5P35

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 158

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 1 21 1
Unit cell lengths	45.291, 72.856, 52.624
Unit cell angles	90.00, 109.32, 90.00

Refinement procedure

Resolution	42.740 - 1.240
R-factor	0.1299
Rwork	0.129
R-free	0.14890
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.192
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]	42.740		1.310
High resolution limit [Å]	1.240	3.710	1.240
Rmerge	0.030	0.011	0.248
Rmeas	0.036	0.013	0.298
Total number of observations	276386
Number of reflections	86046	3415	12396
<I/σ(I)>	21.58	87.07	4.07
Completeness [%]	94.2	97.3	84.2
Redundancy	3.212
CC(1/2)	1.000	1.000	0.932

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 158 with the SMILES code CC(C)C1=NOC(NC(=O)CN2CCC(C)CC2)=C1