5P4A

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 199

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.1
Synchrotron site	BESSY
Beamline	14.1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2013-04-04
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.918409
Spacegroup name	P 21 21 21
Unit cell lengths	45.310, 72.638, 104.254
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	41.555 - 1.348
R-factor	0.1494
Rwork	0.148
R-free	0.17680
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.152
Data reduction software	XDS
Data scaling software	XDS
Phasing software	PHASER (2.5.7)
Refinement software	PHENIX

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	45.310		1.430
High resolution limit [Å]	1.350	4.030	1.350
Rmerge	0.071	0.031	0.488
Rmeas	0.077	0.034	0.526
Total number of observations	554659
Number of reflections	76321	3093	12003
<I/σ(I)>	17.64	51.43	3.87
Completeness [%]	99.5	99.3	97.9
Redundancy	7.267
CC(1/2)	0.999	0.999	0.881

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	4.6	290	0.1 M ammonium acetate, 0.1 M sodium acetate, 24-30% PEG 4000; crystal obtained by streak-seeding and soaked with 90 mM of fragment 199 with the SMILES code O=C1NC(=O)C2(CCCCC2)N1