Table 1.
Data Collection and Refinement Statistics.
| Enzyme Structure | Mn2+2-TcFIGase (pH 8.0) | Mn2+2-N114H TcFIGase (pH 7.5) | Apo-TcFIGaseox (pH 4.6) | Mn2+2-TcFIGaseox (pH 6.0) | Mn2+2-TcFIGaseox (pH 8.5) |
|---|---|---|---|---|---|
| A. Data Collection | |||||
| Wavelength (Å) | 1.5418 | 1.075 | 1.075 | 1.5418 | 1.5418 |
| Resolution limits (Å) | 50.0–1.85 | 50.0–1.80 | 50.0–1.53 | 50.0–1.80 | 50.0–1.52 |
| No. total/unique reflections | 108650/44906 | 156011/24658 | 187951/40029 | 77546/24341 | 144418/40463 |
| Space group | H3 | H3 | H3 | H3 | H3 |
| a, b, c (Å) | 128.9, 128.9, 85.4 | 129.4, 129.4, 42.5 | 129.4, 129.4, 42.6 | 129.5, 129.5, 42.7 | 129.7, 129.7, 42.5 |
| α, β, r (deg) | 90, 90, 120 | 90, 90, 120 | 90, 90,120 | 90, 90, 120 | 90, 90, 120 |
| Completenessa (%) | 99.2 (98.8) | 100 (100) | 99.9 (100) | 98.2 (97.3) | 98.4 (95.1) |
| I/σIa | 14.2 (2.0) | 19.0 (2.9) | 17.3 (2.7) | 10.0 (2.3) | 14.4 (2.7) |
| Rsyma,b | 0.059 (0.438) | 0.088 (0.754) | 0.077 (0.527) | 0.117 (0.466) | 0.077 (0.422) |
| Redundancya | 2.5 (2.4) | 6.3 (6.1) | 4.7 (4.5) | 3.2 (3.1) | 3.6 (3.2) |
| B. Refinement | |||||
| No. of reflections used in refinement/test set | 42190 (2123) | 23858/1211 | 39028/1994 | 23603/1207 | 39990/2050 |
| Rwork/Rfree(%)a,c | 18.7/21.7 (24.0/30.8) | 18.8/22.1 (24.6/28.2) | 13.4/16.1 (22.6/25.5) | 17.1/21.0 (21.7/25.6) | 14.6/16.2 (40.0/46.1) |
| Twining fraction | 0 | 0 | 0.25 | 0 | 0.42 |
| Twin law | N/A | N/A | h, -h-k, -l | N/A | h, -h-k, -l |
| No. of atomsd | |||||
| protein | 4571 | 2288 | 2231 | 2235 | 2212 |
| solvent | 265 | 93 | 160 | 178 | 122 |
| Mn2+ | 4 | 2 | 0 | 2 | 2 |
| glycerol | 6 | 0 | 0 | 0 | 0 |
| Root-mean-square deviation | |||||
| bonds (Å) | 0.006 | 0.009 | 0.008 | 0.008 | 0.008 |
| angles (deg) | 0.9 | 1.1 | 1.1 | 1.1 | 1.2 |
| Average B factor (Å2) | |||||
| main chain | 27 | 35 | 16 | 24 | 21 |
| side chain | 29 | 37 | 20 | 27 | 23 |
| solvent | 32 | 38 | 24 | 30 | 24 |
| metal ions | 26 | 29 | N/A | 23 | 19 |
| Ramachandran plot (%) | |||||
| allowed | 91.1% | 89.8% | 91.4% | 90.7% | 90.2% |
| additionally allowed | 8.9% | 10.2% | 8.2% | 9.3% | 9.3% |
| generously allowed | 0.0% | 0.0% | 0.4% | 0.0% | 0.4% |
| disallowed | 0.0% | 0.0% | 0.0% | 0.0% | 0.0% |
a
Values in parentheses refer to the highest resolution shell.
b
Rsym = ΣhΣi|I(h)i – <I(h)>|/ΣhΣiI(h)i, where I(h) is the intensity of reflection h, Σh is the sum over all reflections and Σi is the sum over i measurements of reflection h.
c
Rwork = Σ||Fo| – |Fc||/Σ|Fo| for reflections contained in the working set. Rfree = Σ||Fo| – |Fc||/Σ|Fo| for reflections contained in the test set held aside during refinement (5% of total). |Fo| and |Fc| are the observed and calculated structure factor amplitudes, respectively.
d
Per asymmetric unit.