Table 1.
Data processing and refinement statistics for the orthorhombic and monoclinic insulin crystallized in presence of urea and thiocyanate respectively.
| Data sets | ||||
| Urea containing crystals | Na-SCN containing crystals | |||
| C2221urea | C2urea | C2221scn | C2scn | |
| Data processing | ||||
| Values in parenthesis are for the highest resolution shell | ||||
| Wavelength (Å) | 1.0 | 1.1 | 1.3 | 1.3 |
| Cell axis a, b, c (Å) | 58.9, 219.3, 223.7 | 100.2, 60.2, 62.9 | 59.0, 219.5, 224.5 | 100.6, 60.8, 62.1 |
| Cell angles α β γ (deg) | 90.0 90.0 90.0 | 90.0 116.2 90.0 | 90.0 90.0 90.0 | 90.0 116.1 90.0 |
| Temperature (K) | 100 | 100 | 100 | 100 |
| Diffraction limit (Å) | 2.05 | 1.70 | 1.97 | 1.70 |
| Highest resolution shell (Å) | 2.1 – 2.05 | 1.75 – 1.70 | 2.0 – 1.97 | 1.75 – 1.704 |
| No. of observations | 450 276 (23593) | 72 333 (3616) | 885 954 (9682) | 143 773 (4037) |
| Unique reflections | 91 251 (6331) | 34 195 (1952) | 102 732 (3997) | 34 924 (1890) |
| Redundancy | 4.9 (3.7) | 2.1 (1.8) | 8.6 (2.4) | 4.1 (2.1) |
| Rmergea (%) | 8.6 (39.3) | 3.4 (16.9) | 9.0 (37.3) | 4.3 (13.3) |
| I/σ (I) | 11.6 (3.2) | 13.7 (4.1) | 17.7 (2.4) | 21.6 (6.5) |
| Refinement statistics | ||||
| Values in parenthesis are for the highest resolution shell | ||||
| Resolution range (Å) | 28.31 – 2.05 | 19.57 – 1.70 | 19.99 – 1.97 | 19.78 – 1.70 |
| Highest resolution shell (Å) | 2.10 – 2.05 | 1.74 – 1.70 | 2.02 – 1.97 | 1.75 – 1.704 |
| No. of reflections | 86 749 (6376) | 32 471 (1621) | 97 508 (6629) | 33 178 (1700) |
| Completeness | 99.9 (100) | 92.3 (62.5) | 99.5 (93.1) | 94.8 (67.5) |
| R value (%) b | 18.4 (21.3) | 18.5 (22.9) | 17.5 (21.7) | 17.8 (25.5) |
| Rfree value (%) b | 22.7 (28.8) | 22.3 (33.4) | 21.1 (25.4) | 22.1 (33.1) |
| r.m.s.d.c | ||||
| Bond length (Å) | 0.016 | 0.012 | 0.014 | 0.011 |
| Bond angles (deg) | 1.6 | 1.3 | 1.4 | 1.3 |
| B factors (Å 2) d | ||||
| Average all atoms | 32.2 | 27.2 | 33.8 | 20.9 |
| All PheB1 | 40.1 (18) | 27.4 (6) | 42.4 (18) | 18.7 (6) |
| α-helical PheB1 | 42.0 (7) | 29.5 (3) | 36.8 (5) | 21.7 (3) |
| Non-helical PheB1 | 38.9 (11) | 25.4 (3) | 43.6 (13) | 15.8 (3) |
a Rmerge = S|Ii - I|/SI where Ii is an individual intensity measurement and I is the mean intensity for this reflection.
b R value = crystallographic R-factor = S|Fobs| - |Fcalc|/S|Fobs|, where Fobs and Fcalc are the observed and calculated structure factors respectively. Rfree value is the same as R value but calculated on 5% of the data not included in the refinement.
c Root-mean-square deviations of the parameters from their ideal values.
d Figures in parenthesis indicate number of monomers in each group.