Table 2.
Crystallographic data.
| Ligand | ALK-IN-1 | BI 2536 | GSK650394 |
|---|---|---|---|
| Data collection | |||
| X-ray source | DLS I24 | APS 24-ID-C | DLS I24 |
| Wavelength (Å) | 0.9686 | 0.9791 | 0.9686 |
| Space group | P1 | P43212 | P43212 |
| Cell dimensions | |||
|
a, b, c (Å) α, β, γ (°) |
54.8, 54.9, 56.6 72.4, 78.4, 89.7 |
73.5, 73.5, 119.3 90.0, 90.0, 90.0 |
73.0, 73.0, 119.3 90.0, 90.0, 90.0 |
| Resolution (Å)* | 19.72–2.20 (2.27–2.20) | 19.88–1.80 (1.84–1.80) |
19.97–2.00 (2.05–2.00) |
| No. of unique reflections* | 28,914 (2,482) | 31,086 (1,798) | 20,267 (1,601) |
| Rmerge (%)* | 7.80 (32.6) | 9.60 (115.0) | 9.60 (172.4) |
|
Mean I/σI * Mean CC(1/2)* |
5.8 (1.3) 1.0 (0.5) |
15.4 (2.2) 1.0 (0.8) |
12.5 (1.4) 1.0 (0.5) |
| Completeness (%)* | 92.8 (92.0) | 99.9 (100) | 89.9 (99.6) |
| Redundancy* | 1.8 (1.8) | 12.9 (12.8) | 10.3 (10.4) |
| Refinement | |||
| Resolution (Å) |
19.73–2.20 (2.26–2.20) |
19.88–1.80 (1.85–1.80) |
19.97–2.00 (2.05–2.00) |
| Rcryst/Rfree (%) | 18.2/22.1 | 19.1/22.8 | 19.3/23.7 |
| No. of atoms/Mean B-factor (Å) | |||
| Protein atoms | 3,967/50.1 | 2,114/30.4 | 2,081/46.4 |
| Solvent atoms | 80/44.1 | 192/39.1 | 102/53.3 |
| Ligand atoms | 73/47.5 | 38/23.4 | 32/39.8 |
| Rmsd bond lengths (Å) | 0.010 | 0.011 | 0.009 |
| Rmsd bong angles (degrees) | 1.03 | 1.43 | 1.31 |
| Ramachandran statistics (%) | |||
| Favored | 98.1 | 98.1 | 98.0 |
| Allowed | 1.9 | 1.9 | 2.0 |
| Outlier | 0 | 0 | 0 |
| PDB ID | 6BRC | 6BQQ | 6BKU |
| Crystallization conditions | 26% PEG 3350, 0.2 M ammonium sulfate, 0.1 M SBG buffer, pH 6.0 | 22% PEG 3350, 0.21 M ammonium sulfate, 0.1 M CHC buffer, pH 7.5 | 20% PEG smear medium, 0.2 M sodium formate, 0.1 M sodium-potassium phosphate, 10% glycerol, pH 6.2 |
| Ligand | CP-673451 | TAE-226 | Crenolanib |
| Data collection | |||
| X-ray source | DLS I24 | APS 24-ID-C | APS 24-ID-C |
| Wavelength (Å) | 0.9686 | 0.9791 | 0.9791 |
| Space group | P212121 | P43212 | P212121 |
| Cell dimensions | |||
|
a, b, c (Å) α, β, γ (°) |
49.0, 77.7, 78.1 90.0, 90.0, 90.0 |
73.7, 73.7, 123.9 90.0, 90.0, 90.0 |
49.1, 77.8, 78.7 90.0, 90.0, 90.0 |
| Resolution (Å)* | 19.78–1.90 (1.94–1.90) |
19.94–2.00 (2.05–2.00) |
19.89–1.95 (2.00–1.95) |
| No. of unique reflections* | 22,633 (1,224) | 22,752 (1,687) | 22,637 (1,565) |
| Rmerge (%)* | 5.80 (93.1) | 9.30 (100) | 4.80 (89.9) |
|
Mean I/σI * Mean CC(1/2)* |
13.1 (1.8) 1.0 (0.6) |
12.2 (2.1) 1.0 (0.7) |
18.9 (1.9) 1.0 (0.8) |
| Completeness (%)* | 93.6 (76.8) | 96.5 (98.5) | 99.8 (99.9) |
| Redundancy* | 5.2 (4.8) | 8.4 (8.6) | 6.4 (6.7) |
| Refinement | |||
| Resolution (Å) | 19.78–1.90 (1.95–1.90) | 19.94–2.00 (2.05–2.00) | 19.89–1.95 (2.00–1.95) |
| Rcryst/Rfree (%) | 18.6/22.7 | 18.7/22.5 | 18.9/22.7 |
| No. of atoms/Mean B-factor (Å) | |||
| Protein atoms | 2,076/40.4 | 2,167/39.2 | 2,023/41.2 |
| Solvent atoms | 90/44.0 | 112/42.9 | 100/45.1 |
| Ligand atoms | 37/33.4 | 47/41.1 | 37/35.8 |
| Rmsd bond lengths (Å) | 0.009 | 0.014 | 0.015 |
| Rmsd bong angles (degrees) | 1.33 | 1.60 | 1.64 |
| Ramachandran statistics (%) | |||
| Favored | 97.3 | 98.0 | 96.0 |
| Allowed | 2.7 | 2.0 | 4.0 |
| Outlier | 0 | 0 | 0 |
| PDB ID | 6BLE | 6BQL | 6BQP |
| Crystallization conditions | 28% PEG 3350, 0.07 M ammonium acetate, 0.1 M SBG buffer pH 5.5 | 24% PEG 3350, 0.14 M ammonium acetate, 0.1 M CHC buffer pH 7.5 | 22% PEG 3350, 0.21 M ammonium acetate, 0.1 M CHC buffer pH 7.0 |
*Numbers in parenthesis indicate statistics for the highest resolution shell.