5P5Q

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 251

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)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	45.340, 73.230, 52.770
Unit cell angles	90.00, 109.31, 90.00

Refinement procedure

Resolution	41.181 - 1.284
R-factor	0.1219
Rwork	0.121
R-free	0.14030
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.200
Data reduction software	iMOSFLM
Data scaling software	SCALA
Phasing software	PHASER (2.5.7)
Refinement software	PHENIX

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	42.790	42.789	1.350
High resolution limit [Å]	1.284	4.060	1.280
Rmerge	0.050	0.035	0.225
Rmeas	0.058	0.041	0.265
Rpim	0.030	0.021	0.138
Total number of observations	282021	9346	41814
Number of reflections	82272
<I/σ(I)>	13.1	29.9	4.9
Completeness [%]	99.3	99.8	99.1
Redundancy	3.4	3.5	3.5

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 251 with the SMILES code C[C@H]1C[C@H]1C(=O)NCC1=CC=C(C=C1)N1CCCC1=O