Table 1.
Crystal Data and Structure Refinement for [Re(CO)3(DTGH)-NNO]PF6·H2O (5 PF6·H2O), [Re(CO)3(DTG)-NNN]·H2O (6·H2O), [Re(CO)3(UEDDAH)-NNO] (8), [Re(CO)3(DTMH)-NNO]·2H2O (9·2H2O) and [Re(CO)3(DTA)-NNN]·CH3OH (12·CH3OH)
| 5 PF6·H2O | 6·H2O | 8 | 9·2H2O | 12·CH3OH | |
|---|---|---|---|---|---|
| empirical formula | C9H15F6N3O6PRe | C9H14N3O6Re | C9H11N2O7Re | C10H18N3O9Re | C10H18N3O6Re |
| fw | 592.41 | 446.43 | 445.40 | 510.47 | 462.47 |
| T (K) | 173 (2) | 100 (2) | 173 (2) | 100 (2) | 173 (2) |
| λ (Å) | 1.54178 | 1.54178 | 1.54178 | 0.71073 | 1.54178 |
| crystal system | monoclinic | monoclinic | orthorhombic | monoclinic | monoclinic |
| space group | P21/c | P21/n | Pna21 | P21/n | P21/n |
| unit cell dimensions | |||||
| a (Å) | 9.7966 (4) | 7.8847 (10) | 11.8855 (5) | 10.241 (9) | 8.2324 (9) |
| b (Å) | 12.3907 (5) | 12.7776 (2) | 7.7212 (3) | 13.256 (11) | 12.6243 (13) |
| c (Å) | 14.4301 (5) | 13.4044 (2) | 13.6549 (6) | 11.602 (11) | 13.6879 (14) |
| β (°) | 107.363 (2) | 94.2740 (10) | 90 | 92.37 (2) | 96.321 (14) |
| V (Å3) | 1671.81 (11) | 1346.70 (3) | 1253.11 (9) | 1574 (2) | 1413.9 (3) |
| Z | 4 | 4 | 4 | 4 | 4 |
| ρ calc (mg/m3) | 2.354 | 2.202 | 2.361 | 2.155 | 2.173 |
| μ (mm−1) | 16.086 | 17.929 | 19.309 | 7.773 | 17.103 |
| R indices [I>4σ(I)] | R1 = 0.0633 | R1 = 0.0756 | R1 = 0.0230 | R1 = 0.0946 | R1 = 0.0252 |
| wR2 = 0.2006 | wR2 = 0.2629 | wR2 = 0.0583 | wR2 = 0.2390 | wR2 = 0.0661 | |
| R indices (all data) | R1 = 0.0690 | R1 = 0.0890 | R1 = 0.0230 | R1 = 0.1051 | R1 = 0.0257 |
| wR2 = 0.2197 | wR2 = 0.2966 | wR2 = 0.0583 | wR2 = 0.2491 | wR2 = 0.0665 | |
R1 = (Σ | |Fo| - |Fc| | )/Σ |Fo|; wR2 = [Σ[w(Fo2 – Fc2)2]/Σ[w(Fo2)2]]1/2 ; where w = 1/[σ2(Fo2) + (aP)2 + bP] and P = [(Max;0, Fo2) + 2 Fc2]/3