Table 1. Crystal Data, Data Collection Parameters, and Structure Refinement Details for (Bu4N)[cis-MCl4(NO)(Hind)] (M = Ru (1); Os (3)) and (Bu4N)[trans-MCl4(NO)(Hind)] (M = Ru (2); Os (4)).
| compound | 1 | 2 | 3 | 4 |
|---|---|---|---|---|
| empirical formula | C23H42Cl4N4ORu | C23H42Cl4N4ORu | C23H42Cl4N4OOs | C23H42Cl4N4OOs |
| fw | 633.48 | 633.48 | 722.61 | 722.62 |
| space group | P21/n | P21/c | P21/n | P21/c |
| a [Å] | 12.4091(4) | 10.0975(5) | 12.35414(12) | 10.0836(7) |
| b [Å] | 52.5720(15) | 15.8422(9) | 52.4121(4) | 15.8530(10) |
| c [Å] | 13.7339(4) | 18.9705(10) | 13.87637(13) | 18.9740(10) |
| α [deg] | ||||
| β [deg] | 100.7330(10) | 100.759(2) | 100.7569(9) | 101.298(7) |
| γ [deg] | ||||
| V [Å3] | 8802.9(5) | 2981.3(3) | 8827.14(14) | 2974.3(3) |
| Z | 12 | 4 | 12 | 4 |
| λ [Å] | 0.70713 | 0.71073 | 1.54184 | 0.71070 |
| ρcalcd [g cm–3] | 1.434 | 1.411 | 1.631 | 1.614 |
| cryst size [mm3] | 0.14 × 0.14 × 0.10 | 0.15 × 0.02 × 0.02 | 0.27 × 0.17 × 0.14 | 0.57 × 0.29 × 0.15 |
| T [K] | 150(2) | 150(2) | 100(2) | 100(2) |
| μ [mm–1] | 0.921 | 0.906 | 11.698 | 4.668 |
| R1a | 0.0715 | 0.0310 | 0.0316 | 0.0304 |
| wR2b | 0.1288 | 0.0641 | 0.0860 | 0.0697 |
| GOFc | 1.064 | 1.025 | 1.042 | 1.033 |
a
R1 = ∑∥Fo| – |Fc∥/∑|Fo|.
b
wR2 = {∑[w(Fo2 – Fc2)2]/∑[w(Fo2)2]}1/2.
c
GOF = {∑[w(Fo2 – Fc2)2]/(n – p)}1/2, where n is the number of reflections and p is the total number of parameters refined.