Table II. Summary of crystallographic analysis of tACs.
| Data collection statistics | ||||||||||||
| Dataset |
|
Unit cell and space group |
Resolution (Å) |
Measured, unique reflections |
|
|
Rmergea |
I/σ(I)b |
Completeness (%) |
|
||
| GRESAG4.1, crystal form A | a = 49.9 Å, b = 60.1 Å,c = 79.7 Å (P212121) | 10–1.46 | 498 167, 40 911 | 0.082 (0.283) | 24.7 (4.3) | 98.7 (98.9) | ||||||
| + Pb(Me)3Ac | 10–1.50 | 97 405, 31 193 | 0.047 (0.091) | 22.3 (11.5) | 96.7 (80.8) | |||||||
| + GdCl3 | 10–2.80 | 7230, 3401 | 0.123 (0.277) | 13.6 (5.7) | 76.0 (77.2) | |||||||
| + MeHgOH | 10–2.30 | 38 256, 10 880 | 0.079 (0.177) | 24.0 (11.1) | 99.3 (99.6) | |||||||
| GRESAG4.1, crystal form B | a = 123.8 Å, b = 35.8 Å,c = 59.3 Å (P21212) | 10–2.10 | 42 128, 16 265 | 0.045 (0.250) | 21.6 (3.6) | 88.2 (68.8) | ||||||
| GRESAG4.3 | a = 89.7 Å, b = 89.7 Å,c = 67.4 Å (I41) | 20–1.63 | 175 430, 49 013 | 0.036 (0.084) | 21.1 (11.6) | 98.9 (99.7) | ||||||
| + Mg2+ |
|
|
|
23–1.90 |
136 749, 21 016 |
|
|
0.095 (0.194) |
26.4 (13.1) |
99.5 (99.7) |
|
|
| Phasing statistics | ||||||||||||
| Phasing powere |
||||||||||||
| Derivative | Risoc | Sites | RCullisd | 5.2 Å | 3.8 Å | 3.1 Å | 2.7 Å | 2.4 Å | 2.2 Å | 2.0 Å | 1.9 Å | Total |
| Pb(Me)3Ac, A | 0.186 | 5 | 0.66 | 3.15 | 2.10 | 1.80 | 2.01 | 2.05 | 1.91 | 1.94 | 2.15 | 2.04 |
| MeHgOH, A | 0.257 | 5 | 0.81 | 2.60 | 1.51 | 1.27 | 1.31 | 1.44 | 1.39 | 1.46 | ||
| GdCl3 (I), A | 0.265 | 3 | 0.75 | 3.01 | 1.96 | 1.72 | 1.79 | 2.03 | ||||
| GdCl3 (II), A | 0.258 | 3 | 0.76 | 3.28 | 1.89 | 1.48 | 1.55 | 1.90 | ||||
| Figure of merit | 0.81 | 0.69 | 0.63 | 0.57 | 0.58 | 0.51 | 0.46 | 0.45 | 0.55 | |||
| Refinement statistics | ||||||||||||
| Dataset (PDB code) | Resolution(Å) | Reflections(F > 0) | R-factor, Rfreef | No. of atoms,waters, heteroatoms | r.m.s.d.bonds (Å)g | r.m.s.d.angles (°)g | ||||||
| GRESAG4.1, form A (1FX4) | 10–1.46 | 39 779 | 0.178, 0.205 | 2142, 273, 13 | 0.031 | 2.26 | ||||||
| GRESAG4.1, form B | 20–2.00 | 16 219 | 0.240, 0.290 | 1935, 151, 0 | 0.010 | 1.42 | ||||||
| GRESAG4.3, –Mg2+ | 20–1.63 | 33 441 | 0.210, 0.240 | 2084, 265, 0 | 0.010 | 1.40 | ||||||
| GRESAG4.3, +Mg2+ (1FX2) | 20–1.90 | 21 016 | 0.220, 0.230 | 2073, 269, 1 | 0.008 | 1.28 | ||||||
aRmerge = ΣhklΣi|Ii(hkl) – <I(hkl)> |/ΣhklΣiIi(hkl); values in parentheses correspond to the highest resolution shell.
bAs calculated with the program TRUNCATE (CCP4, 1994).
cRiso = Σ||Fderiv| – |Fnative||/Σ|Fnative|
dRCullis = Σ||FPH ± FP| – FH(calc)|/Σ|FPH ± FP|
eThe phasing power is the ratio of the r.m.s. value of |FH| and the r.m.s. of the lack-of-closure error.
fRfactor = Σ|Fobs – Fcalc|/ΣFobs; Rfree calculated with 5% of the data.
gR.m.s.ds for bond angles and length in regard to Engh and Huber parameters (Engh and Huber, 1991).