Table 2. Data-collection and refinement statistics for IMISX samples.
All data-processing statistics are reported with Friedel pairs merged except for insulin-S and lyso-Br. Values in parentheses are for the highest resolution shell.
| Insulin-N | Insulin-N | Lyso-N | AlgE | PepTSt | β2AR | DgkA | Insulin-S | Lyso-Br | |
|---|---|---|---|---|---|---|---|---|---|
| PDB code | 5d52 | 5d53 | 5d5c | 5d5d | 5d58 | 5d5a | 5d56 | 5d5e | 5d5f |
| Crystal-growth temperature (K) | 293 | 293 | 293 | 293 | 293 | 293 | 277 | 293 | 293 |
| Data collection | |||||||||
| Temperature (K) | 293 | 100 | 100 | 100 | 100 | 100 | 100 | 100 | 100 |
| Phasing method | MR | MR | MR | MR | MR | MR | MR | S-SAD | Br-SAD |
| Space group | I213 | I213 | P43212 | P212121 | C2221 | C2 | P212121 | I213 | P43212 |
| Unit-cell parameters | |||||||||
| a, b, c (Å) | 79.71, 79.71, 79.71 | 78.36, 78.36, 78.36 | 77.70, 77.70, 38.94 | 46.33, 66.35, 176.84 | 100.16, 109.52, 111.47 | 108.04, 170.58, 40.44 | 75.61, 93.19, 142.74 | 78.20, 78.20, 78.20 | 78.28, 78.28, 38.12 |
| α, β, γ (°) | 90, 90, 90 | 90, 90, 90 | 90, 90, 90 | 90, 90, 90 | 90, 90, 90 | 90, 106.30, 90 | 90, 90, 90 | 90, 90, 90 | 90, 90, 90 |
| Unit-cell volume (Å3) | 506452 | 481153 | 235092 | 543605 | 1222773 | 745287 | 1005760 | 478212 | 233590 |
| Wavelength (Å) | 1.0 | 0.97857 | 1 | 0.97856 | 0.97852 | 1.0332 | 1 | 2.06643 | 0.91881 |
| ISa threshold | 5 | — | — | — | — | 5 | 3 | 3 | — |
| CCset cutoff | — | — | — | — | — | — | 0.9 | 0.9 | — |
| No. of crystals | 25 | 1 | 2 | 1 | 2 | 104 | 12 | 6 | 8 |
| Resolution (Å) | 50–1.80 (1.85–1.80) | 50–1.50 (1.54–1.50) | 50–1.70 (1.74–1.70) | 50–2.40 (2.46–2.40) | 50–2.40 (2.46–2.40) | 50–2.50 (2.57–2.50) | 50–2.80 (2.87–2.80) | 50–2.40 (2.46–2.40) | 50–1.50 (1.54–1.50) |
| R meas | 0.295 (2.354) | 0.123 (1.420) | 0.195 (1.650) | 0.162 (1.186) | 0.122 (0.999) | 0.203 (2.084) | 0.244 (2.982) | 0.118 (0.712) | 0.250 (2.233) |
| R p.i.m. † | 0.081 (0.652) | 0.049 (0.579) | 0.082 (0.692) | 0.086 (0.612) | 0.059 (0.487) | 0.085 (0.879) | 0.080 (1.012) | 0.030 (0.309) | 0.746 (0.688) |
| 〈I/σ(I)〉 | 6.96 (0.88) | 9.08 (1.21) | 6.16 (1.10) | 5.98 (1.45) | 9.31 (2.18) | 7.27 (1.11) | 4.42 (1.00) | 19.50 (2.00) | 6.39 (0.97) |
| Completeness (%) | 100 (100) | 99.9 (100) | 99.7 (100) | 92.6 (90.8) | 99.4 (98.8) | 95.1 (91.0) | 98.8 (98.6) | 99.9 (99.5) | 99.4 (92.0) |
| Multiplicity | 13.2 (13.0) | 6.4 (6.0) | 5.5 (5.7) | 3.6 (3.8) | 4.3 (4.2) | 5.7 (5.6) | 9.3 (8.7) | 16.0 (5.3) | 11.2 (10.5) |
| CC1/2 | 0.99 (0.46) | 0.99 (0.46) | 0.99 (0.32) | 0.99 (0.62) | 0.99 (0.62) | 0.99 (0.21) | 0.99 (0.36) | 0.998 (0.86) | 0.98 (0.38) |
| CCanom ‡ | — | — | — | — | — | — | — | 0.47 | 0.44 |
| Mosaicity§ (°) | 0.11 | 0.14 | 0.09 | 0.12 | 0.17 | 0.12 | 0.25 | 0.16 | 0.12 |
| Refinement | |||||||||
| Resolution (Å) | 39.85–1.80 | 38.76–1.50 | 39.55–1.70 | 25.22–2.40 | 45.68–2.40 | 43.96–2.50 | 46.52–2.80 | 27.70–2.41 | 35.06–1.50 |
| No. of reflections | 7975 | 13002 | 13594 | 20520 | 24159 | 23086 | 25188 | 6025 | 35932 |
| R work/R free | 0.17/0.21 | 0.16/0.17 | 0.18/0.22 | 0.22/0.26 | 0.21/0.25 | 0.21/0.26 | 0.24/0.28 | 0.17/0.22 | 0.18/0.21 |
| No. of atoms | |||||||||
| Protein | 414 | 814 | 1019 | 3222 | 3475 | 3546 | 4444 | 414 | 1019 |
| Ligand/ion | 10 | 37 | 21 | 233 | 502 | 210 | 260 | 21 | 19 |
| Water | 30 | 63 | 96 | 23 | 64 | 53 | 13 | 31 | 141 |
| B factors (Å2) | |||||||||
| Protein | 24.59 | 21.10 | 22.36 | 49.16 | 55.52 | 64.45 | 93.72 | 33.04 | 20.11 |
| Ligand/ion | 41.86 | 47.34 | 35.28 | 68.58 | 71.79 | 86.14 | 113.75 | 53.68 | 30.53 |
| Water | 36.05 | 31.63 | 27.14 | 46.03 | 53.43 | 61.90 | 89.98 | 41.49 | 27.79 |
| R.m.s. deviations | |||||||||
| Bond lengths (Å) | 0.012 | 0.009 | 0.008 | 0.010 | 0.005 | 0.006 | 0.004 | 0.002 | 0.007 |
| Bond angles (°) | 1.094 | 1.045 | 1.022 | 1.220 | 0.932 | 1.487 | 0.580 | 0.514 | 1.038 |
| Ramachandran plot | |||||||||
| Favoured (%) | 98.0 | 98.0 | 99.24 | 95.70 | 98.19 | 98.62 | 99.65 | 98.00 | 98.47 |
| Allowed (%) | 2.0 | 2.00 | 0.76 | 4.00 | 1.81 | 1.38 | 0.35 | 2.00 | 1.53 |
| Outliers (%) | 0 | 0 | 0 | 0.30 | 0 | 0 | 0 | 0 | 0 |
| MolProbity clashscore | 3.6 | 3.5 | 5.4 | 6.6 | 9.1 | 5.5 | 6.8 | 2.4 | 2.5 |
†
R p.i.m. was calculated as R meas/(multiplicity)1/2.
‡
Anomalous correlation coefficient evaluated with data truncated to 2.4 Å resolution for insulin-S and to 2.0 Å resolution for lyso-Br.
§
For IMISX data, mosaicity is reported as the median over all crystals.