7M3Y
Structure of TIM-3 in complex with 8-chloro-2-methyl-9-(3-mehtylpyridin-4-yl)-[1,2,4]triazolo[1,5-c]quinazolin-5(6H)-one (compound 22)
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 | 2018-07-19 |
Detector | RAYONIX MX300HE |
Wavelength(s) | 0.987 |
Spacegroup name | C 2 2 21 |
Unit cell lengths | 46.958, 85.343, 53.697 |
Unit cell angles | 90.00, 90.00, 90.00 |
Refinement procedure
Resolution | 26.850 - 1.690 |
R-factor | 0.1882 |
Rwork | 0.187 |
R-free | 0.21310 |
Structure solution method | MOLECULAR REPLACEMENT |
Starting model (for MR) | 5f71 |
Data reduction software | HKL-2000 |
Data scaling software | HKL-2000 |
Phasing software | PHASER (2.8.1) |
Refinement software | PHENIX (1.19.1_4122) |
Data quality characteristics
Overall | Inner shell | Outer shell | |
Low resolution limit [Å] | 30.000 | 30.000 | 1.720 |
High resolution limit [Å] | 1.690 | 4.580 | 1.690 |
Rmerge | 0.097 | 0.037 | 0.763 |
Rmeas | 0.104 | 0.040 | 0.817 |
Rpim | 0.036 | 0.015 | 0.288 |
Total number of observations | 99824 | ||
Number of reflections | 12404 | 689 | 607 |
<I/σ(I)> | 6.3 | ||
Completeness [%] | 100.0 | 99.9 | 100 |
Redundancy | 8 | 7.3 | 7.9 |
CC(1/2) | 0.999 | 0.766 |
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 |