Table 1. Data collection and refinement statistics.
| T-state α(Fe-CO) hybrid Hb
|
T-state β(Fe-CO) hybrid Hb
|
||||||
|---|---|---|---|---|---|---|---|
| Bound state | Photo-product | Difference map* | Bound state | Photo-product | Difference map* | R-state HbCO difference map* | |
| Data collection | |||||||
| Light | None | Laser, red | None (laser, red) | None | Laser, red | None (laser, red) | None (multiple beams) |
| Temperature, K | 100 | 25 | 25 (25) | 100 | 25 | 25 (25) | 25 (35) |
| Resolution range, Å | 20-1.60 | 20.0-1.55 | 20.0-1.70 (20.0-1.70) | 20.0-1.45 | 20.0-1.45 | 20.0-1.75 (20.0-1.75) | 20.0-2.50 (20.0-2.50) |
| Reflections | |||||||
| Measured | 437,187 | 600,432 | 403,926 (387,426) | 751,479 | 878,993 | 385,971 (381,959) | 50,436 (51,059) |
| Unique | 144,674 | 153,793 | 120,229 (119,562) | 200,565 | 197,252 | 110,529 (111,952) | 9,387 (9,363) |
| Completeness, %† | 94.4/83.9 | 90.7/51.8 | 94.4/82.0 (93.7/78.2) | 95.9/77.3 | 95.9/70.4 | 93.8/63.9 (94.7/66.3) | 97.1/87.5 (96.7/86.5) |
| Mean <I>/<σ(I)> | 26.0 | 5.8 | 7.2 (7.2) | 8.1 | 7.9 | 5.8 (6.2) | 7.0 (7.2) |
| Multiplicity | 3.0 | 3.9 | 3.4 (3.2) | 3.7 | 4.5 | 3.5 (3.4) | 5.4 (5.5) |
| Rmerge‡, %† | 3.5/9.6 | 6.0/27.6 | 5.6/22.6 (5.9/22.5) | 6.7/21.3 | 5.7/20.4 | 6.5/19.7 (6.3/19.0) | 5.9/29.8 (5.6/27.8) |
| Refinement statistics | |||||||
| Resolution range, Å | 20.0-1.60 | 20.0-1.55 | 20.0-1.45 | 20.0-1.45 | |||
| σcut-off | 0.0 | 0.0 | 0.0 | 0.0 | |||
| Reflections used | 144,674 | 153,793 | 200,565 | 197,252 | |||
| R-factor§, % | 17.4 | 18.4 | 19.1 | 18.7 | |||
| Free R-factor, % | 20.4 | 21.3 | 21.1 | 20.8 | |||
| Solvent | 715 | 937 | 929 | 969 | |||
| rms deviations from ideals | |||||||
| Bond lengths, Å | 0.012 | 0.013 | 0.010 | 0.009 | |||
| Bond angles, o | 1.312 | 1.480 | 1.310 | 1.350 | |||
To increase the signal-to-noise ratio of difference Fourier maps, both of the datasets on the photoproduct and the bound state were collected from the same crystal.
Completeness and Rmerge are given for overall data and for the highest-resolution shell (overall/the highest-resolution shell). The highest-resolution shells for the most leftward column to the right are 1.66-1.60 Å, 1.61-1.55 Å, 1.76-1.70 Å, 1.50-1.45 Å, 1.50-1.45 Å, 1.81-1.75 Å, and 2.59-2.50 Å, respectively.
Rmerge = Σ|Ii — 〈I〉|/Σ|Ii|; where Ii is the intensity of an observation and 〈I〉 is the mean value for that reflection and the summations are over all reflections.
R-factor = Σh∥Fo(h)| — |Fc(h)∥ /ΣhFo(h), where Fo and Fc are the observed and calculated structure factor amplitudes, respectively. The free R-factor was calculated with 5% of the data excluded from the refinement.