Table 4.
Crystal data, data collection and structure refinement.
| Compound | 1 | 2 | 4 | 6 | 7 | 8 | 9 | 10 | 12 |
|---|---|---|---|---|---|---|---|---|---|
| Formula | C12H12Cl3FeN6 | C13H16Cl2FeN6O+·Cl− | C10H11Cl3FeN5 | C11H13Cl3FeN5 | C24H24FeN122+·2(CF3SO3)−·C4H10O | C24H24FeN122+·2(CF3SO3)−·solvent | C26H28FeN122+·2(CF3SO3) −·C5H12O | C20H22FeN102+·2(CF3SO3)−·C4H10O | C22H26FeN102+·2(CF3SO3)−·CH4O |
| FeL1Cl3 | [FeL2Cl2(CH3OH)]+·Cl− | FeL4Cl3 | FeL6Cl3 | (FeL12)2+·2(CF3SO3)−·C4H10O | (FeL22)2+·2(CF3SO3)−·solvent | (FeL32)2+·2(CF3SO3)−·C5H12O | (FeL42)2+·2(CF3SO3)−·C4H10O | (FeL62)2+·2(CF3SO3)−·CH3OH | |
| Formula weight | 402.48 | 434.52 | 363.44 | 377.46 | 908.66 | 834.54 | 950.74 | 830.58 | 816.56 |
| Crystal system | triclinic | monoclinic | triclinic | monoclinic | monoclinic | monoclinic | triclinic | monoclinic | orthorhombic |
| Space group | P-1 | P21/n | P-1 | P21/c | C2/c | P21/c | P-1 | P21/c | Pca21 |
| a (Å) | 7.459(2) | 7.6840(4) | 7.5198(4) | 7.2144(2) | 23.1912(8) | 12.9879(7) | 12.4297(8) | 15.5382(2) | 22.3563(6) |
| b (Å) | 9.055(2) | 13.9429(6) | 8.1040(6) | 12.4684(3) | 17.0021(5) | 13.0532(8) | 13.0407(7) | 12.55315(14) | 8.3830(2) |
| c (Å) | 12.460(3) | 16.8684(6) | 12.4702(10) | 16.7244(4) | 22.3107(8) | 21.9024(19) | 13.4814 (7) | 18.1225 (2) | 17.5420(6) |
| α (°) | 75.69(2) | 90 | 75.205(6) | 90 | 90 | 90 | 88.870(4) | 90 | 90 |
| β (°) | 87.94(2) | 98.281(4) | 84.655(5) | 99.730(2) | 116.163(4) | 91.711(6) | 74.131(5) | 91.2230(13) | 90 |
| γ (°) | 66.12(3) | 90 | 66.519(6) | 90 | 90 | 90 | 75.262(5) | 90 | 90 |
| V(Å3) | 743.7(4) | 1788.39(14) | 673.87(9) | 1482.75(7) | 7895.8(5) | 3711.5(4) | 2029.9(2) | 3534.05(7) | 3287.60(16) |
| Z | 2 | 4 | 2 | 4 | 8 | 4 | 2 | 4 | 4 |
| Dx(g cm−3) | 1.797 | 1.614 | 1.791 | 1.691 | 1.529 | 1.493 | 1.556 | 1.561 | 1.650 |
| F(000) | 406 | 884 | 366 | 764 | 3728 | 1696 | 980 | 1704 | 1672 |
| μ (mm−1) | 13.136 | 1.305 | 14.392 | 1.553 | 0.577 | 0.604 | 0.565 | 0.634 | 0.680 |
| Reflections: | |||||||||
| collected | 1450 | 7518 | 4550 | 6161 | 18337 | 13346 | 30279 | 15200 | 17885 |
| unique (Rint) | 917 (0.042) | 3576 (0.024) | 2666 (0.054) | 3106 (0.022) | 7987 (0.031) | 6526 (0.059) | 7129 (0.083) | 7095 (0.015) | 5695 (0.029) |
| with I>2σ(I) | 716 | 2958 | 2319 | 2688 | 6243 | 3623 | 5726 | 6301 | 5323 |
| R(F) [I>2σ(I)] | 0.078 | 0.033 | 0.075 | 0.029 | 0.058 | 0.081 | 0.059 | 0.030 | 0.063 |
| wR(F2) [I>2σ(I)] | 0.233 | 0.081 | 0.196 | 0.059 | 0.174 | 0.153 | 0.156 | 0.072 | 0.165 |
| R(F) [all data] | 0.104 | 0.044 | 0.084 | 0.037 | 0.077 | 0.146 | 0.070 | 0.035 | 0.067 |
| wR(F2) [all data] | 0.233 | 0.087 | 0.204 | 0.063 | 0.188 | 0.174 | 0.169 | 0.075 | 0.169 |
| Goodness of fit | 1.05 | 1.05 | 1.14 | 1.04 | 1.24 | 1.02 | 1.07 | 1.02 | 1.08 |
| max/min Δρ (e·Å−3) | 0.77/−0.98 | 0.50/−0.29 | 1.75/−0.79 | 0.32/−0.31 | 1.68/−0.67 | 0.87/−0.45 | 1.14/−0.62 | 0.34/−0.39 | 0.83/−0.92 |
| CCDC number | 1851825 | 1851824 | 1851829 | 1851826 | 1871758 | 1871759 | 1871760 | 1871763 | 1871761 |