TABLE 1.
Crystallographic data collection and refinement statistics
| Closed CAlipase (Wild-Type) | Blocked CAlipase (BMK-Bound) | Open CAlipase (LPC-Bound) | |
| Data collection | |||
| Beamline | PAL-5C | PAL-7A | PAL-7A |
| Wavelength (Å) | 0.98 | 0.98 | 0.98 |
| Resolution range (Å)a | 38.36–1.75 | 31.89–1.60 | 35.88–2.40 |
| Space group | P21212 | P21212 | P31 |
| Unit cell parameters (Å) | a = 55.3 | a = 94.5 | a = 185.9 |
| b = 93.3 | b = 129.7 | b = 185.9 | |
| c = 129.7 | c = 55.5 | c = 205.1 | |
| Observations (total/unique) | 68,476/63,249 | 91,178/89,860 | 311,475/68,958 |
| Completeness (%) | 92.8 (87.6) | 98.7 (84.0) | 97.6 (83.3) |
| Rsymb | 7.7 (29.5) | 6.1 (23.3) | 10.7 (34.1) |
| CC1/2 | 0.95 (0.82) | 0.99 (0.96) | 0.99 (0.83) |
| Redundancy | 3.7 (3.7) | 12.4 (5.9) | 3.5 (2.5) |
| I/sigma | 21.0 (10.1) | 25.7 (7.8) | 19.0 (5.8) |
| Refinement | |||
| Rworkc/Rfreec (%) | 17.9/22.2 | 14.5/16.7 | 18.5/25.6 |
| Protein/ligand atoms | 4,712/60 | 4,712/114 | 61,283/204 |
| Water molecules | 521 | 705 | 2515 |
| Average B value (Å2) | 18.0 | 14.0 | 32.0 |
| r.m.s.d. bond (Å) | 0.013 | 0.014 | 0.010 |
| r.m.s.d. angle (°) | 1.728 | 1.638 | 1.686 |
| Ramachandran plot (%) | |||
| Favored | 93.97 | 94.95 | 93.05 |
| Allowed | 5.70 | 5.05 | 6.79 |
| Disallowed | 0.33 | 0.00 | 0.16 |
a
Numbers in parentheses indicate the statistics for the last resolution shell.
b
Rsym = ∑(|Ihkl−<Ihkl>|/∑<Ihkl>, where Ihkl = single value of measured intensity of hkl reflection, and <Ihkl> = mean of all measured value intensity of hkl reflection.
c
Rwork = ∑(|Fobs−Fcalc|/∑Fobs, where Fobs = observed structure factor amplitude, and Fcalc = structure factor calculated from model. Rfree is computed in the same manner as Rwork, but from a test set containing 5% of data excluded from the refinement calculation.