Table 5. Crystallographic data collection and refinement statistics on Sac-KDGA.
Values in parentheses are for the highest resolution shell. Rsym=|I−〈I〉|/I, where I is the observed intensity and 〈I〉 is the average intensity. Rcryst=hkl, work ||Fobs|−k|Fcalc||/hkl|Fobs|×100%, where Fobs=observed structure factor and Fcalc=calculated structure factor. Rfree=R calculated with 5% of randomly selected data that were omitted from the refinement.
| Native, pH 7.5 | Native, pH 7.5 | Pyruvate, pH 6.3 | |
|---|---|---|---|
| Space group | P3121 | P6522 | P3121 |
| Unit cell dimensions (Å) | a=b=108.2 c=171.9 | a=b=109.5 c=319.6 | a=b=109.1 c=171.3 |
| Resolution (Å) | 30–1.8 (1.88–1.8) | 36–2.5 (2.59–2.5) | 50–2.5 (2.65–2.5) |
| Wavelength (Å) | 0.934 | 0.934 | 0.933 |
| Unique reflections | 107995 | 36273 | 39118 |
| Completeness (%) | 99.9 (99.8) | 90.1 (55.2) | 99.6 (97.1) |
| Redundancy | 10.9 (4.0) | 33.1(19.8) | 6.2 (4.2) |
| I/σ(I) | 14.1 (2.3) | 23.8 (8.4) | 17.6 (5.3) |
| Rsym (%) | 9.6 (55.9)* | 15.5 (37.8) | 5.3 (34.8) |
| Refinement | |||
| Rcryst (%) | 15.7 | 17.6 | 15.9 |
| Rfree (%) | 17.9 | 21.7 | 19.1 |
| Number of atoms | |||
| Protein | 4634 | 4598 | 4616 |
| Pyruvate | − | − | 10 |
| Solvent | 412 | 95 | 162 |
| Average B factor (Å2) protein | 35.5 | 52.0 | 52.9 |
| Pyruvate | − | − | 42.6 |
| Solvent | 44.2 | 43.6 | 50.8 |
| Rmsd bonds/angles (Å/°) | 0.012/1.5 | 0.008/1.3 | 0.008/1.3 |
*The value for the highest resolution shell is affected by anisotropy in diffraction.