5P3S

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 181

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	45.169, 72.992, 52.560
Unit cell angles	90.00, 109.11, 90.00

Refinement procedure

Resolution	42.680 - 1.170
R-factor	0.1258
Rwork	0.125
R-free	0.14150
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.199
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]	42.680		1.240
High resolution limit [Å]	1.170	3.500	1.170
Rmerge	0.032	0.020	0.188
Rmeas	0.037	0.023	0.239
Total number of observations	364243
Number of reflections	102974	4134	12665
<I/σ(I)>	19.86	61.48	4.28
Completeness [%]	94.9	99.5	72.4
Redundancy	3.537
CC(1/2)	0.999	0.999	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 181 with the SMILES code C[C@H]1C[C@@H](C)CN(CC2=NC(N)=NC(=N2)N(C)C)C1