3O65
Crystal structure of a Josephin-ubiquitin complex: Evolutionary restraints on ataxin-3 deubiquitinating activity
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | NSLS BEAMLINE X6A |
Synchrotron site | NSLS |
Beamline | X6A |
Detector technology | CCD |
Collection date | 2008-10-10 |
Detector | ADSC QUANTUM 210 |
Wavelength(s) | 0.9780 |
Spacegroup name | P 3 2 1 |
Unit cell lengths | 159.150, 159.150, 146.290 |
Unit cell angles | 90.00, 90.00, 120.00 |
Refinement procedure
Resolution | 19.903 - 2.700 |
R-factor | 0.1781 |
Rwork | 0.176 |
R-free | 0.22420 |
Structure solution method | SAD |
RMSD bond length | 0.009 |
RMSD bond angle | 1.140 |
Data reduction software | XDS |
Data scaling software | XSCALE |
Phasing software | RESOLVE (2.14) |
Refinement software | PHENIX (1.6.1_357) |
Data quality characteristics
Overall | Inner shell | Outer shell | |
Low resolution limit [Å] | 2.770 | ||
High resolution limit [Å] | 2.700 | 12.080 | 2.700 |
Rmerge | 0.096 | 0.040 | 0.588 |
Number of reflections | 112055 | 992 | 7798 |
<I/σ(I)> | 15.42 | 37.3 | 1.6 |
Completeness [%] | 98.4 | 77.4 | 92.9 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | 6.5 | 291 | The protein complex was at 8 mg/ml in 10 mM Tris pH 7,5mm DTT. 2 microlitres drops were set up under paraffin oil. To 1.1 microlitres of precipitant (1.6 M sodium citrate pH 6.5, pH adjusted with HCl) 0.9 microlitres of protein was added, the final concentration of precipitant was therefore 0.88 M sodium citrate. For cryo crystals were passed through the 1.6 M sodium citrate pH 6.5 preciptant solution and then flash frozen in liquid nitrogen, microbatch under paraffin oil, temperature 291K |