4IJP
Crystal Structure of Human PRPF4B kinase domain in complex with 4-{5-[(2-Chloro-pyridin-4-ylmethyl)-carbamoyl]-thiophen-2-yl}-benzo[b]thiophene-2-carboxylic acid amine
Experimental procedure
Experimental method | SINGLE WAVELENGTH |
Source type | SYNCHROTRON |
Source details | APS BEAMLINE 21-ID-F |
Synchrotron site | APS |
Beamline | 21-ID-F |
Temperature [K] | 100 |
Detector technology | CCD |
Collection date | 2011-06-13 |
Detector | MARMOSAIC 225 mm CCD |
Wavelength(s) | 0.979 |
Spacegroup name | P 1 |
Unit cell lengths | 52.140, 52.540, 79.130 |
Unit cell angles | 102.56, 105.25, 92.29 |
Refinement procedure
Resolution | 47.610 - 2.250 |
R-factor | 0.2504 |
Rwork | 0.250 |
R-free | 0.26490 |
Structure solution method | MOLECULAR REPLACEMENT |
RMSD bond length | 0.008 |
RMSD bond angle | 1.010 |
Data reduction software | DENZO |
Data scaling software | SCALEPACK |
Refinement software | BUSTER-TNT (BUSTER 2.9.1) |
Data quality characteristics
Overall | Inner shell | Outer shell | |
Low resolution limit [Å] | 50.000 | 50.000 | 2.330 |
High resolution limit [Å] | 2.250 | 4.850 | 2.250 |
Rmerge | 0.051 | 0.027 | 0.427 |
Number of reflections | 36692 | ||
<I/σ(I)> | 8.5 | ||
Completeness [%] | 98.4 | 99.3 | 97.5 |
Redundancy | 2.3 | 2.3 | 2.3 |
Crystallization Conditions
crystal ID | method | pH | temperature | details |
1 | VAPOR DIFFUSION, HANGING DROP | 7 | 291 | 0.2M ammonium sulfate, 20-30% PEG 3350 and 0.1M HEPES pH7.0 5 mM compound final concentration added to cryo-protectant solution for soaking of apo crystals, VAPOR DIFFUSION, HANGING DROP, temperature 291K |