5P1E

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 97

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	2015-07-17
Detector	MAR CCD 165 mm
Wavelength(s)	0.895
Spacegroup name	P 1 21 1
Unit cell lengths	45.191, 72.793, 52.596
Unit cell angles	90.00, 109.11, 90.00

Refinement procedure

Resolution	28.150 - 1.589
R-factor	0.1376
Rwork	0.136
R-free	0.17560
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.008
RMSD bond angle	1.151
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]	42.700		1.690
High resolution limit [Å]	1.590	4.740	1.590
Rmerge	0.104	0.035	0.498
Rmeas	0.118	0.040	0.572
Total number of observations	180578
Number of reflections	43186	1649	6851
<I/σ(I)>	17.42	44.88	3.37
Completeness [%]	99.5	97.9	98.3
Redundancy	4.181
CC(1/2)	0.998	0.998	0.839

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 97 with the SMILES code ClC1=CC2=C(N=C3CCCN3C2=O)C(Cl)=C1