TABLE 1.
X-ray data collection and crystallization refinement statistics
| PenI at pH 9.5 | PenI at pH 7.5 | PenA at pH 4.2 | |
|---|---|---|---|
| Data collection | |||
| Space group | P21 | P21 | C2 |
| Cell constant | 41.4, 52.8, 50.5 | 41.4, 52.7, 50.5 | 121.0, 69.9, 84.4 |
| a, b, c | 90.0, 92.6, 90.0 Å | 90.0, 92.5, 90.0 Å | 90.0, 90.0, 90.0 Å |
| Wavelength | 1.000 Å | 1.000 Å | 1.000 Å |
| Resolution | 50 to 1.18 Å (1.22 to 1.18 Å | 50 to 1.05 Å (1.07 to 1.05 Å) | 50 to 1.20 Å (1.22 to 1.20 Å) |
| Observations | 274,380 (21,669) | 375,483 (8696) | 845,028 (36,428) |
| Unique reflections | 68,595 (6191) | 98,393 (3781) | 208,965 (10,119) |
| Rmerge | 0.088 (0.286) | 0.092 (0.350) | 0.039 (0.450) |
| Completeness | 96.4% (87.5%) | 97.8% (75.7%) | 95.5% (93.1%) |
| Average I/σ(I) | 14.8 (4.3) | 13.6 (2.6) | 31.6 (2.7) |
| Data refinement | |||
| Resolution range | 15 to 1.18 | 15 to 1.05 | 15 to 1.2 |
| No. of reflections used (F > 0σ(F)) | 66,491 | 95,315 | 202,528 |
| Rwork/Rfreea | 0.1138/0.1528 | 0.1345/0.1602 | 0.1322/0.1749 |
| Rtotal | 0.1150 | 0.1354 | 0.1334 |
| Residue in Ramachandran zone | |||
| Favored/allowed | 260 (98.5%)/4 (1.5%) | 262 (99.2%)/2 (0.8%) | 759 (98.8%)/9 (1.2%) |
| Disallowed | 0 | 0 | 0 |
| r.m.s.d. values from ideality | |||
| Bond lengths | 0.013 Å | 0.014 Å | 0.013 Å |
| Bond angles | 0.031 Å | 0.029 Å | 0.031 Å |
| Zero chiral volumes | 0.080 Å3 | 0.081 Å3 | 0.074 Å3 |
| Nonzero chiral volumes | 0.088 Å3 | 0.096 Å3 | 0.080 Å3 |
| Mean B-factor (no. of atoms) | |||
| Protein | 9.35 (2130) | 12.57 (2104) | 16.39 (6039) |
| Solvent | 21.83 (249) | 26.27 (171) | 31.16 (929) |
| Others | 14.06 (19) | 35.38 (23) | None |
| Total | 10.68 (2398) | 13.82 (2298) | 18.36 (6968) |
| No. of hydrogen atoms | 2137 | 2088 | 5949 |
a Rfree values were calculated from 3% of reflections, respectively.