9D02

Co-crystal structure of circularly permuted human taspase-1 bound to ligand SMDC1014883 (2R)-4-(ethenesulfonyl)-1-{[3-fluoro-4-(trifluoromethoxy)phenyl]methyl}-2-[(prop-2-yn-1-yloxy)methyl]piperazine

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	CLSI BEAMLINE 08ID-1
Synchrotron site	CLSI
Beamline	08ID-1
Temperature [K]	100
Detector technology	CCD
Collection date	2017-05-17
Detector	MARMOSAIC 225 mm CCD
Wavelength(s)	0.97856
Spacegroup name	P 65
Unit cell lengths	60.430, 60.430, 317.710
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	49.710 - 2.150
R-factor	0.159
Rwork	0.157
R-free	0.19500
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	internal molecule
Data reduction software	XDS
Data scaling software	XSCALE
Phasing software	PHENIX
Refinement software	PHENIX (DEV_2733)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	49.710	49.710
High resolution limit [Å]	2.150	2.150
Rmerge	0.074	0.530
Rmeas	0.081	0.048
Total number of observations	202637
Number of reflections	35557	422
<I/σ(I)>	15.07	2.91
Completeness [%]	99.9	99.9
Redundancy	5.699	5.334
CC(1/2)	0.998	0.997

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP	5.8	287	Human taspase-1 VCID 11900 at 9.23 mg/mL in 20 mM HEPES pH 8, 0.5 M NaCl, 5% glycerol against Pact screen condition B11 containing 0.1M MES, pH 5.8, 17% PEG 6000, 0.2M Calcium chloride + 2.5mM 108131 (SMDC1014883) supplemented with 20% ethylene glycol as a cryo-protectant, crystal tracking ID 291536 B3, unique puck ID zhg3-3