5UUU

Design, Synthesis, and Evaluation of the First Selective and Potent G-protein-Coupled Receptor Kinase 2 (GRK2) Inhibitor for the Potential Treatment of Heart Failure

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	SSRL BEAMLINE BL14-1
Synchrotron site	SSRL
Beamline	BL14-1
Temperature [K]	100
Detector technology	CCD
Collection date	2014-07-10
Detector	MARMOSAIC 325 mm CCD
Wavelength(s)	0.97949
Spacegroup name	P 31 2 1
Unit cell lengths	126.180, 126.180, 96.369
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	30.000 - 2.700
R-factor	0.2151
Rwork	0.213
R-free	0.25700
Structure solution method	MOLECULAR REPLACEMENT
RMSD bond length	0.007
RMSD bond angle	1.065
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	PHASER
Refinement software	REFMAC

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	50.000	50.000	2.750
High resolution limit [Å]	2.700	7.320	2.700
Rmerge	0.083	0.024
Rmeas	0.089	0.026
Rpim	0.039	0.010	0.649
Total number of observations	177721
Number of reflections	24714
<I/σ(I)>	7.1
Completeness [%]	100.0	99.5	100
Redundancy	7.2	6.7	7.3
CC(1/2)		0.999	0.557

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	5.6	273	18% PEG MME 2000, 0.1 M MES pH 5.6, and 0.0175M Ammonium Sulfate