5P2U

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 147

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.3
Synchrotron site	BESSY
Beamline	14.3
Temperature [K]	100
Detector technology	CCD
Collection date	2014-02-15
Detector	MAR CCD 165 mm
Wavelength(s)	0.8944
Spacegroup name	P 1 21 1
Unit cell lengths	45.254, 72.845, 52.570
Unit cell angles	90.00, 109.27, 90.00

Refinement procedure

Resolution	22.500 - 1.379
R-factor	0.1321
Rwork	0.131
R-free	0.16170
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.188
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]	42.718		1.460
High resolution limit [Å]	1.380	4.120	1.380
Rmerge	0.052	0.021	0.462
Rmeas	0.059	0.024	0.532
Total number of observations	275267
Number of reflections	66059	2536	10526
<I/σ(I)>	17.32	55.11	2.96
Completeness [%]	99.6	99.3	98.6
Redundancy	4.166
CC(1/2)	0.999	0.999	0.831

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 147 with the SMILES code CC(C)OC(=O)C1=C(C)C(C(C)=O)=C(C)N1