6QAF

Crystal structure of human Arginase-1 at pH 9.0 in complex with CB-1158/INCB001158

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	ESRF BEAMLINE MASSIF-1
Synchrotron site	ESRF
Beamline	MASSIF-1
Temperature [K]	100
Detector technology	PIXEL
Collection date	2017-12-14
Detector	DECTRIS PILATUS3 2M
Wavelength(s)	0.966
Spacegroup name	P 3
Unit cell lengths	90.130, 90.130, 69.111
Unit cell angles	90.00, 90.00, 120.00

Refinement procedure

Resolution	51.740 - 1.610
R-factor	0.149
Rwork	0.147
R-free	0.17700
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	6q9p
RMSD bond length	0.009
RMSD bond angle	1.356
Data reduction software	MOSFLM (7.2.0)
Data scaling software	Aimless (0.7.1)
Phasing software	MOLREP (11.6.02)
Refinement software	REFMAC (5.8.0218)

Data quality characteristics

	Overall	Outer shell
Low resolution limit [Å]	51.740	1.640
High resolution limit [Å]	1.610	1.610
Rmerge	0.058	0.658
Rmeas	0.076	0.868
Rpim	0.049	0.561
Number of reflections	79090	3888
<I/σ(I)>	6.9
Completeness [%]	96.9	96
Redundancy	2	2.1
CC(1/2)	0.996	0.368

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, HANGING DROP	4	293	Crystals were generated from 22.5 % PEG 1500, 0.2 M MIB buffer pH 4.0 (sodium malonate, imidazole and boric acid in a 2:3:3 molar ratio). Crystals were equilibrated to soaking solution (22.5 % PEG 1500, 0.2 M MMT buffer pH 9.0 (DL-malic acid, MES, Tris base in a 1:2:2 molar ratio). Subsequently, crystals were gradually soaked for 4 days in soaking solution containing 15 mM compound 3.