5P3D

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 166

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	45.276, 73.095, 52.620
Unit cell angles	90.00, 109.33, 90.00

Refinement procedure

Resolution	42.725 - 1.180
R-factor	0.1259
Rwork	0.125
R-free	0.14340
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.216
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]	42.725		1.250
High resolution limit [Å]	1.180	3.530	1.180
Rmerge	0.040	0.030	0.171
Rmeas	0.049	0.036	0.220
Total number of observations	238554
Number of reflections	96335	3453	12392
<I/σ(I)>	13.36	36.63	3.78
Completeness [%]	90.7	85	72.3
Redundancy	2.476
CC(1/2)	0.998	0.998	0.942

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 166 with the SMILES code C[C@H](OC(=O)C1=CC2=C(CCC2)S1)C(N)=O