Table 1 Crystallographic data and structure refinement for compounds 1–3.
1 | 2 | 3 | |
|---|---|---|---|
Empirical formula | C61H109.5N4.5O25S2V6 | C50H100N12O19V6 | C42H88Br2N2O19V6 |
Size [mm3] | 0.1 × 0.2 × 0.3 | 0.4 × 0.35 × 0.15 | 0.15 × 0.2 × 0.35 |
Formula weight | 1675.79 | 1478.55 | 1390.60 |
Crystal system | Monoclinic | Monoclinic | Triclinic |
Space group | C2/c | C2/c | P-1 |
a [Å] | 29.7672(12) | 28.0514(15) | 10.8872(2) |
b [Å] | 16.4119(4) | 16.1942(6) | 13.0882(4) |
c [Å] | 16.6684(5) | 16.8286 | 20.4111(6) |
α [°] | 81.547(3) | ||
β [°] | 108.645(3) | 115.432(4) | 83.464(2) |
γ [°] | 85.946(2) | ||
V [Å3] | 7715.7(4) | 6903.9(5) | 2853.86(14) |
Z | 4 | 4 | 2 |
Dcalc [g.cm−3] | 1.443 | 1.379 | 1.618 |
Temperature [K] | 173.0(1) | 106.1(2) | 297.51(18) |
Tmax/Tmin | 1.000/0.504 | 1.000/0.899 | 1.000/0.577 |
Absorption coeff. [mm−1] | 6.992 | 0.849 | 10.131 |
F (000) | 3508.0 | 3008 | 1428.0 |
θ range [°] | 3.84 to 76.32 | 2.99 to 29.60 | 3.42 to 75.95 |
Reflections collected | 27383 | 13862 | 20449 |
GOF on F 2 | 1.048 | 1.055 | 1.052 |
Final R indices [I > 2σ(I)] | R 1 = 0.0509, wR 2 = 0.1456 | R 1 = 0.0632, wR 2 = 0.1625 | R1 = 0.0685, wR 2 = 0.2029 |
R indices (all data) | R 1 = 0.0562, wR 2 = 0.1510 | R 1 = 0.0862, wR 2 = 0.1781 | R1 = 0.0834, wR 2 = 0.2153 |
