| Crystal data |
|
M
r
|
311.04 |
347.08 |
| Crystal system, space group |
Triclinic, P
|
Orthorhombic, P
c
a21
|
| Temperature (K) |
200 |
180 |
|
a, b, c () |
5.4886(11), 7.8518(15), 11.574(2) |
10.9603(4), 7.9667(7), 26.7735(18) |
| , , () |
99.663(16), 90.366(16), 90.244(16) |
90, 90, 90 |
|
V (3) |
491.71(17) |
2337.8(3) |
|
Z
|
2 |
8 |
| Radiation type |
Mo K
|
Mo K
|
| (mm1) |
1.24 |
1.06 |
| Crystal size (mm) |
0.04 0.03 0.02 |
0.38 0.31 0.08 |
| |
| Data collection |
| Diffractometer |
Stoe IPDS2 |
Stoe IPDS2 |
| Absorption correction |
Integration Coppens (1970 ▶) |
Integration (Coppens, 1970 ▶) |
|
T
min, T
max
|
0.644, 0.789 |
0.684, 0.923 |
| No. of measured, independent and observed [I > 2(I)] reflections |
2659, 2636, 2529 |
15755, 5326, 4919 |
|
R
int
|
0.074 |
0.062 |
| (sin /)max (1) |
0.686 |
0.650 |
| |
| Refinement |
|
R[F
2 > 2(F
2)], wR(F
2), S
|
0.031, 0.089, 1.20 |
0.042, 0.113, 1.09 |
| No. of reflections |
2636 |
5326 |
| No. of parameters |
168 |
380 |
| No. of restraints |
12 |
37 |
| H-atom treatment |
All H-atom parameters refined |
Only H-atom coordinates refined |
|
max, min (e 3) |
0.36, 0.75 |
0.41, 0.67 |
| Absolute structure |
|
Refined as an inversion twin |
| Absolute structure parameter |
|
0.45(9) |
