Table 2.
Data collection and refinement statistics.
| NADP+ complex | NADP+–inhibitor complex | NADP+–LY354899 complex | |
|---|---|---|---|
| Spacegroup | P21 | P21 | P21 |
| Unit cellparameters, a, b, c, (Å) and β | 55.0, 80.1, 68.6, 107° | 55.5, 80.9, 68.5, 107° | 55.2, 80.5, 68.5, 107° |
| Resolution range (Å)a | 52.6–1.45 (1.53–1.45) | 20.86–2.00 (2.11–2.00) | 20.67–2.00 (2.11–2.00) |
| Number of measurements | 357 135 (47 440) | 91 096 (12 233) | 87 114 (11 109) |
| Number of unique reflections | 100 394 (14559) | 38 850 (5634) | 36 783 (4948) |
| Multiplicity | 3.6 (3.3) | 2.3 (2.2) | 2.4 (2.2) |
| Completeness (%) | 99.7 (99.3) | 99.0 (99.1) | 95.2 (88.4) |
| Mean I/σI | 13.1 (2.9) | 18.7 (8.1) | 12.9 (6.3) |
| Wilson B (Å2) | 14.9 | 18.9 | 15.9 |
| R merge b | 0.055 (0.423) | 0.030 (0.095) | 0.044(0.118) |
| Rworkc/Rfreed | 0.122/0.152 | 0.171/0.214 | 0.168/0.208 |
| rmsd bonds (Å) | 0.0085 | 0.0051 | 0.005 |
| rmsd angles (°) | 1.478 | 1.146 | 1.132 |
| Ramachandran plot (%) | |||
| Favoured/allowed | 99.0/1.0 | 98.1/1.9 | 98.2/1.8 |
| Protein residues/atoms | 568/4329 | 564/4175 | 564/4207 |
| Overall B (Å2) chain A/B | 16.9/16.4 | 22.1/19.1 | 16.7/15.2 |
| Waters | 740 | 592 | 654 |
| Overall B (Å2) | 30.5 | 24.8 | 21.2 |
| NADP+ | 2 | 2 | 2 |
| Overall B (Å2) | 27.2/26.1 | 27.7/25.2 | 24.2/23.3 |
| Inhibitors | – | 2 | 2 |
| Overall B (Å2) | – | 18.0/15.8 | 12.9/12.1 |
| Poly(ethylene glycol)/glycerol/Cl− | 1/5/5 | –/2/1 | –/2/1 |
| Overall B (Å2) | 39.2/32.2/20.7 | 30.8/17.4 | 30.9/14.6 |
a
Values in parentheses refer to the highest resolution bin.
b
Rmerge = ΣhΣi||(h,i) − <I(h)> Σh ΣI |(h,i).
c
Rwork = Σhkl||Fo| − |Fc||/Σ|Fo|, where Fo is the observed structure factor and Fc is the calculated structure factor.
d
Rfree is the same as Rwork, except it is calculated using 5% of the data that are not included in any refinement.