5P8V

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 364

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	2014-01-22
Detector	MAR CCD 165 mm
Wavelength(s)	0.895
Spacegroup name	P 1 21 1
Unit cell lengths	45.463, 73.308, 53.019
Unit cell angles	90.00, 109.62, 90.00

Refinement procedure

Resolution	42.824 - 1.579
R-factor	0.137
Rwork	0.135
R-free	0.17350
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.008
RMSD bond angle	1.137
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]	42.824		1.670
High resolution limit [Å]	1.580	4.710	1.580
Rmerge	0.070	0.022	0.491
Rmeas	0.079	0.025	0.562
Total number of observations	189287
Number of reflections	44898	1745	7185
<I/σ(I)>	17.89	53.19	3.35
Completeness [%]	99.6	99	99
Redundancy	4.215
CC(1/2)	0.999	0.999	0.833

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 364 with the SMILES code CC1=CC(C(O)=O)=C2C=NN(C3CCCC3)C2=N1