5P0T

Automated refinement of diffraction data obtained from an endothiapepsin crystal treated with fragment 76

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	BESSY BEAMLINE 14.2
Synchrotron site	BESSY
Beamline	14.2
Temperature [K]	100
Detector technology	CCD
Collection date	2014-06-04
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.91841
Spacegroup name	P 1 21 1
Unit cell lengths	45.286, 72.838, 52.696
Unit cell angles	90.00, 109.38, 90.00

Refinement procedure

Resolution	29.379 - 1.129
R-factor	0.1316
Rwork	0.131
R-free	0.14610
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	4y5l
RMSD bond length	0.006
RMSD bond angle	1.209
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]	42.721		1.200
High resolution limit [Å]	1.130	3.380	1.130
Rmerge	0.053	0.017	0.534
Rmeas	0.061	0.020	0.624
Total number of observations	487908
Number of reflections	120304	4599	19315
<I/σ(I)>	16.49	67.75	2.51
Completeness [%]	99.7	99.4	99.3
Redundancy	4.055
CC(1/2)	0.999	0.999	0.778

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 76 with the SMILES code C1CCC2=C(C1)NC1=NC=NN1[C@H]2C1=CC=CC=C1