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