5P2J

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 137

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	45.268, 73.317, 52.801
Unit cell angles	90.00, 109.32, 90.00

Refinement procedure

Resolution	21.942 - 1.559
R-factor	0.1438
Rwork	0.142
R-free	0.18230
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.008
RMSD bond angle	1.157
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]	42.719		1.650
High resolution limit [Å]	1.560	4.650	1.560
Rmerge	0.081	0.028	0.618
Rmeas	0.093	0.032	0.711
Total number of observations	193060
Number of reflections	46280	1789	7358
<I/σ(I)>	13.13	41.64	2.41
Completeness [%]	99.5	98.9	98.8
Redundancy	4.171
CC(1/2)	0.998	0.999	0.748

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 137 with the SMILES code ClC1=CC=C(C=C1)[C@@H](NC(=O)C1=CN=CC=N1)C1CC1