摘要
The title compound was prepared by dissolving 1.3g MoCl3·3H2O into 20 ml anhydrous formic acid. The solution was then heated and refluxed for half an hour. After cooling a bit, 20ml anhydrous ethanol saturated with HCl and 0.5g （Et4N）I were added to the solution. The brown twin crystals were crystallized in three days. The formula of the product was confirmed by elemental chemical analysis. Found: Mo, 36.09; Cl, 26.84; C, 15.19; H, 3.54; N, 1.76. Calcd: Mo, 36.82; Cl, 27.21; C, 16.90; H, 2.97; N, 1.79. Diffraction work of a selected twin
The title compound was prepared through oxidation of MoCl_3 in the liquid phase. The crystal belongs to the orthohombic system with space group D_(2h)^(16)-Pmnb and unit cell parameters: a=11.403 (1), b=12.345 (2), c=14.292(2)■, V=2011.8(8)(?)~3; Z=4, D_c 2.396g/cm^3. The 2303 independent reflections were collected on a CAD4 four-circle diffractometer with Mo Kα radiation in a range 2≤θ≤27. The crystal structure was solved by heavy-atoms method and refined by a full matrix least-squares technique to final discrepancy factors R=0.050 and R_w=0.056 for 1513 reflections of I≥3σ(I). The configuration of cluster anion was characterized to have the same M1 type strueture as presented in a previous paper. The average bond lengths Mo—Mo is 2.577■, Mo—O-μ3 is 1.982■. In addition, relation of Mo—Mo bonds with the bridging atom, bond order, and other lignds coordinated to the Mo atom is discussed briefly.
