Table 1. Processing and refinement statistics for the first and last thaumatin data set at each temperature.
All samples initially diffracted beyond the resolution limit of our experimental geometry (1.52 Å). As the samples became damaged the resolution dropped and scaling was truncated so that 〈I〉/〈σ(I)〉 = 2 in the highest resolution bin (of a total of ten bins). R merge, intensity statistics, mosaicity and unit-cell parameters were determined with DENZO/SCALEPACK (Otwinowski & Minor, 1997 ▶). R values and atomic B factors were determined with BUSTER-TNT (Blanc et al., 2004 ▶). Data sets at intermediate doses exhibited statistics that interpolated between those of the first and last data sets within error.
25 K | 100 K | 180 K | 240 K | 300 K | ||||||
---|---|---|---|---|---|---|---|---|---|---|
Data set | First | Last | First | Last | First | Last | First | Last | First | Last |
PDB code | 4ek0 | 4eka | 4ekb | 4ekh | 4eko | 4ekt | 4el2 | 4el3 | 4el7 | 4ela |
Resolution (Å) | 1.52 | 1.55 | 1.52 | 1.75 | 1.52 | 1.75 | 1.52 | 1.95 | 1.52 | 2.00 |
Unit-cell parameters (Å) | ||||||||||
a = b | 57.130 | 57.350 | 57.390 | 57.510 | 57.770 | 57.900 | 58.270 | 58.320 | 58.370 | 58.330 |
c | 150.30 | 150.78 | 149.74 | 149.90 | 149.94 | 150.07 | 150.72 | 150.75 | 151.27 | 151.30 |
〈I〉 | 3092.1 | 2074.8 | 1909.7 | 1232.8 | 657.4 | 409.0 | 373.2 | 131.6 | 254.7 | 106.6 |
〈I〉/〈σ(I)〉 | 37.66 | 31.67 | 33.68 | 27.09 | 26.29 | 21.87 | 22.89 | 13.70 | 20.37 | 12.84 |
Reflections | 38888 | 37321 | 39378 | 26246 | 39290 | 26034 | 38012 | 18682 | 35453 | 17277 |
R merge (%) | 8.4 | 8.8 | 8.5 | 11 | 7.5 | 8.8 | 7.8 | 9.9 | 8.2 | 13 |
Wilson B (Å2) | 15.39 | 22.39 | 16.67 | 24.93 | 16.00 | 23.20 | 18.44 | 25.29 | 18.34 | 26.93 |
Mean B (Å2) | 19.16 | 26.04 | 20.22 | 27.53 | 19.17 | 26.39 | 23.28 | 29.94 | 24.06 | 31.95 |
R/R free (%) | 18.4/20.1 | 19.1/20.0 | 17.5/19.3 | 18.1/21.1 | 17.0/18.8 | 17.5/20.1 | 16.2/19.2 | 16.2/20.2 | 16.3/18.0 | 16.3/19.2 |
Mosaicity (°) | 0.232 | 0.442 | 0.194 | 0.433 | 0.190 | 0.269 | 0.057 | 0.147 | 0.041 | 0.163 |