Table 1.
Data collection, phasing and refinement statistics
| Norrin–Fz4CRD–SOS | Methylated Norrin–Fz4CRD | Norrin | Norrin Se-Met | Methylated Norrin | |
|---|---|---|---|---|---|
| Crystal form | I | I | II | ||
| Data collection | |||||
| Space group | P6122 | P4322 | P212121 | P212121 | P212121 |
| Cell dimensions | |||||
| a, b, c (Å) | 119.1, 119.1, 119.2 | 98.9, 98.9, 120.4 | 46.4, 79.1, 243.3 | 45.8, 78.8, 232.8 | 102.7, 53.1, 96.1 |
| α, β, γ (°) | 90, 90, 90 | 90, 90, 120 | 90, 90, 90 | 90, 90, 90 | 90, 90, 90 |
| Peak | |||||
| Wavelength | 0.9200 | 0.9795 | 0.9686 | 0.9795 | 0.9795 |
| Resolution (Å) | 47.34–3.00 (3.18– 3.00) | 49.46–2.30 (2.38–2.30) | 65.56–2.40 (2.49–2.40) | 116.39–3.18 (3.26–3.18) | 33.65–2.00 (2.05–2.00) |
| Rpim (%) | 3.1 (54.8) | 4.5 (56.1) | 6.1 (42.3) | 2.8 (23.4) | 4.1 (58.3) |
| I/σI | 14.6 (1.6) | 10.7 (1.4) | 7.8 (1.9) | 20.2 (3.0) | 9.1 (1.7) |
| Completeness (%) | 100 (100) | 98.9 (97.2) | 99.9 (100) | 99.9 (99.9) | 100 (100) |
| Redundancy | 19.6 (20.6) | 6.0 (5.6) | 5.6 (5.7) | 33.3 (9.9) | 5.6 (5.8) |
| Refinement | |||||
| Resolution (Å) | 47.34–3.00 (3.18–3.00) | 49.46–2.30 (2.38–2.30) | 65.56–2.40 (2.49–2.40) | 33.65–2.00 (2.05–2.00) | |
| No. reflections | 10,503 (1648) | 26,816 (2514) | 34,722 (3384) | 36,272 (2635) | |
| Rwork/Rfree | 21.5/26.7 | 19.7/22.1 | 21.6/26.2 | 23.3/24.8 | |
| No. atoms | |||||
| Protein | 1759 | 2557 | 4930 | 3187 | |
| Ligand/ion | 83 | 39 | 101 | 10 | |
| Water | 0 | 115 | 164 | 122 | |
| B-factors | |||||
| Protein | 113 | 63 | 70 | 57 | |
| Ligand/ion | 133 | 71 | 92 | 73 | |
| Water | 0 | 57 | 55 | 51 | |
| R.m.s deviations | |||||
| Bond lengths (Å) | 0.005 | 0.004 | 0.009 | 0.005 | |
| Bond angles (°) | 1.18 | 0.93 | 1.08 | 1.07 | |
| Ramachandran plot | |||||
| Favored (%) | 95.5 | 97.0 | 96.7 | 97.2 | |
| Allowed (%) | 4.5 | 3.0 | 3.3 | 2.8 | |
| PDB code | 5BQC | 5BQE | 5BPU | 5BQ8 | |
| Norrin | Fz4CRD | Fz4CRD | |
|---|---|---|---|
| Crystal form | III | I | II |
| Data collection | |||
| Space group | C121 | P212121 | P61 |
| Cell dimensions | |||
| a, b, c (Å) | 86.8, 38.1, 177.2 | 72.6, 102.1, 116.5 | 76.1, 76.1, 204.5 |
| α, β, γ (°) | 90, 94, 90 | 90, 90, 90 | 90, 90, 90 |
| Wavelength | 0.9795 | 0.9686 | 0.9686 |
| Resolution (Å) | 44.19–2.30 (2.38–2.30) | 41.77–2.20 (2.27–2.20) | 47.37–2.40 (2.49–2.40) |
| Rpim (%) | 2.8 (36) | 4.1 (49.5) | 2.6 (33.9) |
| I/σI | 16.7 (2.0) | 12.8 (2.0) | 14.5 (2.2) |
| Completeness (%) | 99.2 (97.7) | 99.2 (99.7) | 99.5 (99.4) |
| Redundancy | 5.8 (6.0) | 4.3 (4.4) | 4.0 (4.1) |
| Refinement | |||
| Resolution (Å) | 44.19–2.30 (2.38–2.30) | 41.77–2.20 (2.27–2.20) | 47.37–2.40 (2.49–2.40) |
| No. reflections | 26,073 (2538) | 44,268 (3802) | 25,975 (2724) |
| Rwork/Rfree | 22.1/25.0 | 17.7/22.3 | 20.3/24.3 |
| No. atoms | |||
| Protein | 3104 | 3866 | 3877 |
| Ligand/ion | 72 | 70 | 99 |
| Water | 54 | 148 | 69 |
| B-factors | |||
| Protein | 91 | 47 | 76 |
| Ligand/ion | 72 | 67 | 72 |
| Water | 142 | 43 | 68 |
| R.m.s deviations | |||
| Bond lengths (Å) | 0.006 | 0.01 | 0.005 |
| Bond angles (°) | 1.03 | 1.35 | 0.94 |
| Ramachandran plot | |||
| Favored (%) | 96.0 | 99.0 | 97.0 |
| Allowed (%) | 4.0 | 1.0 | 3.0 |
| PDB code | 5BQB | 5BPB | 5BPQ |
All structures were determined from one crystal.
Values in parentheses are for highest-resolution shell.