Table 1.
Crystallography data collection and refinement statistics
| Protein |
|||||
|---|---|---|---|---|---|
| ACER3-cryo | ADIPOR2-cryo | ADIPOR2-RT | ADIPOR2-Tb-XO4 | ADIPOR2-Gd-DO3 | |
| PDB ID | 6YXH | 6YX9 | 6YXD | 6YXG | 6YXF |
| Data collection | |||||
| Photon energy (keV) | 12.4 | 12.4 | 12.4 | 7.5 | 7.2 |
| Beam size (μm2) | 20 × 10 | 20 × 10 | 10 × 5 | 20 × 10 | 20 × 10 |
| Synchrotron | Swiss Light Source | Swiss Light Source | P14–PETRA III, DESY | Swiss Light Source | Swiss Light Source |
| Detector | EIGER-16M | EIGER-16M | EIGER-16M (4M ROI) | EIGER-16M | EIGER-16M |
| Photon flux (ph/s) | 6.1 × 1011 | 6.1 × 1011 | 1.17 × 1013 | 6.1 × 1011 | 6.1 × 1011 |
| Exposure time (ms)/frame | 100 | 100 | 1.3 | 100 | 100 |
| Oscillation range/crystal | 10° | 10° | 0.6° | 10° | 10° |
| Collection strategy | 10° wedge/crystal | 10° wedge/crystal | helical line scan on each drop; ∼400 lines; 2- and 10-μm vertical and horizontal steps, respectively | 10° wedge/crystal | 10° wedge/crystal |
| Total no. of frames | NA | NA | 382,552 | NA | NA |
| No. of hits (datasets collected) | 21,250 (425) | 15,750 (315) | 28,949 | 28,500 (570) | 20,500 (410) |
| No. of indexed framesa | 18,550 (371) | 5,200 (104) | 25,297 | 23,350 (467) | 17,800 (356) |
| No. of datasets merged | 101 | 100 | N/A | 210 | 96 |
| No. of CD boluses | 9 | 1 | 5 | 16 | 7 |
| No. of crystals/bolus | ∼17 | ∼33 | ∼100 | ∼27 | ∼22 |
| Effective collection timeb (min) | 8.4 (30.9) | 8.3 (26.2) | 20 (76) | 38.9 (47.5) | 29.6 (35) |
| Protein consumption (μL) | 1.6 | 0.3 | 1.5 | 4.8 | 2.1 |
| Crystal size (μm3, approx.) | 20 × 10 × 5 | 30 × 20 × 5 | 30 × 20 × 5 | 30 × 20 × 5 | 30 × 20 × 5 |
| Space group | C2221 | P21221 | P21221 | P21221 | P21221 |
| Unit cell: a, b, c (Å) | 61.5, 69.9, 259.5 | 74.7, 100.6, 109.7 | 75.4, 100.8, 114.9 | 74.6, 100.7, 110.5 | 74.6, 100.6, 111.2 |
| Structure refinement | |||||
| Resolution rangec (Å) | 46.2–2.6 (2.62–2.6) | 22–2.4 (2.49–2.40) | 50–2.9 (2.98–2.9) | 48.0–3.0 (3.1–3.0) | 48.7–3.0 (3.1–3.0) |
| No. of unique reflectionsa | 17,701 (1,275) | 30,556 (2,326) | 15,292 (1,971) | 32,012 (2,150) | 31,468 (2,336) |
| Multiplicitya | 36.01 (35.28) | 37.12 (33.69) | 130.57 (4.24) | 34.82 (13.14) | 14.98 (6.18) |
| CC1/2a | 0.99 (0.330) | 0.99 (0.561) | 0.98 (0.737) | 0.99 (0.3) | 0.98 (0.3) |
| I/σ(I)a | 8.4 (0.98) | 8.3 (1.02) | 8.6 (1.4) | 7.33 (1.5) | 5.06 (1.1) |
| Completeness (%)a | 100 (100) | 99.4 (100) | 100 (75.7) | 99.9 (100) | 98.8 (99.7) |
| Wilson B factor (Å2) | 65.9 | 60.7 | 42.3 | 79.1 | 78.9 |
| R-work/R-free (%)a | 23.2 (32.2)/28.0 (34.9) | 20.7 (38.0)/24.8 (40.6) | 19.9 (23.4)/25.3 (39.3) | 21.5 (34.6)/25.2 (50.3) | 21.4 (30.6)/25.9 (40.8) |
| Clashscore | 9.2 | 8.1 | 6.4 | 10.9 | 11.1 |
| RMS bond (Å) | 0.01 | 0.005 | 0.003 | 0.01 | 0.01 |
| RMS angle (°) | 1.06 | 0.710 | 0.659 | 1.10 | 1.15 |
| Ramachandran favored/outlier (%) | 93.97/1.44 | 98.22/0.0 | 98.02/0.0 | 93.76/0.97 | 92.48/0.99 |
| Average B factor (Å2) | |||||
| Macromolecule | 77.0 | 79.7 | 47.8 | 79.5 | 78.8 |
| Ligand | – | 100.3 | 68.5 | 91.5 | 90.5 |
| Solvent | 65.6 | 72.5 | 57.4 | 79.3 | 82.8 |
| Metal ions | Zn2+: 99.0 | Zn2+: 72.0 | Zn2+: 33.0 | Zn2+: 66.0 | Zn2+: 62.0 |
| Ca2+:116.0 | |||||
| Na+: 84.0 | |||||
| Mg2+: 71.5 | |||||
| SO42–: 123.1 | |||||
a
Values in parenthesis represent number of 10˚ wedges used.
b
Values in parenthesis indicate total time in minutes, which includes the screening of many CrystalDirect pins or drops in plate-containing microcrystals.
c
Values in parentheses represent high-resolution shells.