5P8B

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 344

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	2014-01-22
Detector	MAR CCD 165 mm
Wavelength(s)	0.8944
Spacegroup name	P 1 21 1
Unit cell lengths	45.290, 72.986, 52.770
Unit cell angles	90.00, 109.46, 90.00

Refinement procedure

Resolution	22.268 - 1.548
R-factor	0.1491
Rwork	0.146
R-free	0.19900
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.008
RMSD bond angle	1.114
Data reduction software	HKL-2000
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]	30.000	30.000	1.580
High resolution limit [Å]	1.550	4.200	1.550
Rmerge	0.062	0.018	0.422
Total number of observations	95741
Number of reflections	38417
<I/σ(I)>	9.1
Completeness [%]	81.8	74.1	69.1
Redundancy	2.5	2.8	2.4

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 344 with the SMILES code CCN1C=C(C=N1)C1=NC2=CC=CC=C2N1