5P0A

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 57

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	CCD
Collection date	2012-11-16
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.8912
Spacegroup name	P 1 21 1
Unit cell lengths	45.196, 72.689, 52.579
Unit cell angles	90.00, 109.49, 90.00

Refinement procedure

Resolution	42.605 - 1.818
R-factor	0.1481
Rwork	0.145
R-free	0.21280
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.010
RMSD bond angle	1.181
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]	42.605		1.930
High resolution limit [Å]	1.820	5.420	1.820
Rmerge	0.096	0.031	0.494
Rmeas	0.110	0.036	0.567
Total number of observations	120060
Number of reflections	28747	1097	4568
<I/σ(I)>	15.41	39.92	3.28
Completeness [%]	99.4	95.8	98.8
Redundancy	4.176
CC(1/2)	0.997	0.999	0.848

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 57 with the SMILES code NC1=C(N)C=C(Br)C=C1