TABLE 1.
Crystallographic statistics
Values in parentheses are for the high resolution shell.
| Crystal data | Xyn30D | Xyn30D-CBM35 | Xyn30D-CBM35/GlcA | Xyn30D-CBM35/GlcA-Xyl |
|---|---|---|---|---|
| Space group | P32 | P212121 | P212121 | P212121 |
| Unit cell parameters | ||||
| a (Å) | 174.0 | 39.4 | 39.9 | 39.8 |
| b (Å) | 174.0 | 47.4 | 47.5 | 47.3 |
| c (Å) | 183.9 | 103.0 | 102.7 | 103.0 |
| Data collection | ||||
| Beamline | ID23–2 (ESRF) | Rotating anode | P13 (PETRA III/DESY) | I03 (Diamond) |
| Temperature (K) | 100 | 100 | 100 | 100 |
| Wavelength (Å) | 0.8726 | 1.5418 | 0.9786 | 0.9762 |
| Resolution (Å) | 40.76-2.40 (2.53-2.40) | 51.51-2.18 (2.30-2.18) | 102.74-1.50 (1.58-1.50) | 34.86-1.35 (1.42-1.35) |
| Data processing | ||||
| Total reflections | 1,435,305 (209,187) | 123,458 (14,761) | 414,192 (60,119) | 502,825 (73,033) |
| Unique reflections | 125,591 (18,229) | 10,371 (1,270) | 32,026 (4,619) | 43,659 (6256) |
| Multiplicity | 11.4 (11.5) | 11.9 (11.6) | 12.9 (13.0) | 11.5 (11.7) |
| Completeness (%) | 100.0 (100.0) | 97.5 (83.8) | 99.6 (100) | 100 (100) |
| I/σ (I) | 4.8 (1.4) | 8.8 (4.2) | 4.4 (1.5) | 4.6 (1.5) |
| Mean I/σ (I) | 14.7 (4.6) | 25.7 (12.9) | 16.0 (5.1) | 17.3 (6.6) |
| Rmerge (%)a | 14.3 (57.7) | 6.8 (16.9) | 9.7 (51.0) | 8.4 (42.7) |
| Rpim (%)b | 4.4 (17.8) | 2.0 (5.1) | 2.8 (14.6) | 2.6 (13.0) |
| Molecules per ASU | 8 | 1 | 1 | 1 |
| Refinement | ||||
| Rwork/Rfree (%)c | 17.9/20.4 | 20.9/26.9 | 15.7/16.7 | 16.4/17.5 |
| No. of atoms/average B (Å2) | ||||
| Protein | 33,155/23.4 | 976/17.2 | 1,060/15.4 | 1,149/11.3 |
| Carbohydrate | 0 | 6/17.8 | 26/15.3 | 21/24.4 |
| Calcium ions | 16/36.1 | 2/15.4 | 2/11.9 | 2/8.3 |
| Water molecules | 95/14.9 | 56/20.5 | 121/24.4 | 116/22.1 |
| Ramachandran plot (%) | ||||
| Favored | 96 | 98 | 98 | 99 |
| Outliers | 0.5 | 0 | 0 | 0 |
| RMS deviations | ||||
| Bonds (Å) | 0.0073 | 0.0091 | 0.0149 | 0.0138 |
| Angles (°) | 1.2439 | 1.2904 | 1.4939 | 1.5773 |
| PDB accession codes | 4QAW | 4QB1 | 4QB2 | 4QB6 |
a Rmerge = Σhkl Σi |Ii(hkl) − [I(hkl)]|/Σhkl Σi Ii(hkl), where Ii(hkl) is the ith measurement of reflection hkl and [I(hkl)] is the weighted mean of all measurements.
b Rpim = Σhkl [1/(N − 1)]1/2 Σi|Ii(hkl) − [I(hkl)]|/Σhkl Σi Ii(hkl), where N is the redundancy for the hkl reflection.
c Rwork/Rfree = Σhkl|Fo − Fc|/Σhkl|Fo|, where Fc is the calculated and Fo is the observed structure factor amplitude of reflection hkl for the working/free (5%) set, respectively.