Junxhe Xu

Hydrothermal synthesis and characterization of [Ni(phen)3]2[Mo8O26]·2H2O

Abstract The reaction of MoO3, H2MoO4 and Ni(Ac)2·6H2O with 1,10-phenanthroline by a hydrothermal method furnishes the discrete cluster [Ni(phen)3]2[Mo8O26]·2H2O (1). The structure of 1 is triclinic, space group P1, a=11.4965(10), b=11.6829(13), c=15.1518(15) A, α=83.032(8), β=71.557(7), γ=78.319(7)°, R=0.0433 for 7397 observed [I>2σ(I)] reflections. The crystallographically determined solid state structure of 1 shows that the cluster consists of two complex cations, one cluster anion [Mo8O26]4− and two water molecules of crystallization. Each nickel ion is coordinated by six nitrogen atoms from three phenanthroline ligands, forming a distorted octahedron, and the anion has a β-configuration formed by eight edge-sharing MoO6 octahedra. Compound 1 was characterized by means of elemental analysis, IR spectra and TGA analysis.

Mobybdenum(VI)-oxygen complex containing citrage ligand: synthesis and characterization of K6[Mo2O5(cit)2]·5H2O

Abstract The complex, K6[Mo2O5(cit)2]·5H2O was obtained by crystallization from reaction of [Et4N]3[Mo2FeS8O2 and potassium citrate (K3cit) in methanol and water under an atmosphere of pure nitrogen at ambient temperature. The complex is triclinic, space group P1, a = 11.843(8) A, b = 13.717(8) A, c = 10.287(5) A, α = 108.11(4) °, β = 99.42(5) (1) °, γ = 66.52(4) °, R = 0.034 for 4510 observed (I > 3 σ (I)) reflections. Single crystal structure analysis reveals that citrate ligand coordinated to molybdenum atom through two carboxylato oxygens and one deprotonated hydroxyl oxygen together with one bridging oxygen atom and two terminal oxygen atoms completes distorted coordination octahedron around each molybdenum atom. IR spectra are in agreement with the structure.

NH4)2Na3(V3W3O19).12H2O

(NH 4 ) 2 Na 3 (V 3 W 3 O 19 ).12H 2 O, diammonium trisodium nonadecaoxo(tritungsto)trivanadate dodecahydrate, is a mixed V/W salt in which each site has an approximately equal population of V and W atoms. The centrosymmetric polyanion consists of six (V/W)O 6 edge-sharing distorted octahedra and has a well established structure. Each of the three Na + cations is surrounded by six water molecules in a distorted octahedron. The (V/W)-O distances are between 1.644 (14) and 2.2885 (10) A.

(NH4)3[PMo12O40].21H2O

The determinaton of the crystal structure of the title compound, triammonium hexatriacontaoxo(tetraoxophosphato)dodecamolybdate(3−) heneicosahydrate, shows that the polyanion has a pseudo-Keggin structure with m\overline{3}m symmetry. The central PO4 group is disordered with P—O distances of 1.55 (3) A. The Mo—O distances range from 1.617 (14) to 2.414 (14) A.