6D1Z

Crystal structure of Tyrosine-protein kinase receptor in complex with 5-(4-fluorophenyl)thieno[2,3-d]pyrimidin-4(3H)-one Inhibitor

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	DIAMOND BEAMLINE I02
Synchrotron site	Diamond
Beamline	I02
Temperature [K]	93
Detector technology	PIXEL
Collection date	2013-05-09
Detector	DECTRIS PILATUS3 6M
Wavelength(s)	1
Spacegroup name	C 1 2 1
Unit cell lengths	113.150, 45.660, 78.880
Unit cell angles	90.00, 126.88, 90.00

Refinement procedure

Resolution	39.150 - 1.870
R-factor	0.1797
Rwork	0.178
R-free	0.20960
RMSD bond length	0.010
RMSD bond angle	0.950
Data reduction software	xia2
Data scaling software	Aimless (0.1.27)
Phasing software	BUSTER
Refinement software	BUSTER

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	39.150	39.150	1.920
High resolution limit [Å]	1.870	8.360	1.870
Rmerge	0.109	0.030	0.860
Rmeas	0.131	0.037	1.030
Rpim	0.072	0.022	0.569
Total number of observations	84657
Number of reflections	26217	274	1963
<I/σ(I)>	9.7
Completeness [%]	97.6	80.2	99.1
Redundancy	3.2	2.9	3.2
CC(1/2)	0.978	0.996	0.392

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7.63	294	Well volume: 30.0 uL Well Ingredients: Salt: 0.2571428571 M (1.9285714282 uL of stock 4.0 M) potassium formate Precipitant: 20.0 %w/v (12.0 uL of stock 50.0 %w/v) PEG 3350 Buffer: 0.1 M (3.0 uL of stock 1.0 M) Tris (pH 7.63) Plate setup temperature: 13 C Plate incubation temperature: 21 C Drop volume from well: 0.1 uL Drop protein volume: 0.3 uL Protein: 6.00 mg/mL (0.17 mM) Compound1: small molecule to aid crystallization (1.20 mM) Soak of 10mM compound 3 for > 1h into co-crystals of TrkA + compound1