7M41

Structure of TIM-3 in complex with N-(4-(8-chloro-2-methyl-5-oxo-5,6-dihydro-[1,2,4]traizolo[1,5-c]quinazolin-9-yl)-3-methylphenyl)-1H-imidazole-2-sulfonamide (compound 38)

Experimental procedure

Experimental method	SINGLE WAVELENGTH
Source type	SYNCHROTRON
Source details	APS BEAMLINE 21-ID-F
Synchrotron site	APS
Beamline	21-ID-F
Temperature [K]	100
Detector technology	CCD
Collection date	2019-11-26
Detector	RAYONIX MX300HE
Wavelength(s)	0.987
Spacegroup name	C 1 2 1
Unit cell lengths	85.215, 46.828, 53.905
Unit cell angles	90.00, 93.05, 90.00

Refinement procedure

Resolution	26.910 - 1.790
R-factor	0.172
Rwork	0.170
R-free	0.21270
Structure solution method	MOLECULAR REPLACEMENT
Starting model (for MR)	5f71
Data reduction software	HKL-2000
Data scaling software	HKL-2000
Phasing software	PHASER (2.8.3)
Refinement software	PHENIX (1.19.1_4122)

Data quality characteristics

	Overall	Inner shell	Outer shell
Low resolution limit [Å]	30.000	30.000	1.830
High resolution limit [Å]	1.790	4.880	1.790
Rmerge	0.088	0.053	0.289
Rmeas	0.095	0.057	0.309
Rpim	0.034	0.021	0.111
Number of reflections	19569	1036	933
<I/σ(I)>	11.3
Completeness [%]	97.8	99	96.5
Redundancy	7.6	7.1	7.8
CC(1/2)		0.998	0.979

Crystallization Conditions

crystal ID	method	pH	temperature	details
1	VAPOR DIFFUSION, SITTING DROP		291	0.8 M sodium tartrate dibasic dihydrate, 0.1 M HEPES pH 6.8-8.2, and 10 mM CaCl2