6Z55

Crystal structure of CLK3 in complex with macrocycle ODS2004070

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	DIAMOND BEAMLINE I04-1
Synchrotron site	Diamond
Beamline	I04-1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2012-07-13
Detector	DECTRIS PILATUS3 2M
Wavelength(s)	0.9200
Spacegroup name	C 1 2 1
Unit cell lengths	96.730, 131.360, 83.800
Unit cell angles	90.00, 107.80, 90.00

Refinement procedure

Resolution	37.990 - 1.700
R-factor	0.1584
Rwork	0.157
R-free	0.19500
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	2eu9
RMSD bond length	0.014
RMSD bond angle	1.807
Data reduction software	iMOSFLM
Data scaling software	SCALA (3.3.20)
Phasing software	PHASER
Refinement software	REFMAC (5.8.0258)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	79.788	37.958	1.790
High resolution limit [Å]	1.700	5.380	1.700
Rmerge		0.040	0.733
Rmeas	0.083	0.045	0.830
Rpim	0.038	0.019	0.382
Total number of observations	469469	17440	69001
Number of reflections	104048	3472	15308
<I/σ(I)>	10.7	30.7	2
Completeness [%]	95.5	98.5	96.5
Redundancy	4.5	5	4.5

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	7	277.15	18% PEG 3350, 0.2M potassium/sodium phosphate, 0.1M bis-tris-propane pH 7.0, 10% ethylene glycol