Table 2.
Data collection and refinement statistics
| GCase+IFG, pH 7.5 (C1) | GCase, pH 5.5 (C2) | GCase pH 4.5 (C3) | GCase pH 4.5 soaked (C4) | α-Gal A (L1) | α-Gal A + GAL (L2) | α-Gal A + DGJ (L3) | |
|---|---|---|---|---|---|---|---|
| Data collection | |||||||
| Space group | P21 | P21 | P21 | P21 | P3221 | P3221 | P3221 |
| Cell dimensions | |||||||
| a, b, c (Å) | 110.3, 92.0, 152.4 | 110.05, 91.7, 152.3 | 110.5, 91.8, 152.8 | 109.3, 91.7, 152.5 | 90.4, 90.4, 217.5 | 89.5, 89.5, 215.9 | 89.6, 89.6, 216.6 |
| α, β, γ (°) | 90. 111.2, 90 | 90, 111.1, 90 | 90, 111.2, 90 | 90, 111.0, 90 | 90, 90,120 | 90, 90,120 | 90, 90, 120 |
| Resolution (Å)* | 32.0−2.40 (2.49−2.40) | 141.4−1.85 (1.92−1.85) | 34−2.2 (2.28−2.20) | 142−2.3 (2.38−2.30) | 78.3−3.0 (3.11−3.0) | 77.6−2.2 (2.28−2.20) | 77.6−2.7 (2.85−2.70) |
| Rsym | 11.3(37.5) | 9.1(44.9) | 10.3(47.3) | 9.1(44.2) | 10.3(62.9) | 9.4(40.2) | 9.7(42.8) |
| I / σI | 8.7(2.1) | 23(2.5) | 9.8(2.2) | 21.8(2.1) | 15.3(1.9) | 17.7(2.6) | 6.4(1.8) |
| Completeness (%)+ | 93.2(79.8) | 93.5(76.0) | 96.4(91.2) | 80.8(58.9) | 88.7(66.0) | 81.9(42.7) | 97.7(98.7) |
| Redundancy | 3.1 | 5.4 | 2.5 | 6.0 | 6.3 | 6.3 | 2.4 |
| Refinement | |||||||
| Resolution (Å) | 32−2.4 | 141.4−1.8 | 20−2.2 | 42−2.5 | 78.3−3.0 | 77.6−2.2 | 77.6.2−2.7 |
| No. reflections | 98363 | 216309 | 131814 | 81268 | 17705 | 40251 | 26223 |
| Rwork / Rfree* | 17.8/24.5 | 19.0/23.1 | 22.0/27.6 | 20.4/27.5 | 23.6/30.0 | 21.3/26.9 | 23.7/30.3 |
| No. molecules | |||||||
| Protein residues | 1988 | 1988 | 1988 | 1988 | 780 | 781 | 781 |
| N-acetyl-glucosamine | 4 | 4 | 4 | 6 | 4 | 12 | 11 |
| (NAG) | |||||||
| Mannose (MNN) | 2 | 5 | |||||
| Sulfate anion (SO42--) | 28 | 1 | 4 | 5 | |||
| Phosphate anion (PO43−) | 64 | 63 | 50 | ||||
| Glycerol (GOL) | 5 | ||||||
| Chaperone | 2 (IFG) | 2 (DGJ) | |||||
| Tris | 1 | ||||||
| Galactose | 2 | ||||||
| Water | 923 | 1699 | 1181 | 222 | 162 | 73 | |
| B-factors | |||||||
| Protein | 26.2 | 26.1 | 24.6 | 49.2 | 121.0 | 71.1 | 63.4 |
| NAG | 34.8 | 33.7 | 30.9 | 62.3 | 139.6 | 93.0 | 80.8 |
| MNN | 199.9 | 88.5 | |||||
| SO42-- | 46.7 | 126.9 | 91.0 | ||||
| PO43− | 74.6 | 63.4 | 79.4 | ||||
| GOL | 43.9 | ||||||
| Chaperone | 28.2 | 58.5 | |||||
| Tris | 58.7 | ||||||
| Galactose | 55.6 | ||||||
| Water | 29.0 | 37.7 | 28.5 | 43.3 | 54.3 | 45.0 | |
| R.m.s deviations | |||||||
| Bond lengths (Å) | 0.02 | 0.017 | 0.016 | 0.016 | 0.018 | 0.020 | 0.016 |
| Bond angles (°) | 1.957 | 1.683 | 1.682 | 1.706 | 1.844 | 2.049 | 1.912 |
*
Highest resolution shell is shown in parenthesis. 5% of reflections were selected for Rfree.
+
GCase crystals are shaped as thin plates that diffract anisotropically along their thin edge, and resulting in incomplete data in the highest resolution bin. α-Gal A crystals are very radiation-sensitive rods, so some data were not collected in the highest resolution bin.