Table 1.
Crystallographic data collection and refinement statistics
r.m.s.d. is the root mean square deviation from ideal geometry.
| WT 10–307 +0P–sunitinib | WT 1–307 +2P–sunitinib | 1–307 T165E,S171E–sunitinib | |
|---|---|---|---|
| Data collection statistics | |||
| Wavelength (Å) | 1.00 | 1.00 | 1.00 |
| Resolution range (Å) | 107.95–2.17 | 74.97–2.97 | 60.18–2.03 |
| Space group | R32 | R32 | P1 |
| Cell edge a, b, c (Å); angle (°) | 165.91, 165.91, 163.58; 90.00, 90.00, 120.00 | 149.93, 149.93, 156.75; 90.00, 90.00, 120.00 | 55.81, 58.92, 60.93; 82.44, 82.31, 64.34 |
| Molecules per asymmetric unit | 2 | 2 | 2 |
| Total reflections (outer shell) | 454,280 (4,444) | 142,751 (1,488) | 155,437 (1,687) |
| Unique reflections (outer shell) | 46,182 (433) | 14,226 (149) | 43,684 (458) |
| Multiplicity (outer shell) | 9.8 (10.3) | 10.0 (10.0) | 3.6 (3.7) |
| Completeness (%) (outer shell) | 100.0 (99.3) | 100.0 (100.00) | 97.3 (95.8) |
| Mean I/σ(I) (outer shell) | 14.81 (2.33) | 12.5 (2.3) | 14.9 (2.10) |
| Wilson B-factor (Å2) | 44.31 | 55.04 | 42.36 |
| Rmerge (outer shell)a | 0.097 (1.210) | 0.196 (1.067) | 0.042 (0.620) |
| Rpimb | 0.033 (0.399) | 0.065 (0.356) | 0.026 (0.374) |
| CC1/2 (outer shell)c | 0.999 (0.701) | 0.996 (0.861) | 0.999 (0.874) |
| Refinement statistics | |||
| Resolution range (Å) | 17.78–2.17 | 74.97–2.97 | 27.69–2.03 |
| Rwork/Rfreed | 0.192/0.219 | 0.207/0.251 | 0.201/0.229 |
| Number of atoms (protein/ligand/water) | 4,463/58/412 | 4,225/58/16 | 4,332/58/320 |
| r.m.s.d. bond length (Å) | 0.014 | 0.056 | 0.013 |
| r.m.s.d. bond angle (°) | 1.71 | 1.00 | 1.57 |
| Ramachandran plot | |||
| Most favored region (%) | 98 | 95 | 96 |
| Allowed regions (%) | 2 | 5 | 4 |
| Disallowed regions (%) | 0 | 0 | 0 |
a Rmerge = ΣhklΣi|Ii − 〈I〉|/−ΣhklΣIi where Ii is the intensity of the ith observation, 〈I〉 is the mean intensity of the reflection, and the summations extend over all unique reflections (hkl) and all equivalents (i), respectively.
b Rpim is a measure of the quality of the data after averaging the multiple measurements, and Rpim = Σhkl[n/(n − 1)]1/2Σi|Ii(hkl) − 〈I(hkl)〉|/ΣhklΣiIi(hkl) where n is the multiplicity and other variables are as defined for Rmerge (39).
c CC1/2 is the Pearson correlation coefficient.
d Rwork = Σ|Fo − Fc|/ΣFo where Fo and Fc are observed and calculated structure factors, respectively, Rfree was calculated from a randomly chosen 5% of reflections excluded from the refinement, and Rwork was calculated from the remaining 95% of reflections.