---|---|---|---|
| Data collection | |||
| No. merged data sets | 5 | 1 | 1 |
| Space group (number) | P41212 (92) | R3 (146) | R32 (155) |
| Cell dimension (Å) | a = b = 67.9, c = 607.2 | a = b = 78.0, c = 326.9 | A = b = 84.7, c = 225.1 |
| Wavelength (Å) | 0.9793 | 1.0332 | 1.0332 |
| Resolution (Å) | 3.0 | 2.5 | 2.8 |
| No. molecules in the ASU | 3 (trimer) | 2 | 1 |
| No. observed reflections | 1,844,233 | 66,423 | 36,002 |
| No. unique reflections | 28,173 | 25,427 | 7,883 |
| Completeness (%)a | 94.4 (67.6) | 98.9 (98.8) | 99.0(97.2) |
| Multiplicity | 66.9 | 2.6 | 4.6 |
| Rmergeb | 0.228 (2.43) | 0.090 (0.86) | 0.070(3.36) |
| <I/σI> | 20.4 (0.8) | 5.1 (0.9) | 7.6(0.2) |
| Wilson B/anisotropic ΔB (Å2) | 119.4/33.9 | 52.0/5.3 | 138.0/77.8 |
| SAD phasing and automatic chain building | |||
| Δanomalous cc1/2 | 0.907 | ||
| No. found/true Se sites | 17/15 | ||
| No. residues/fragments built | 546/44 | ||
| Model-map correlation | 0.64 | ||
| Rc/Rfreed | 0.39/0.43 | ||
| Refinement | |||
| Resolution range (Å) | 30.0–3.0 | 20.0–2.6 | 30–3.2 |
| Total no. of reflections | 26,761 | 21,436 | 5125 |
| Completeness (%) | 94.4 | 98.7 | 98.9 |
| Rc/Rfreed | 0.225/0.296 | 0.206/0.229 | 0.201/0.301 |
| No. protein residues | 983 | 576 | 241 |
| No. waters/imidazoles | – | 32/2 | – |
| RMSD from ideal geometry | |||
| Bond length (Å)/angles (°) | 0.019/1.8 | 0.012/1.5 | 0.005/1.8 |
| Average B (Å2) | 141.9 e | 80.3 e | 151.6 |
| Ramachandran plot (%) | |||
| Allowed/outliers | 97.2/2.8 | 99.8/0.2 | 99.0/1.0 |
aThe values in parentheses are for the highest resolution shells.
bRmerge = Σhkl [(Σj|Ij − < I >|)/Σj|Ij|].
cR = Σhkl||Fo| − |Fc||/Σhkl|Fo|, where Fo and Fc are the observed and calculated structure factors, respectively.
dRfree is computed from randomly selected 5% of reflections omitted from the refinement.
eB factors calculated after TLS refinements (5 and 7 groups for the WT/tartrate and SeMet/LiSO4 crystals, respectively).