5HD4

Dissecting Therapeutic Resistance to ERK Inhibition Rat Wild Type SCH772984 in complex with (3R)-1-(2-oxo-2-{4-[4-(pyrimidin-2-yl)phenyl]piperazin-1-yl}ethyl)-N-[3-(pyridin-4-yl)-2H-indazol-5-yl]pyrrolidine-3-carboxamide

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 17-ID
Synchrotron site	APS
Beamline	17-ID
Temperature [K]	100
Detector technology	CCD
Collection date	2004-12-17
Detector	MAR CCD 165 mm
Wavelength(s)	1.00001
Spacegroup name	P 21 21 2
Unit cell lengths	71.532, 91.406, 63.227
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	23.070 - 1.450
R-factor	0.1775
Rwork	0.176
R-free	0.19920
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	1ERK
RMSD bond length	0.009
RMSD bond angle	1.000
Data reduction software	DENZO (1.97.7)
Data scaling software	SCALEPACK (1.97.7)
Phasing software	MOLREP
Refinement software	BUSTER (2.11.4)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	23.070	1.500
High resolution limit [Å]	1.450	1.450
Rmerge	0.049	0.523
Number of reflections	72235
<I/σ(I)>	14.5	2.8
Completeness [%]	97.8	97.3
Redundancy	4.4	3.9

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	6.4	277	0.1M MES, PH 6.4, 2.0M AMMONIUM SULFATE, 5% PEG 400, 0.5% DMSO, 1% GLYEROL, 0.0005M OLOMOUCINE, 10 DAY SOAK WITH NEW COMPOUND at 500 MICROMOLAR CONCENTRATION