5P2V

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 148

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	45.235, 73.058, 52.758
Unit cell angles	90.00, 109.37, 90.00

Refinement procedure

Resolution	24.886 - 1.317
R-factor	0.127
Rwork	0.126
R-free	0.14650
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.195
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]	42.675		1.400
High resolution limit [Å]	1.320	3.940	1.320
Rmerge	0.054	0.019	0.485
Rmeas	0.062	0.022	0.558
Total number of observations	315683
Number of reflections	75902	2927	11900
<I/σ(I)>	18.27	58.31	3.03
Completeness [%]	99.2	98.9	96.8
Redundancy	4.159
CC(1/2)	0.999	0.999	0.832

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 148 with the SMILES code O=C(CC1=CC=CC=C1)NN1C=NC2=CC=CC=C12