4WQ3
Human calpain PEF(S) with (2Z,2Z')-2,2'-disulfanediylbis(3-(6-bromoindol-3-yl)acrylic acid) bound
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | DIAMOND BEAMLINE I04-1 |
Synchrotron site | Diamond |
Beamline | I04-1 |
Temperature [K] | 100 |
Detector technology | PIXEL |
Collection date | 2013-03-16 |
Detector | DECTRIS PILATUS 2M |
Wavelength(s) | 0.920 |
Spacegroup name | P 1 21 1 |
Unit cell lengths | 49.560, 79.310, 57.020 |
Unit cell angles | 90.00, 91.47, 90.00 |
Refinement procedure
Resolution | 39.650 - 1.790 |
R-factor | 0.1795 |
Rwork | 0.178 |
R-free | 0.21490 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | 4phj |
RMSD bond length | 0.021 |
RMSD bond angle | 2.024 |
Data reduction software | xia2 |
Data scaling software | Aimless (0.1.27) |
Phasing software | PHASER |
Refinement software | REFMAC (5.8.0049) |
Data quality characteristics
Overall | Inner shell | Outer shell | |
Low resolution limit [Å] | 39.650 | 39.650 | 1.840 |
High resolution limit [Å] | 1.790 | 8.010 | 1.790 |
Rmerge | 0.071 | 0.038 | 0.634 |
Rpim | 0.043 | 0.021 | 0.368 |
Total number of observations | 150579 | 1880 | 12226 |
Number of reflections | 40565 | ||
<I/σ(I)> | 11 | 29.6 | 2 |
Completeness [%] | 97.6 | 96.5 | 99.8 |
Redundancy | 3.7 | 3.9 | 3.9 |
CC(1/2) | 0.994 | 0.998 | 0.744 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, SITTING DROP | 7 | 294 | 3 UL PROTEIN (10 MG/ML PEF(S), 5 MM SODIUM CACODYLATE, 2 MM EDTA, 5 MM BME, 1 MM CALCIUM CHLORIDE, PH 7.0) + 3 UL PRECIPITANT (50 MM SODIUM CACODYLATE, 12.5% PEG6000, 20 MM CALCIUM CHLORIDE, PH 7.0) + 1 UL WATER |