5P54

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 229

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	2014-06-04
Detector	DECTRIS PILATUS 6M
Wavelength(s)	0.918409
Spacegroup name	P 1 21 1
Unit cell lengths	45.261, 72.944, 52.735
Unit cell angles	90.00, 109.41, 90.00

Refinement procedure

Resolution	26.806 - 1.087
R-factor	0.13
Rwork	0.130
R-free	0.13980
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.207
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]	42.687		1.150
High resolution limit [Å]	1.090	3.250	1.090
Rmerge	0.046	0.023	0.419
Rmeas	0.054	0.027	0.496
Total number of observations	478496
Number of reflections	134127	5139	20972
<I/σ(I)>	14.45	50.43	2.52
Completeness [%]	99.0	99.2	96.1
Redundancy	3.567
CC(1/2)	0.999	0.999	0.815

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 229 with the SMILES code CC1=CC(=O)N2C3=C(CCCC3)C(C#N)=C2N1