1AQ1

HUMAN CYCLIN DEPENDENT KINASE 2 COMPLEXED WITH THE INHIBITOR STAUROSPORINE

Experimental procedure

Source type	SYNCHROTRON
Source details	ELETTRA BEAMLINE 5.2R
Synchrotron site	ELETTRA
Beamline	5.2R
Temperature [K]	100
Detector technology	IMAGE PLATE AREA DETECTOR
Collection date	1996-12
Detector	MARRESEARCH
Spacegroup name	P 21 21 21
Unit cell lengths	53.500, 70.500, 73.600
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	25.000 - 2.000
Rwork	0.220
R-free	0.26000
Structure solution method	DIFFERENCE FOURIER
Starting model (for MR)	1hck
Data reduction software	MOSFLM
Data scaling software	CCP4 ((SCALA))
Phasing software	CCP4
Refinement software	REFMAC

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	20.000	2.100
High resolution limit [Å]	2.000	2.000
Rmerge	0.101 *	0.500
Total number of observations	53349 *
Number of reflections	17731
<I/σ(I)>	5.7	1.4
Completeness [%]	92.9	89.4
Redundancy	3	2.7

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	Vapor diffusion, sitting drop *	7.4	20 *	PROTEIN AT 10MG/ML IN 15MM NACL, 10MM HEPES, PH7.4, MIXED WITH WELL BUFFER (50MM AMMONIUM ACETATE, 10% PEG4K, 0.1M HEPES PH 7.4) IN EQUAL VOLUMES, THEN VAPOUR DIFFUSION AGAINST WELL BUFFER. CDK2 CRYSTALS WERE SOAKED FOR 20 HOURS IN A SOLUTION OF 0.5MM STAUROSPORINE IN 1X WELL BUFFER PREPARED FROM STOCKS 2X WELLBUFFER AND 10MM STAUROSPORINE IN 100% DMSO., vapor diffusion

Crystallization Reagents in Literatures

ID	crystal ID	solution	reagent name	concentration (unit)	details
1	1	drop	CDK2	10 (mg/ml)
2	1	drop		15 (mM)
3	1	drop	HEPES	10 (mM)
4	1	reservoir		50 (mM)
5	1	reservoir	PEG4000	10 (%)
6	1	reservoir	HEPES	0.1 (M)