| Popis: |
Two new monocapped trinuclear molybdenum and tungsten clusters, which also contain different numbers of bridging halogen atoms and carboxylate groups, have been synthesized and characterized by X-ray diffraction, thus completing an entire series of monocapped trinuclear molybdenum and tungsten clusters with 1–6 bridging carboxylate ligands. Compound 1, (Et4N)[W3OCl5(OAc)4]·3CH2Cl2, was obtained as a byproduct in the reaction of (Et4N)3[W2Cl9] with acetic acid and acetic anhydride. Crystallographic data: space group P212121, a=12.795(3), b=15.685(3), c=19.436(3) A, V=3901(1) A3, Z=4, R=0.037. The W-W distances are 2.7280(7), 2.5754(8) and 2.5715(8) A. The average oxidation state of the tungsten atoms is +3.33. Compound 2, (Et4N)[Mo3OCl6(OAc)2(PMe3)2], was synthesized by the reaction of (Et4N)[Mo3OCl6(OAc)3] with Me3SiCl and PMe3 in THF. Crystallographic data: space group Pna21, a=27.459(7), b=13.660(5), c=18.524(5) A, V=6948 A3, Z=8, R=0.052. The Mo-Mo distances are 2.627(4), 2.546(3) and 2.631(6) A. The entire series of monocapped trinuclear molybdenum and tungsten clusters with 0–6 μ-CH3CO2 groups is reviewed. |
