Table 3.
Data collection and refinement statistics
Values for the highest-resolution shell are shown in parentheses. RMSD, root mean square deviation.
| Time/dose-resolved water-bound heme | Cyanide-bound heme | |||||||
|---|---|---|---|---|---|---|---|---|
| Beamline | I04 DLS | ID23-1 ESRF | ||||||
| Oscillation (degrees) | 0.1 | 0.1 | ||||||
| Exposure/image (s) | 0.04 | 0.1 | 0.1 | |||||
| Beam size (μm) | 26 × 15 | 20 × 20 | 20 × 20 | |||||
| Images/wedge | 100 | 100 | 3600 | |||||
| Wavelength (Å) | 0.9795 | 0.9919 | 0.9919 | |||||
| Flux (photon s−1) | 6.99 × 1010 | 1.89 × 1010 | 1.89 × 1010 | |||||
| Scaled wedges | 723 | 645 | 1 | |||||
| Image range from wedge | 1–4 | 5–8 | 17–20 | 35–38 | 71–74 | 96–99 | 1–5 | 1–3600 |
| Dose (kGy) | 2.15 | 4.3 | 10.8 | 20.4 | 40.3 | 53.6 | 2.3 | 1590.0 |
| Total exposed time (s) | 0.12 | 0.32 | 0.8 | 1.52 | 2.96 | 4 | 0.5 | 360 |
| Fe(II) % reduced | 5.2 | 10.5 | 26.4 | 50 | 98.7 | 100 | 5.7 | 100 |
| Space group | P 1 21 1 | P 1 21 1 | P 1 21 1 | |||||
| Unit cell (Å) | a = 50.89 | a = 50.89 | a = 50.57 | |||||
| b = 76.65 | b = 76.59 | b = 75.74 | ||||||
| c = 76.58 | c = 76.31 | c = 75.71 | ||||||
| Unit cell (degrees) | α = γ = 90.00 | α = γ = 90.00 | α = γ = 90.00 | |||||
| β = 108.01 | β = 107.87 | β = 107.85 | ||||||
| Resolution range (Å) | 48.40–1.90 | 48.40–1.90 | 48.40–1.90 | 47.67–1.90 | 47.67–1.90 | 47.67–1.90 | 36.31–1.80 | 36.03–1.52 |
| Rmerge | 0.18 (0.48) | 0.20 (0.54) | 0.20 (0.54) | 0.20 (0.57) | 0.20 (0.58) | 0.21 (0.60) | 0.21 (0.75) | 0.06 (0.85) |
| Rmeas | 0.22 (0.59) | 0.23 (0.64) | 0.24 (0.64) | 0.24 (0.68) | 0.24 (0.70) | 0.25 (0.74) | 0.25 (0.90) | 0.07 (0.10) |
| Rpim | 0.12 (0.33) | 0.12 (0.34) | 0.12 (0.34) | 0.12 (0.36) | 0.13 (0.37) | 0.14 (0.41) | 0.13 (0.49) | 0.04 (0.57) |
| All observations | 185,150 (11,453) | 238,147 (14,639) | 241,170 (14,925) | 241,538 (14,758) | 235,160 (14,352) | 202,833 (12,376) | 267,452 (15,345) | 246,785 (24,852) |
| Unique observations | 42,694 (2727) | 43,499 (2791) | 43,564 (2794) | 43,584 (2795) | 43,552 (2789) | 43,298 (2778) | 51,235 (3003) | 81,528 (8142) |
| Mean (I/σI) | 5.4 (3.0) | 6.2 (3.4) | 6.1 (3.4) | 6.2 (3.4) | 6.0 (3.3) | 5.5 (2.9) | 6.1 (2.7) | 3.0 (3.1) |
| CC½ | 0.96 (0.65) | 0.96 (0.37) | 0.96 (0.47) | 0.96 (0.39) | 0.95 (0.33) | 0.95 (0.41) | 0.97 (0.70) | 0.99 (0.50) |
| Completeness (%) | 96.8 (96.6) | 98.6 (98.8) | 98.7 (98.9) | 98.8 (98.9) | 98.7 (98.7) | 98.1 (98.3) | 99.2 (99.0) | 97.8 (97.4) |
| Multiplicity | 4.3 (4.2) | 5.5 (5.2) | 5.5 (5.3) | 5.5 (5.3) | 5.4 (5.1) | 4.7 (4.5) | 5.2 (5.1) | 3.0 (3.1) |
| Rwork (%) | 17.2 | 17 | 16.9 | 18.4 | 18.1 | 17.2 | 17.2 | 16.7 |
| Rfree (%) | 19.9 | 19.1 | 18.1 | 20.1 | 19.8 | 19 | 19.7 | 18.2 |
| Refined residues | 599 | 599 | 599 | 599 | 599 | 599 | 597 | 597 |
| Refined H2O | 671 | 634 | 655 | 644 | 621 | 669 | 785 | 560 |
| Average B-factor (Å2) | 12 | 12 | 12 | 12 | 12 | 12 | 10.34 | 26.26 |
| RMSD bond length (Å) | 0.023 | 0.022 | 0.024 | 0.018 | 0.017 | 0.015 | 0.013 | 0.015 |
| RMSD bond angle (degrees) | 1.54 | 1.52 | 1.59 | 1.42 | 1.36 | 1.24 | 1.15 | 1.66 |
| Ramachandran favored (%) | 98.15 | 97.98 | 97.64 | 98.15 | 97.98 | 97.82 | 98.65 | 98.48 |
| Rotamer outliers (%) | 0.6 | 1.18 | 1.19 | 0.8 | 1.01 | 0.4 | 1.38 | 1.2 |
| Molprobity overall (percentile) | 100 | 98 | 99 | 100 | 100 | 100 | 99 | 100 |
| PDB accession code | 6RQY | 6RR1 | 6RR4 | 6RR5 | 6RR6 | 6RR8 | 6RPE | 6RPD |