Table 1.
Data and refinement statistics calculated for probe-only and pump–probe data.
| Analysis approach | Same resolution limits imposed | Automatically determined high-resolution limits | ||||
|---|---|---|---|---|---|---|
| Data set | Single-pulse | pump–probe | Single-pulse (all) | Single-pulse | pump–probe | Single-pulse (all) |
| # diffraction images used | 3500 | 3500 | 5500 | 3500 | 3500 | 5500 |
| Space group | P212121 | P212121 | P212121 | P212121 | P212121 | P212121 |
| Cell dimensions (Å, °) |
55.7 158.1 67.7 90.0 90.0 90.0 |
55.4 157.8 67.4 90.0 90.0 90.0 |
55.7 158.1 67.7 90.0 90.0 90.0 |
55.7 158.1 67.7 90.0 90.0 90.0 |
55.4 157.8 67.4 90.0 90.0 90.0 |
55.7 158.1 67.7 90.0 90.0 90.0 |
| # indexed | 3500 | 3500 | 5500 | 3500 | 3500 | 5500 |
| Resolution (Å) | 27.85–2.50 (2.57–2.50) | 27.42–2.50 (2.57–2.50) | 28.48–2.50 (2.57–2.50) | 28.48–2.53 (2.60–2.53) | 27.42–2.77 (2.77–2.84) | 28.48–2.54 (2.61–2.54) |
| I/σ(I) | 2.1 (1.0) | 2.0 (0.5) | 2.4 (1.2) | 2.1 (1.0) | 2.5 (1.0) | 2.4 (1.2) |
| Rsplit (%) | 48.3 (105.7) | 40.1 (235.3) | 40.0 (91.4) | 48.1 (100.3) | 36.9 (115.7) | 39.7 (89.6) |
| CC1/2 | 0.705 (0.172) | 0.857 (0.107) | 0.8 (0.294) | 0.702 (0.233) | 0.851 (0.307) | 0.798 (0.317) |
| CC* | 0.909 (0.542) | 0.961 (0.44) | 0.943 (0.674) | 0.908 (0.615) | 0.959 (0.686) | 0.942 (0.694) |
| Completeness (%) | 99.9 (99.7) | 99.8 (99.7) | 100.0 (99.9) | 99.9 (100.0) | 99.8 (99.7) | 100.0 (100.0) |
| Multiplicity | 18.2 (12.4) | 16.4 (11.0) | 28.1 (19.1) | 18.4 (12.3) | 18.3 (11.8) | 28.6 (18.9) |
| Wilson B (Å2) | 47.4 | 59.0 | 48.3 | 48.2 | 61.2 | 49.2 |
| Refinement | ||||||
| Unit cell parameters: a b c, α β γ (Å,°) | 55.7 158.1 67.7, 90.0 90.0 90.0 | |||||
| Images used | 3500 | 3500 | 5500 | |||
| Resolution (Å) | 28.48–2.53 | 27.42–2.77 | 28.48–2.54 | |||
| No. reflections | 19541 | 14810 | 19339 | |||
| Rwork/Rfree | 0.22757/0.28826 | 0.18841/0.27316 | 0.20701/0.27266 | |||
| No. atoms | ||||||
| Protein | 4332 | 4332 | 4332 | |||
| Ligands |
172 (4 haems) 8 (4 COs) |
172 (4 haems) 8 (4 COs) |
172 (4 haems) 8 (4 COs) |
|||
| Water | 38 | 38 | 38 | |||
| B-factors (Å2) | ||||||
| Chain A (haem A) | 42.1 (35.7) | 52.4 (47.1) | 41.3 (35.5) | |||
| Chain B (haem B) | 46.4 (41.6) | 57.8 (53.2) | 46.3 (42.4) | |||
| Chain C (haem C) | 50.3 (40.9) | 59.9 (53.4) | 49.5 (40.4) | |||
| Chain D (haem D) | 56.1 (45.5) | 68.5 (57.4) | 55.5 (45.2) | |||
| Water | 41.4 | 49.6 | 42.7 | |||
| R.m.s deviations | ||||||
| Bond lengths (Å) | 0.007 | 0.008 | 0.007 | |||
| Bond angles (°) | 1.490 | 1.608 | 1.549 | |||
| Percentage of residues in Ramachandran plot region | ||||||
| Preferred | 95.4 | 93.8 | 94.6 | |||
| Allowed | 4.1 | 5.5 | 4.7 | |||
| Disallowed | 0.5 | 0.7 | 0.7 | |||
| PDB code | 7AET | 7AEV | 7AEU | |||
Values are given for either applying the same or automatically determined resolution limits, respectively, for the probe-only and pump/probe data. The first/fourth columns show the statistics of the probe data, the second/fifth for the pump/probe data using the same number of images and the third/six column the statistics of the single-pulse data, using all images available. All diffraction images that passed the filtering set were included in this analysis, irrespective of the probe pulse energy. For the automatic resolution determination, each data set was divided into 20 resolution bins, and I/σ(I) was calculated for each bin. The resolution of the bin where this value was still >1.0 was taken as the high-resolution limit.