8E2M
Bruton's tyrosine kinase (BTK) with compound 13
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | APS BEAMLINE 17-ID |
Synchrotron site | APS |
Beamline | 17-ID |
Temperature [K] | 100 |
Detector technology | PIXEL |
Collection date | 2015-10-26 |
Detector | DECTRIS PILATUS 6M |
Wavelength(s) | 1.000 |
Spacegroup name | P 2 21 21 |
Unit cell lengths | 38.155, 72.394, 103.946 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 38.155 - 1.904 |
R-factor | 0.1579 |
Rwork | 0.154 |
R-free | 0.19910 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | Internal Previously Solved BTK Structure |
RMSD bond length | 0.009 |
RMSD bond angle | 0.870 |
Data reduction software | DENZO |
Data scaling software | SCALEPACK |
Phasing software | PHASER (2.6.0) |
Refinement software | PHENIX (1.10_2155) |
Data quality characteristics
Overall | Inner shell | Outer shell | |
Low resolution limit [Å] | 50.000 | 50.000 | 1.930 |
High resolution limit [Å] | 1.900 | 5.160 | 1.900 |
Rmerge | 0.124 | 0.056 | 0.543 |
Rmeas | 0.141 | 0.065 | 0.618 |
Rpim | 0.065 | 0.031 | 0.290 |
Number of reflections | 23105 | 1290 | 1103 |
<I/σ(I)> | 15.1 | ||
Completeness [%] | 99.4 | 99.1 | 98.4 |
Redundancy | 4.3 | 3.9 | 4.1 |
CC(1/2) | 0.996 | 0.835 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, HANGING DROP | 6.5 | 277 | 25-33% PEG-5000 MME, 100 mM MES pH 6.35-6.75, 200 mM Ammonium Sulfate |