Table 2.
Diffraction data collection and processing.
| Diffraction source Wavelength (Å) Temperature (K) Detector |
Beamline 22-ID, SER-CAT, APS, ANL, IL, USA 1.000 100 Rayonix 300HS high speed CCD detector |
|||
|---|---|---|---|---|
|
| ||||
| BfL(LF) # | BfL(GalNAc) | BfL(Gb4) | BfL(BG-A) | |
| Crystal-to-detector dist. (mm) | 175 | 230 | 180 | 220 |
| Rotation range per image (°) | 0.25 | 0.25 | 0.5 | 0.5 |
| Total rotation range (°) | 125 | 125 | 360 | 200 |
| Exposure time per image (s) | 0.25 | 0.25 | 0.75 | 0.75 |
| Space group | P212121 | P212121 | P212121 | P21 |
| a, b, c (Å) | 45.99 58.00 190.6 | 45.89 58.95 187.3 | 44.68 88.23 110.8 | 78.83 44.82 65.77 |
| α, β, γ (°) | 90 90 90 | 90 90 90 | 90 90 90 | 90 100.05 90 |
| Mosaicity (°) | 0.19 | 0.87 | 0.25 | 0.39 |
| Resolution range (Å) | 50 - 1.43 (1.45 - 1.43)* | 50 - 1.71 (1.74 - 1.71) | 50 - 1.43 (1.45 - 1.43) | 50 - 1.65 (1.68 - 1.65) |
| Total No. of reflections | 426,074 | 232,093 | 1,022,165 | 178,921 |
| No. of unique reflections | 90,961 (3002) | 55,964 (2385) | 79,081 (2287) | 52,931 (2035) |
| Completeness (%) | 95.5 (63.9) | 99.0 (86.3) | 96.5 (56.3) | 96.9 (74.3) |
| Multiplicity | 4.7 (2.5) | 4.1 (2.4) | 12.9 (4.7) | 3.4 (2.2) |
| <I/σ(I)> | 23.2 (2.4) | 11.9 (3.1) | 36.8 (2.7) | 15.7 (2.4) |
| R merge † | 0.040 (0.443) | 0.111 (0.367) | 0.046 (0.436) | 0.0543 (0.300) |
| R p.i.m ‡ | 0.029 (0.327) | 0.053 (0.237) | 0.019 (0.213) | 0.039 (0.230) |
| Overall B, Wilson plot (Å2) | 14.4 | 13.0 | 11.0 | 10.6 |
| CC1/2& | 0.940 (0.759) | 0.938 (0.815) | 0.980 (0.862) | 0.964 (0.885) |
|
| ||||
| BfL(Tn-168) | BfL(Tn-168) | BfL(Tn-207) | BfL(Tn-200) | |
|
| ||||
| Crystal-to-detector dist. (mm) | 128 | 160 | 220 | 260 |
| Rotation range per image (°) | 0.25 | 1.0 | 0.5 | 0. 5 |
| Total rotation range (°) | 180 | 400 | 180 | 250 |
| Exposure time per image (s) | 0.25 | 1.05 | 0.5 | 0.5 |
| Space group | P212121 | P21 | P212121 | P212121 |
| a, b, c (Å) | 44.86 88.50 110.8 | 54.38 46.16 92.11 | 44.69 88.46 111. | 65.08 187.3 258.4 |
| α, β, γ (°) | 90 90 90 | 90 92.56 90 | 90 90 90 | 90 90 90 |
| Mosaicity (°) | 0.38 | 0.56 | 0.80 | 0.44 |
| Resolution range (Å) | 50 - 1.17 (1.19 - 1.17) | 40 - 1.35 (1.37 - 1.35) | 50 - 1.66 (1.69 - 1.66) | 50 - 2.70 (2.80 - 2.70) |
| Total No. of reflections | 1,008,306 | 793,282 | 366,225 | 489,032 |
| No. of unique reflections | 147,131 (5701) | 100,009 (4951) | 52,813 (2432) | 85,387 (3781) |
| Completeness (%) | 98.5 (77.1) | 99.9 (99.6) | 99.7 (94.2) | 98.4 (88.8) |
| Multiplicity | 6.9 (4.2) | 7.9 (5.7) | 6.9 (4.0) | 5.7 (5.2) |
| <I/σ(I)> | 17.3 (2.9) | 27.6 (2.4) | 28.5 (2.0) | 14.5 (1.8) |
| R merge † | 0.038 (0.426) | 0.066 (0.751) | 0.051 (0.568) | 0.075 (0.660) |
| R p.i.m ‡ | 0.032 (0.237) | 0.027 (0.322) | 0.026 (0.292) | 0.050 (0.397) |
| Overall B, Wilson plot (Å2) | 13.6 | 14.4 | 14.2 | 32.3 |
| CC1/2& | 0.966 (0.810) | 0.961 (0.761) | 0.962 (0.741) | 0.966 (0.814) |
#
BfL(LF) refers to the ‘ligand-free’ structure of BfL.
*
Values in parentheses are for the highest resolution shell.
†
Rmerge = Σ(|(I − <I>)| / Σ(I).
‡
Estimated Rp.i.m. = Rmerge[N/(N−1)]1/2, where N is the multiplicity of data.
&
CC1/2 = Σ(x − <x>)(y − <y>) / [Σ(x − <x>)2 Σ (y − <y>)2]1/2.
#
For more extensive definitions of these indicators see http://shelx.uni-ac.gwdg.de/~athorn/pdf/thorn_cshl2014_quality_indicators.pdf and the references cited therein.