Table 3.
Crystallographic statistics of data collection and structure refinement
| PDB code | 2H9H | 2HAL | 2H6M |
|---|---|---|---|
| 3C variant | C24S | C24S | C24S |
| 3C–inhibitor complex | 3C–BBL–Ia | 3C–BBL–II | 3C–BBL–Ib |
| Space group | P212121 | P212121 | P212121 |
| a (Å) | 44.67 | 44.58 | 44.77 |
| b (Å) | 56.06 | 56.24 | 56.09 |
| c (Å) | 80.97 | 81.05 | 80.91 |
| α (°), β (°), γ (°) | 90, 90, 90 | 90, 90, 90 | 90, 90, 90 |
| No. molecule/asymmetric unit | 1 | 1 | 1 |
| Vm (Matthews' coefficient)/% solvent content | 2.1/41.7 | 2.1/41.7 | 2.1/41.7 |
| Data collection | ALS Beamline 8.3.1 | ||
| Resolution range (Å) | 26.5–1.35 (1.40–1.35)a | 40.0–1.35 (1.40–1.35) | 46.08–1.40 (1.45–1.40) |
| Wavelength (Å) | 1.115879 | 1.115879 | 1.115869 |
| Observations | 98,591 | 10,6957 | 112,266 |
| Unique reflections | 36,919 (1013) | 38,893 (1897) | 32,357 (3192) |
| I/σ(I) | 12.7 (2.6) | 13.0 (1.50) | 13.0 (1.72) |
| Data completeness (%) | 81.2 (22.6) | 85.3 (42.4) | 79.1 (79.8) |
| Rmergeb | 0.056 (0.307) | 0.061 (0.288) | 0.068 (0.353) |
| Refinement | |||
| No. reflections used | 34,342 (1263) | 36,916 (1244) | 30,672 (2235) |
| Resolution range (Å) | 26.49–1.39 (1.43–1.39) | 20.0–1.35 (1.39–1.35) | 46.08–1.40 (1.44–1.40) |
| Free set size (%) | 5.0 | 5.0 | 5.0 |
| No. atoms | 1946 | 2073 | 1946 |
| No. waters | 263 | 391 | 263 |
| Rworkingc (%) | 18.1 (32.9) | 18.4 (23.1) | 17.7 (30.0) |
| Rfree (%) | 19.7 (29.4) | 20.4 (28.3) | 20.4 (33.0) |
| Mean B valued | 20.97/32.28/37.22 | 17.01/28.07/29.96 | 20.36/33.57/35.82 |
| r.m.s.d. from ideal geometry | |||
| Bond length (Å) | 0.009 | 0.009 | 0.008 |
| Bond angle (°) | 1.200 | 1.144 | 1.152 |
| Chirality | 0.081 | 0.076 | 0.076 |
| Ramachandran plot outliers (phi, psi) | Asp36 (51.2, –129.2) Asp84 (69.4, –69.5) | Asp36 (49.7, –127.5) Asp84 (68.1, –73.0) | Asp36 (50.0, –125.7) Asp84 (69.4, –71.0) |
a
Parentheses indicate values for the highest resolution shell.
b
Rmerge=ΣhΣj|Ihj−<Ih>|/ΣhΣjIhj, where <Ih> is the weighted mean intensity of the symmetry-related reflections Ihj.
c
Rworking=Σh||Fo|-|Fc||/ΣhFo, where |Fo| and |Fc| represent the observed and calculated structure factor amplitudes, respectively. Rfree is Rworking calculated with the reference set.
d
Average B factors of the complex/tetrapeptidyl inhibitor/solvent molecules.