Table 3.
Crystallographic data and structure refinement parameters for 5–8.
| 5 | 6 | 7·2MeCN | 8 | |
|---|---|---|---|---|
| Empirical formula | C66H108Mn6N8O22 | C58H98Mn6N4O22 | C47H78Mn4N6O15 | C72H128Fe2Mn4N6O26 |
| Formula weight (g·mol−1) | 1695.24 | 1533.04 | 1186.91 | 1825.26 |
| T/K | 173(2) | 296(2) | 173(2) | 150(2) |
| Crystal system | Monoclinic | Monoclinic | Triclinic | Monoclinic |
| Space group | P21/n | Pn | P‾1 | C2/c |
| a (Å) | 13.7821(10) | 14.404(3) | 13.4652(18) | 13.4462(15) |
| b (Å) | 21.676(2) | 16.331(3) | 13.7324(18) | 29.008(3) |
| c (Å) | 13.8218(10) | 16.330(3) | 18.150(2) | 23.868(3) |
| α (o) | 90 | 90 | 111.943(2) | 90 |
| β (o) | 98.7840(10) | 103.009(3) | 90.612(2) | 91.930(2) |
| γ (o) | 90 | 90 | 103.879(2) | 90 |
| V (Å3) | 4080.8(5) | 3742.6(14) | 3003.2(7) | 9304.3(18) |
| Z | 2 | 2 | 2 | 4 |
| Dcalc (g·cm−3) | 1.380 | 1.360 | 1.313 | 1.303 |
| μ (mm−1) | 0.971 | 1.050 | 0.884 | 0.900 |
| F(000) | 1772 | 1600 | 1244 | 3848 |
| θ range for data collection (o) | 1.76 to 26.60 | 1.25 to 28.27 | 1.22 to 26.90 | 1.40 to 28.28 |
| Reflections collected | 30,266 | 21,851 | 28,737 | 39,848 |
| Reflections unique | 8537 | 14,323 | 12,922 | 11,443 |
| R int | 0.052 | 0.054 | 0.047 | 0.097 |
| Parameters | 460 | 813 | 716 | 542 |
| GOF | 0.990 | 0.969 | 1.052 | 1.025 |
| R1a [Io > 2σI)] | 0.046 | 0.082 | 0.056 | 0.058 |
| wR2b [Io > 2σI)] | 0.131 | 0.199 | 0.148 | 0.126 |
a R1 = Σ||Fo| − |Fc||/Σ|Fo|. b wR2 = {Σ[w(Fo2 − Fc2)2]/Σ[w(Fo2)2]}1/2.