Table 1.
Statistics on X-ray Data Collection and Model Refinement
| native | tungstate | phosphate | H366A | |
|---|---|---|---|---|
| X-ray Data Collection | ||||
| unit cell dimensions (Å) | 77.9 × 116.1 × 121.4 | |||
| space group | P212121 | |||
| resolution (Å) | 50.0-1.95 | 50.0-2.25 | 50.0-2.8 | 50.0-2.05 |
| no. of unique reflections | 80016 | 101825h | 28141 | 68913 |
| completeness, overall (last shell)a (%) | 99.9 (100.0) | 99.4 (97.1)h | 98.6 (100.0) | 99.8 (100.0) |
| redundancy, overall (last shell)a | 7.6 (7.6) | 5.5 (4.7)h | 5.7 (6.0) | 7.8 (7.0) |
| 〈I〉/〈σ(I)〉, overall (last shell)a | 35.0 (4.5) | 18.5 (2.6)h | 21.1 (2.7) | 26.5 (3.0) |
| Rsymb (%) | 8.4 (50.0) | 9.8 (56.5)h | 10.1 (61.7) | 9.0 (65.4) |
| Model Refinement | ||||
| resolution (Å) | 50.0-1.95 | 50.0-2.25 | 50.0-2.8 | 50.0-2.05 |
| no. of reflections used | 79938 | 50569 | 26559 | 65215 |
| Rfreec (%), overall (last resolution shell) | 24.1 (26.3) | 24.2 (27.6) | 27.1 (34.4) | 26.8 (29.5) |
| Rworkd (%), overall (last resolution shell) | 20.3 (22.1) | 19.4 (22.6) | 23.5 (27.7) | 22.5 (22.7) |
| Rcryste (%) | 20.5 | 19.6 | 23.7 | 22.7 |
| rmsd for bond lengths (Å) | 0.013 | 0.012 | 0.014 | 0.011 |
| rmsd for bond angles (deg) | 1.427 | 1.345 | 1.523 | 1.290 |
| estimated standard uncertaintyf (Å) | 0.161 | 0.228 | 0.434 | 0.203 |
| average temperature factor (Å2) | ||||
| protein atoms | 28.1 | 40.3 | 61.5 | 33.7 |
| water molecules | 30.2 | 36.8 | 46.1 | 33.6 |
| ligand | - | 29.5 | 90.4 | - |
| ions | - | 44.3 | - | 28.3 |
| Ramachandran plotg (%) | 91.8/8.1 | 91.1/8.9 | 87.1/12.9 | 90.8/9.2 |
The last resolution shells are 2.02-1.95, 2.33-2.25, 2.90-2.80, and 2.12-2.05 Å for the native, tungstate-bound (SAD), phosphate-bound, and H366A data, respectively.
Rsym = Σi,hkl|〈I(hkl)〉 − Ii(hkl)|/Σi,hklIi(hkl).
Rfree = Σ(hkl)εT||Fobs| − |Fcalc||/Σ(hkl)εT|Fobs|, where T is the test set (37) obtained by randomly selecting 5% of the data. The last resolution shells are 2.0-1.95, 2.3-2.25, 2.85-2.77, and 2.12-2.05 Å for the native, tungstate-bound, phosphate-bound, and H366A structures, respectively.
Rwork = Σ(hkl)εW||Fobs| − |Fcalc||/Σ(hkl)εW|Fobs|, where W is the working set.
Rcryst = Σ(hkl)|||Fobs| − |Fcalc|||/Σ(hkl)|Fobs| calculated over the entire set of unique reflections.
Calculated from Rfree statistics.
Most favored regions/additional allowed regions.
These statistics were obtained after treating I+ and I− as independent reflections.