TABLE 1.
Data collection, processing, and refinement statistics
| Methylamine-reduced at pH 6.0 | Methylamine-reduced at pH 7.0 | Methylamine-reduced at pH 8.5 | |
|---|---|---|---|
| Data collection | |||
| Space group | P21 | P21 | C2221 |
| Unit cell parameters | |||
| a, b, c (Å) | 103.8, 222.8, 103.6 | 103.8, 222.8, 103.6 | 139.1, 153.3, 223.2 |
| α, β, γ | 90.0°, 95.9°, 90.0° | 90.0°, 95.8°, 90.0° | 90.0°, 90.0°, 90.0° |
| Resolution range (Å) | 50.0–1.70 (1.76–1.70) | 50.0–2.10 (2.14–2.10) | 50.0–2.15 (2.19–2.15) |
| Rmerge | 0.09 (0.59) | 0.10 (0.41) | 0.11 (0.56) |
| I/σI | 14.1 (1.7) | 12.3 (1.83) | 15.8 (3.19) |
| Completeness (%) | 99.7 (97.3) | 98.6 (89.4) | 100.0 (100.0) |
| Redundancy | 4.7 (3.3) | 3.6 (2.4) | 6.8 (6.5) |
| Refinement statistics | |||
| Resolution (Å) | 46.8-1.70 | 49.0-2.10 | 38.6-2.15 |
| No. of reflections (work/test) | 487,365/25,742 | 252,434/13,290 | 122,479/6492 |
| Rwork/Rfree | 13.4/16.4 | 12.9/18.0 | 15.1/19.1 |
| No. of atoms | |||
| Protein | 31,433 | 31,442 | 15,662 |
| Copper | 6 | 6 | 3 |
| Water | 4737 | 4380 | 1260 |
| All other | 335 | 337 | 83 |
| r.m.s.d.a | |||
| Bond lengths (Å) | 0.021 | 0.019 | 0.019 |
| Bond angles | 1.99° | 1.88° | 1.96° |
| Average B-factor (Å2) | 16.1 | 22.8 | 21.2 |
| Relative proportion of cofactor conformers for each protein chain in asymmetric unit (%) | Off-Cu, short cofactor N5/Asp-319 interaction:off-Cu, weak or H2O-mediated cofactor N5/Asp-319 interaction:on-Cu | ||
| A | 100:0:0 | 100:0:0 | 0:35:65 |
| B | 100:0:0 | 100:0:0 | 0:30:70 |
| C | 50:50:0 | 0:100:0 | 0:30:70 |
| D | 100:0:0 | 0:100:0 | NA |
| E | 100:0:0 | 0:100:0 | NA |
| F | 50:50:0 | 0:100:0 | NA |
| Protein Data Bank code | 4KFD | 4KFE | 4KFF |
a r.m.s.d., root mean square deviation; NA, not applicable.