5P12

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 85

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)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	45.363, 73.138, 52.929
Unit cell angles	90.00, 109.65, 90.00

Refinement procedure

Resolution	34.889 - 1.549
R-factor	0.1416
Rwork	0.140
R-free	0.17730
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.008
RMSD bond angle	1.121
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]	42.722		1.640
High resolution limit [Å]	1.550	4.620	1.550
Rmerge	0.090	0.029	0.671
Rmeas	0.103	0.035	0.769
Total number of observations	196261
Number of reflections	47190	1799	7526
<I/σ(I)>	13.17	39.2	2.15
Completeness [%]	99.5	97.3	98.8
Redundancy	4.158
CC(1/2)	0.998	0.998	0.749

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 85 with the SMILES code ClCC(=O)NC1=NC=CC=N1