Molecule | 1 | 2 | 3 |
---|---|---|---|
Empirical formula System, sp. gr ., Z | C 18 H 24 N 6 O 12 Triclinic, P-1, 2 | C 17 H 14 N 6 O 9 Triclinic, P-1, 2 | C 22 H 24 N 6 O 9 Monoclinic, P2 1 /n, 4 |
a, b, c Å | 8.4411(2), 12.1069(4), 13.3113(6) | 8.8720(2), 11.2160(4), 11.5280(4) | 14.9093(5), 9.4785(3), 17.7118(6) |
α, β, γ deg | 111.383(2), 101.163(2), 102.748(10) | 75.6030(10), 75.0350(10), 90 | 90, 100.2370(10), 90 |
V, Å3 | 1177.41(8) | 1073.40(4) | 2463.15(14) |
D x, Mg/m3 | 1.507 | 1.492 | 1.393 |
Radiation, λ, Å | MoKα, 0.71073 | MoKα, 0.71073 | MoKα, 0.71073 |
μ, mm−1 | 0.130 | 0.127 | 0.110 |
T, K | 293 | 293 | 293 |
Sample size, mm | 0.35 x 0.30 x 0.30 | 0.20 x 0.15 x 0.15 | 0.35 x 0.30 x 0.30 |
Diffractometer | Bruker axs kappa apex2 CCD | Bruker axs kappa apex2 CCD | Bruker axs kappa apex2 CCD |
Scan mode | ω and φ | ω and φ | ω and φ |
Absorption correction | Semi-empirical from equivalents 0.9432,0.9758 | Semi-empirical from equivalents 0.9217,0.9965 | Semi-empirical from equivalents 0.9536,0.9765 |
Tmin, Tmax | |||
θmax, deg | 25.00 | 25.00 | 25.00 |
h, k, l ranges | −12 ≤ h ≤ 11,-15 ≤ k ≤ 15, | −9 ≤ h ≤ 9,-19 ≤ k ≤ 19, | −17 ≤ h ≤ 17,-11 ≤ k ≤ 8, |
-15 ≤ l ≤ 15 | −19 ≤ l ≤ 19 | −21 ≤ l ≤ 21 | |
No of reflections: measured/unique (N1), R int | 20646/4121, 0.0278 | 18538/3769, 0.0295 | 21291/4332, 0.0307 |
Refinement method | Full-matrix least-squares on F2 | Full-matrix least-squares on F2 | Full-matrix least-squares on F2 |
No of refined parameters | 345 | 347 | 338 |
R1/wR2 relative to N1 | 0.0400, 0.1101 | 0.0386, 0.1041 | 0.0413, 0.1113 |
R1/wR2 relative to N2 | 0.0459, 0.1167 | 0.0494, 0.1127 | 0.0596, 0.1293 |
S | 1.041 | 1.047 | 1.020 |
∆ρmax/∆ρmin, e/Å3 | 0.390, −0.277 | 0.273, −0.209 | 0.297,-0.192 |
Programs | APEX2, SIR92, SHELXL97, ORTEP-3, Mercury | APEX2, SIR92, SHELXL97, ORTEP-3, Mercury | APEX2, SIR92, SHELXL97, ORTEP-3, Mercury |