Table 4. Crystallographic Data for 1, 4, 42–, and 5.
| 1 | 4 | 42– | 5 | |
|---|---|---|---|---|
| chem formula | C40H34AlClN8 | C32H27AlN4 | C48H67AlN4Na2O8 | C20H17AlI2N4 |
| Mr | 689.18 | 494.55 | 901.01 | 594.16 |
| cryst syst | triclinic | Monoclinic | monoclinic | Monoclinic |
| color, habit | dark red, block | blue, block | orange, block | blue, block |
| size (mm) | 0.15 × 0.12 × 0.08 | 0.22 × 0.17 × 0.13 | 0.22 × 0.05 × 0.04 | 0.31 × 0.13 × 0.05 |
| space group | P1̅ | C2/c | P21/c | P21/c |
| a (Å) | 8.1107(8) | 21.5590(14) | 13.5694(4) | 8.1926(5)) |
| b (Å) | 12.0912(12) | 15.3001(11) | 21.6184(6) | 14.8013(9) |
| c (Å) | 18.7007(19) | 18.3158(12) | 17.2708(5) | 17.4444(12) |
| α (deg) | 76.541(4) | 90 | 90 | 90 |
| β (deg) | 87.705(4) | 119.229(2) | 107.021(2) | 97.715(2) |
| γ (deg) | 85.258(4) | 90 | 90 | 90 |
| V (Å3) | 1777.0(3) | 5272.3(6) | 4844.4(2) | 2096.2(2) |
| Z | 2 | 8 | 4 | 4 |
| ρcalc, g·cm–3 | 1.288 | 1.246 | 1.231 | 1.883 |
| radiation [Å] | 0.71073 | 0.71073 | 1.54178 (Cu) | 0.71073 |
| μ(Mo Kα) (mm–1) | 0.174 | 0.105 | 3.055 | |
| μ(Cu Kα) (mm–1) | 0.989 | |||
| F(000) | 720 | 2080 | 1928 | 1136 |
| temp (K) | 100(2) | 100(2) | 100(2) | 100(2) |
| θ range (deg) | 2.951–25.679 | 2.952–30.583 | 4.890–70.070 | 2.964–30.587 |
| data collected (h, k, l) | –9:9, −14:14, −22:22 | –30:29, −21:21, −24:26 | –16:16, −25:26, −21:21 | –11:11, −21:19, −24:24 |
| no. of rflns collected | 27047 | 74978 | 92849 | 59061 |
| no. of indpndt reflns | 6656 | 8062 | 9025 | 6418 |
| observed reflns Fo ≥ 2.0 σ (Fo) | 5718 | 6984 | 7154 | 5580 |
| R(F) (%) | 7.00 | 3.72 | 4.12 | 2.59 |
| wR(F2) (%) | 17.50 | 10.45 | 9.10 | 5.16 |
| GooF | 1.141 | 1.040 | 1.039 | 1.089 |
| weighting a, b | 0, 8.7365 | 0.0497, 4.3929 | 0.0296, 2.9547 | 0.0155, 3.0472 |
| params refined | 453 | 335 | 577 | 245 |
| min, max resid dens | –0.412, 0.676 | –0.284, 0.401 | –0.260, 0.310 | –0.791, 0.829 |