4WQ2

Human calpain PEF(S) with (Z)-3-(6-bromondol-3-yl)-2-mercaptoacrylic acid bound

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	DIAMOND BEAMLINE I03
Synchrotron site	Diamond
Beamline	I03
Temperature [K]	100
Detector technology	PIXEL
Collection date	2013-03-16
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.976
Spacegroup name	P 1 21 1
Unit cell lengths	49.720, 78.430, 56.300
Unit cell angles	90.00, 91.12, 90.00

Refinement procedure

Resolution	41.990 - 1.640
R-factor	0.1713
Rwork	0.170
R-free	0.19660
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4phj
RMSD bond length	0.019
RMSD bond angle	1.967
Data reduction software	xia2
Data scaling software	Aimless (0.2.12)
Phasing software	PHASER
Refinement software	REFMAC (5.8.0049)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	41.990	41.990	1.680
High resolution limit [Å]	1.640	7.330	1.640
Rmerge	0.052	0.033	0.901
Rpim	0.031	0.022	0.547
Total number of observations	190491	1934	13583
Number of reflections	51550
<I/σ(I)>	16.1	40.2	1.7
Completeness [%]	97.5	89.5	96.5
Redundancy	3.7	3.4	3.6
CC(1/2)	0.997	0.989	0.666

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	7	294	3 UL PROTEIN (10 MG/ML PEF(S), 5 MM SODIUM CACODYLATE, 2 MM EDTA, 5 MM BME, 1 MM CALCIUM CHLORIDE, PH 7.0) + 3 UL PRECIPITANT (50 MM SODIUM CACODYLATE, 12.5% PEG6000, 20 MM CALCIUM CHLORIDE, PH 7.0) + 1 UL WATER