4WQ3

Human calpain PEF(S) with (2Z,2Z')-2,2'-disulfanediylbis(3-(6-bromoindol-3-yl)acrylic acid) bound

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	2013-03-16
Detector	DECTRIS PILATUS 2M
Wavelength(s)	0.920
Spacegroup name	P 1 21 1
Unit cell lengths	49.560, 79.310, 57.020
Unit cell angles	90.00, 91.47, 90.00

Refinement procedure

Resolution	39.650 - 1.790
R-factor	0.1795
Rwork	0.178
R-free	0.21490
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4phj
RMSD bond length	0.021
RMSD bond angle	2.024
Data reduction software	xia2
Data scaling software	Aimless (0.1.27)
Phasing software	PHASER
Refinement software	REFMAC (5.8.0049)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	39.650	39.650	1.840
High resolution limit [Å]	1.790	8.010	1.790
Rmerge	0.071	0.038	0.634
Rpim	0.043	0.021	0.368
Total number of observations	150579	1880	12226
Number of reflections	40565
<I/σ(I)>	11	29.6	2
Completeness [%]	97.6	96.5	99.8
Redundancy	3.7	3.9	3.9
CC(1/2)	0.994	0.998	0.744

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING 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