5P4E

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 203

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	2013-04-12
Detector	MAR CCD 165 mm
Wavelength(s)	0.8944
Spacegroup name	P 1 21 1
Unit cell lengths	45.249, 73.035, 52.712
Unit cell angles	90.00, 109.16, 90.00

Refinement procedure

Resolution	29.447 - 1.399
R-factor	0.1327
Rwork	0.131
R-free	0.15690
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.007
RMSD bond angle	1.161
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]	42.742		1.480
High resolution limit [Å]	1.400	4.180	1.400
Rmerge	0.062	0.024	0.482
Rmeas	0.071	0.027	0.560
Total number of observations	248796
Number of reflections	63639	2454	10178
<I/σ(I)>	15.65	49.85	3.08
Completeness [%]	99.5	99.4	98.6
Redundancy	3.909
CC(1/2)	0.999	0.999	0.816

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 203 with the SMILES code CSC1=NNC(N)=C1S(=O)(=O)C(C)C