5P2F

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 133

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	2013-01-23
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	45.164, 73.198, 52.807
Unit cell angles	90.00, 109.19, 90.00

Refinement procedure

Resolution	26.285 - 1.797
R-factor	0.146
Rwork	0.143
R-free	0.20830
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.009
RMSD bond angle	1.167
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]	42.654		1.910
High resolution limit [Å]	1.800	5.350	1.800
Rmerge	0.100	0.030	0.551
Rmeas	0.115	0.035	0.632
Total number of observations	127595
Number of reflections	30211	1172	4822
<I/σ(I)>	13.03	39.32	2.76
Completeness [%]	99.6	98	98.9
Redundancy	4.223
CC(1/2)	0.997	0.999	0.784

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 133 with the SMILES code CC1=CC(Br)=CC=C1NC(=O)CN