Table 1. X-ray crystallographic data-collection and refinement statistics.
Values in parentheses are for the highest resolution shell. Data were collected from one crystal for each structure.
| LT PKA–MgATP–IP20 | LT PKA–Mg2ATP–IP20 | RT PKA–Mg2ADP·PO4–IP20 | LT PKA–Mg2AMPPNP–IP20 | RT PKA–Mg2AMPPNP–IP20 | |
|---|---|---|---|---|---|
| Data collection | |||||
| Temperature (K) | 100 | 100 | 293 | 100 | 293 |
| Space group | P212121 | P212121 | P212121 | P212121 | P212121 |
| Unit-cell parameters | |||||
| a (Å) | 58.43 | 58.90 | 58.90 | 57.54 | 59.21 |
| b (Å) | 79.92 | 79.80 | 79.63 | 79.65 | 80.03 |
| c (Å) | 98.61 | 98.51 | 99.49 | 98.01 | 99.20 |
| Resolution (Å) | 20.00–2.00 (2.07–2.00) | 28.95–2.20 (2.28–2.20) | 19.86–2.20 (2.28–2.20) | 20.00–1.80 (1.86–1.80) | 20.00–2.30 (2.38–2.30) |
| R merge | 0.089 (0.438) | 0.118 (0.412) | 0.132 (0.449) | 0.044 (0.256) | 0.107 (0.488) |
| 〈I/σ(I)〉 | 9.8 (2.5) | 5.5 (1.9) | 4.8 (1.9) | 38.5 (8.2) | 15.7 (3.3) |
| Completeness (%) | 91.8 (87.1) | 93.3 (91.1) | 95.1 (94.7) | 99.6 (99.0) | 96.3 (94.3) |
| Multiplicity | 4.8 (4.0) | 3.4 (3.3) | 2.9 (2.8) | 6.9 (6.7) | 5.5 (5.6) |
| Refinement | |||||
| Resolution (Å) | 20–2.00 | 20–2.20 | 20–2.20 | 20–1.80 | 20–2.30 |
| No. of reflections | 29134 (2719) | 22475 (2161) | 23181 (2264) | 42275 (4112) | 20784 (2004) |
| R work/R free | 0.199/0.234 | 0.203/0.233 | 0.187/0.222 | 0.179/0.194 | 0.155/0.189 |
| No. of water molecules | 432 | 321 | 211 | 454 | 224 |
| B factors (Å2) | |||||
| Protein | 27.6 | 32.3 | 37.0 | 22.1 | 30.9 |
| Ligand + Mg | 39.5 | 33.0 | 40.8 | 17.4 | 20.0 |
| IP20 | 29.1 | 33.3 | 37.7 | 22.2 | 30.3 |
| Water | 39.8 | 40.6 | 49.8 | 34.8 | 43.9 |
| R.m.s. deviations | |||||
| Bond lengths (Å) | 0.005 | 0.006 | 0.006 | 0.004 | 0.005 |
| Bond angles (Å) | 1.226 | 1.267 | 1.210 | 1.186 | 1.189 |