5P3N

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 176

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	45.225, 72.590, 104.208
Unit cell angles	90.00, 90.00, 90.00

Refinement procedure

Resolution	42.329 - 1.439
R-factor	0.1391
Rwork	0.138
R-free	0.16840
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.171
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]	45.225		1.530
High resolution limit [Å]	1.440	4.300	1.440
Rmerge	0.057	0.019	0.474
Rmeas	0.063	0.021	0.529
Total number of observations	337583
Number of reflections	62654	2571	9869
<I/σ(I)>	20.31	69.43	3.32
Completeness [%]	99.3	99.7	98.1
Redundancy	5.388
CC(1/2)	0.999	1.000	0.870

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 176 with the SMILES code OC(=O)CN1C=C(Br)C=CC1=O