5P5P

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 250

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.2
Synchrotron site	BESSY
Beamline	14.2
Temperature [K]	100
Detector technology	CCD
Collection date	2014-06-04
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	45.270, 72.836, 52.651
Unit cell angles	90.00, 109.33, 90.00

Refinement procedure

Resolution	34.717 - 1.090
R-factor	0.1294
Rwork	0.129
R-free	0.14550
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.208
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]	42.718		1.160
High resolution limit [Å]	1.090	3.260	1.090
Rmerge	0.048	0.020	0.444
Rmeas	0.055	0.023	0.532
Total number of observations	523897
Number of reflections	132550	5105	20308
<I/σ(I)>	16.55	61.87	2.53
Completeness [%]	98.8	99.4	93.7
Redundancy	3.952
CC(1/2)	0.999	0.999	0.786

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 250 with the SMILES code CN1C=CC(NC(=O)C2=COC(Br)=C2)=N1