Table 2. Data-collection and refinement statistics for wild-type ADH complexed with NAD+ and 2,2,2-trifluoroethanol.
Data were refined in the resolution range 20–1.1 Å. Values in parentheses are for the outer shell (1.14–1.10 Å).
| Temperature (K) | 25 | 45 | 65 | 85 | 100 | 125 | 150 |
|---|---|---|---|---|---|---|---|
| PDB code | 7ua6 | 7uc9 | 7uca | 7ucu | 4dxh | 7ude | 7udd |
| No. of reflections | |||||||
| Total | 1142316 | 1065509 | 994485 | 1138600 | 1131238 | 1136081 | 1136366 |
| Unique | 278830 | 277899 | 277772 | 279168 | 277733 | 278692 | 278542 |
| Completeness (%) | 94.2 (90.8) | 93.8 (89.9) | 93.8 (89.8) | 94.2 (90.7) | 93.6 (88.9) | 93.7 (88.9) | 93.5 (88.5) |
| Multiplicity | 4.06 (4.09) | 3.78 (3.78) | 3.54 (3.56) | 4.04 (4.03) | 4.01 (4.01) | 4.00 (4.01) | 4.01 (4.01) |
| R p.i.m. (%) | 3.5 (23.0) | 3.0 (24.5) | 3.2 (25.4) | 3.4 (24.2) | 2.8 (23.8) | 2.9 (30.7) | 3.2 (32.1) |
| 〈I/σ(I)〉 | 9.1 (2.8) | 9.8 (2.2) | 9.5 (2.3) | 9.0 (2.5) | 10.0 (2.0) | 8.9 (1.3) | 8.2 (1.1) |
| R work, R free (%) | 12.2, 14.0 | 12.6, 15.2 | 12.6, 14.6 | 12.4, 14.2 | 12.8, 15.0 | 13.4, 16.0 | 13.5, 16.0 |
| R free reflections | 2775 | 2760 | 2757 | 2768 | 2751 | 2759 | 2762 |
| R.m.s.d., bond lengths (Å) | 0.013 | 0.013 | 0.013 | 0.013 | 0.013 | 0.014 | 0.015 |
| R.m.s.d., angles (°) | 1.88 | 1.93 | 1.91 | 1.88 | 1.92 | 1.95 | 1.98 |
| E.s.u.† (Å) | 0.017 | 0.019 | 0.019 | 0.018 | 0.018 | 0.021 | 0.022 |
| MolProbity scores‡ | 0.89, 98th; 0.96, 98th | 1.21, 98th; 1.03, 98th | 0.97, 98th; 1.01, 98th | 0.81, 98th; 0.91, 99th | 0.56, 98th; 0.89, 99th | 0.81, 98th; 0.91, 99th | 0.97, 98th; 1.01, 98th |
| Ramachandran§ (%) | 97.04 | 97.04 | 97.85 | 97.31 | 96.91 | 97.18 | 97.04 |
| Wilson B (Å2) | 9.0 ± 0.2 | 9.5 ± 0.3 | 9.4 ± 0.2 | 9.3 ± 0.2 | 9.3 ± 0.3 | 10.0 ± 0.3 | 10.4 ± 0.4 |
| REFMAC B ¶ (Å2) | 13.8 | 14.6 | 14.3 | 14.1 | 14.3 | 15.4 | 16.4 |
| B, protein atoms (Å2) | 13.6 | 14.4 | 14.2 | 13.9 | 14.1 | 15.2 | 16.2 |
| B, waters (Å2) | 24.9 | 26.1 | 25.5 | 25.0 | 25.4 | 27.3 | 28.3 |
| B, heteroatoms (Å2) | 16.7 | 17.6 | 17.2 | 17.0 | 17.2 | 18.3 | 19.5 |
| Protein anisotropy | 0.54 | 0.54 | 0.55 | 0.55 | 0.55 | 0.55 | 0.55 |
| B, C4N (A, B)†† (Å2) | 8.0, 9.6 | 8.7, 10.4 | 8.4, 10.7 | 8.5, 10.3 | 8.5, 10.5 | 9.3, 11.8 | 10.1, 12.3 |
| B, C2 (A, B)†† (Å2) | 9.6, 11.6 | 10.0, 12.7 | 9.8, 13.1 | 9.6, 12.4 | 10.2, 13.0 | 11.9, 14.5 | 12.5, 15.2 |
†
Estimated standard uncertainty for coordinates based on maximum likelihood.
‡
MolProbity clashscore, percentile; score, percentile.
§
Ramachandran angles in favored region; there were no outliers.
¶
Anisotropic B factors for 6983 total non-H atoms and analysis with the PARVATI server for 5935 protein atoms, 904 water molecules and 144 heteroatoms: four zinc ions, two TFE molecules, two NAD+ ions and four MRD molecules.
††
Anisotropic B factors for atoms of NAD+ and TFE in subunits A and B.