Reaction of (NH4)2WOS3 with CuI and 4-tert-butylpyridine (4-bpy) in EtOH afforded a tetranuclear neutral cluster WOS3Cu3I(4-bpy)3·0.25EtOH. This compound was characterized by elementary analysis, IR, 1H NMR, TGA, and its crystal structure was determined by X-ray single crystal diffraction. It belongs to monoclinic, space group P2/c with a=2.220 9(2) nm, b=1.364 66(11) nm, c=2.490 6(2) nm, β=104.953(2)°, V=7.292 9(12) nm3, Z=4. The title compound may be viewed as having a half-open cubane-like structure in which three Cu(4-bpy)+ units are linked by a triply-bridging WOS32- unit and a doubly-bridging iodine atom. CCDC: 266412.
Thermoanalysis study has been carried out on the complex of bis[1 (2 thienyl) 4,4,4 trifluoro butanedione 1,3]copper? and its adducts with pyridine, 2,2′ bipyridine, quinoline and dimethyl sulfoxide in a dynamic nitrogen atmosphere by simultaneous TG DTG DSC technique. The experimental results showed that the decomposition modes of the solvent molecules were various according to the different structures of the complex, in general, the decomposition of them was ahead of the decomposition of the ligand 1 (2 thienyl) 4,4,4 triflurobu tanedione 1,3. Among them the adduct with 2,2 bipyridine showed a quite unique thermal behavior. Several methods have been jointly used to study the kinetics of all the thermal decomposition stages for title compounds, which showed that the evolution of the solvent molecules was controlled mainly by Rn mechanism (or Am mechanism for 2,2 bipyridine adduct) with lower activation energy; while the release of 1 (2 thienyl) 4,4,4 trifluro butane dione 1,3 was gove rned by D2 or D3 mode with higher activation energy.
The title compound [Ni(acac)2(dadpm)]∞ (acac=acetylacetonate, dadpm=4 ,4′-diaminodiphenylmethane) was synthesized from Ni(acac)2·2H2O with dadpm in DMF. The structure was characterized by elemental analysis, IR spectroscopy, the rmal analysis and single-crystal X-ray diffraction. X-ray analysis revealed that the central Ni atom is at a center of symmetry, and is octahedrally coordinated by four O atoms from two acac anions and two N atoms from two dadpm ligands. Ea ch dadpm ligand, which has a two-fold axis passing through its methylene C atom, bridges two Ni atoms to form a 1D polymeric chain. Neighboring chains connect v ia H bonding interactions to generate a 2D network. It crystallizes in the monoc linic system, space group P2/c with a=0.556 79(7), b=0.896 06(12), c=2.187 3(3) nm, β=94.942(3)°, V=1.087 2(3) nm3, Z=2, Dc=1.390 g·cm-3, F(000)=480, Mr=455. 17, μ(Mo Kα)=0.924 mm-1, R(F)=0.036 0, wR(F 2)=0.101 0, S=1.013. CCDC: 254565 .
