5P51

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 226

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.3
Synchrotron site	BESSY
Beamline	14.3
Temperature [K]	100
Detector technology	CCD
Collection date	2013-04-18
Detector	MAR CCD 165 mm
Wavelength(s)	0.8944
Spacegroup name	P 1 21 1
Unit cell lengths	45.235, 73.154, 52.701
Unit cell angles	90.00, 109.22, 90.00

Refinement procedure

Resolution	27.782 - 1.119
R-factor	0.1314
Rwork	0.131
R-free	0.14910
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.202
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]	42.714		1.190
High resolution limit [Å]	1.120	3.350	1.120
Rmerge	0.045	0.022	0.365
Rmeas	0.056	0.026	0.498
Total number of observations	294231
Number of reflections	115035	4272	14352
<I/σ(I)>	14.64	48.77	2.43
Completeness [%]	92.4	89.8	71.6
Redundancy	2.557
CC(1/2)	0.999	0.998	0.753

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 226 with the SMILES code FC(F)(F)[C@@H]1C[C@@H](NC2=C(C=NN12)C#N)C1CC1