| Crystal data |
|
M
r
|
421.18 |
540.08 |
| Crystal system, space group |
Trigonal, R
c:H
|
Triclinic, P
|
| Temperature (K) |
293 |
293 |
|
a, b, c (Å) |
8.425 (1), 8.425 (1), 54.749 (11) |
7.346 (2), 9.148 (2), 9.662 (2) |
| α, β, γ (°) |
90, 90, 120 |
64.89 (3), 70.51 (3), 69.94 (3) |
|
V (Å3) |
3365.5 (10) |
538.6 (3) |
|
Z
|
18 |
3 |
| Radiation type |
Mo Kα |
Mo Kα |
| μ (mm−1) |
17.27 |
33.58 |
| Crystal size (mm) |
0.09 × 0.08 × 0.03 |
0.10 × 0.05 × 0.04 |
| |
| Data collection |
| Diffractometer |
Nonius KappaCCD single-crystal four-circle |
Nonius KappaCCD single-crystal four-circle |
| Absorption correction |
Multi-scan (HKL
SCALEPACK; Otwinowski et al., 2003 ▸) |
Multi-scan (HKL
SCALEPACK; Otwinowski et al., 2003 ▸) |
|
T
min, T
max
|
0.306, 0.625 |
0.134, 0.347 |
| No. of measured, independent and observed [I > 2σ(I)] reflections |
3994, 1105, 1014 |
7723, 3906, 3391 |
|
R
int
|
0.023 |
0.021 |
| (sin θ/λ)max (Å−1) |
0.704 |
0.758 |
| |
| Refinement |
|
R[F
2 > 2σ(F
2)], wR(F
2), S
|
0.021, 0.052, 1.12 |
0.022, 0.051, 1.06 |
| No. of reflections |
1105 |
3906 |
| No. of parameters |
62 |
208 |
| No. of restraints |
1 |
4 |
| H-atom treatment |
All H-atom parameters refined |
Only H-atom displacement parameters refined |
| Δρmax, Δρmin (e Å−3) |
0.87, −0.72 |
0.96, −1.13 |
