TABLE 1.
Summary of crystallographic data
r.m.s.d., root mean square deviation.
| Intermediate complex |
||
|---|---|---|
| 2.8 Å | 6.0 Å | |
| Data set | ||
| Wavelength (Å) | 1.0000 | 0.9795 |
| Resolution range (Å) | 29.8–2.8 (2.9–2.8)a | 30.0–6.0 (6.6–6.0) |
| Space group | P 21212 | P 21 |
| Cell parameters | ||
| a, b, c (Å) | 112.0, 238.0, 52.2 | 152.4, 127.3, 210.3 |
| α, β, γ (°) | 90, 90, 90 | 90, 110.2, 90 |
| Unique reflections | 34,114 (4,406) | 18,388 (4,452) |
| Completeness (%) | 97.0 (95.7) | 96.3 (98.7) |
| Redundancy | 3.3 (3.1) | 3.2 (3.4) |
| Rsymb | 0.06 (0.58) | 0.06 (0.78) |
| Mean I/σ(I) | 8.3 (1.6) | 8.9 (1.4) |
| Refinement | ||
| Reflections: work/free | 32,332/1,710 | 17,462/917 |
| Rwork/Rfree | 0.224/0.261 | 0.274/0.303 |
| No. protein atoms | 7,750 | 41,984 |
| No. ligand atoms | 1 | 4 |
| Protein B-factors (Å2) | 111.0 | 361.8 |
| Water/ligand B-factors (Å2) | 111.1 | 357.5 |
| r.m.s.d. of bond lengths (Å) | 0.0148 | 0.0031 |
| r.m.s.d. of bond angles (°) | 1.70 | 0.74 |
| Ramachandran preferred (%) | 96.0 | 91.0 |
| Ramachandran allowed (%) | 3.3 | 6.7 |
| Ramachandran outliers (%) | 0.7 | 2.3 |
a Values in parentheses are for the highest resolution shell.
b Rsym = ΣhklΣi|Ii(hkl) − <I(hkl)>|/ΣhklΣiIi(hkl) where Ii(hkl) is ith observation of reflection hkl and I(hkl) is the weighted average intensity for all observations i of reflection hkl.