Table 1.
Crystallographic Data for Single and Double Cubane Cluster Compounds
| (Et4N)2[3] ·MeCN | (Et4N)2[4] | (Bu4N)2[6] | (Et4N)4[9] ·8MeCN ·3H2O | (Et4N)4[10] ·2MeCN | (Bu4N)4[12] ·6MeCN | |
|---|---|---|---|---|---|---|
| formula | C27H53BF3Fe3N9S4V | C25H50BFe3N17S4V | C44H82BFe3N11S4V | C66H130B2F4Fe6N24O3S8V2 | C54H106B2Fe6N30S8V2 | C98H182B2Fe6N26S8V2 |
| fw | 918.08 | 946.09 | 1122.32 | 2098.36 | 1890.21 | 2438.79 |
| crystal system | monoclinic | monoclinic | monoclinic | orthorhombic | monoclinic | monoclinic |
| space group | P21/c | P21/c | P21/n | Pnnm | P21/c | P21/n |
| Z | 4 | 12 | 4 | 4 | 2 | 2 |
| a, Å | 10.8425(6) | 23.671(8) | 11.224(2) | 14.743(2) | 11.867(10) | 18.617(3) |
| b, Å | 16.8430(10) | 34.548(12) | 40.248(7) | 29.397(4) | 20.779(19) | 16.165(3) |
| c, Å | 21.8996(13) | 15.700(5) | 12.602(2) | 11.0978(15) | 17.148(15) | 23.299(4) |
| β, deg | 96.1270(10) | 108.308(7) | 97.759(3) | 90.00 | 100.134(14) | 110.141(2) |
| V, Å3 | 3976.5(4) | 12189(7) | 5640.8(17) | 4809.7(11) | 4162(6) | 6583(2) |
| dcalcd g/cm3 | 1.534 | 1.547 | 1.322 | 1.955 | 1.509 | 1.189 |
| μ, 1/mm | 1.557 | 1.522 | 1.105 | 2.539 | 1.484 | 0.950 |
| 2θ range, deg | 1.53 → 27.49 | 0.91 → 28.35 | 1.01 → 27.89 | 1.39 → 25.21 | 1.55 → 25.09 | 1.57 → 25.02 |
| GOF (F2) | 0.994 | 1.058 | 1.027 | 1.005 | 1.028 | 0.993 |
| R1a/wR2b | 0.0381/0.0847 | 0.0795/0.1328 | 0.0663/0.1740 | 0.0608/0.1755 | 0.0585/0.1593 | 0.0866/0.1711 |