The reaction between [Cu2(m-dppm)2(MeCN)4](ClO4)2(dppm = bis(diphenylphos- phino)methane) and [Zn(PhS)2(bpy)] (bpy = 2,2-bipyridine, PhS = benzenethiolate) gave the complex [Cu2(m-dppm)2(m-PhS)(MeCN)]ClO40.5(Et2O)(C58H52ClNO4P4SCu20.5Et2O) which was determined by X-ray single-crystal diffraction. The crystal is of orthorhombic, space group P212121 with a = 13.6157(3), b = 20.8022(6), c = 21.3299(6) ? V = 6041.4(3) 3, Mr = 1182.54, Dc = 1.300 g/cm3, F(000) = 2444, m = 0.934 mm-1 and Z = 4. The final R = 0.0773 and wR = 0.1843 for 7744 observed reflections (I > 2s(I)). The dicopper atoms are doubly bridged by dppm as well as one S donor from benzenethiolate. One copper atom is in a distorted trigonal bipyramidal environ- ment, whereas the other adopts a distorted tetrahedral geometry.
Self-assembly between Pt(phen)(edt) (phen=phenanthroline, edt=1,2-ethanedithiolate) and Cu(PPh3)2(MeCN)2(ClO4) (PPh3=triphenylphosphine) gave rise to formation of heterohexanuclear complex Pt4Cu2(edt)4(PPh3)6(ClO4)2(4H2O) (1). The complex was characterized by elemental analyses, ES-MS, UV-Vis, IR, 31P NMR spectroscopy and X-ray crystallography. The molecule consists of two Pt2Cu(edt)2(PPh3)3 units which has a centrosymmmetric inversion to give a cyclic heterohexanuclear skeleton. The PtⅡ and CuⅠ center adopt square-planar and trigonal coordination modes, respectively. The compound shows intense emission at 632 nm in the solid state and at 678 nm in frozen dichloromethane glass at 77 K.
The synthesis and crystal structure of oxo-centered carboxylate-bridge trinuclear ruthenium complex, Ru3O(CH3COO)6(py)2Cl (py = pyridine) (1), are reported herein. The complex 1 has been characterized by IR, cyclic voltammetry (CV), UV-Vis and X-ray crystal analysis. The complex 1 in 0.1 mol/L (n-C4H9)4NPF6-CH2Cl2 solution at room temperature shows four one- electron redox processes at E1/2 = -1.38, -1.20, -0.17 and 1.07 V vs. Ag/AgCl.
The heterotrinuclear complex [PtCu2(m-dppm)2(dmbpy)2(m-h1,h2 C CPhCH3-4)2] (ClO4)21.5CH2Cl2 1 (dmbpy = 4,4-dimethyl-2,2?bipyridine, dppm = bis(diphenylphosphino)meth- ane) has been prepared and characterized by X-ray crystallography. The complex crystallizes in the triclinic system, space group P with a = 12.9359(3), b = 14.3908(2), c = 15.2121(3) ? α = 107.370(1), β = 93.539(1), γ = 108.207(1), V = 2529.59(8) ?, Mr = 2015.96, Z = 1, Dc = 1.323 g/cm3, F(000) = 1019, m(MoKa) = 2.042 mm-1, the final R = 0.0604 and wR = 0.1529 for 8002 observed reflections with I > 2σ(I). The 4-methylphenylacetylides are bonded to the PtII and CuI centers in η1 (s) and η2 (p) coordination modes, respectively. The PtII atom is linked by one dppm bridge to adopt a square planar environment and CuI by one alkynyl ligand to assume a distorted tetrahedral geometry.
A novel dimeric complex [Ru3 (μ3-O)(μ-CH3COO)(CO)]2(μ-dppf)(μ-odppf)(dppf = 1, 1'-bis(diphenylphosphio)ferrocene, odppf = 1, 1'-bis(oxodiphenylphosphoranyl)ferrocene) (1) of oxo-centered triruthenium-aectate cluster units was synthesized and characterized by X-ray crystallography. Compound 1 exhibits a cyclic structure formed by linkages of two triruthenium cluster units Ru3 (μ3-O)(μ-CH3COO)6(CO) through dppf and odppf ligands, respectively. The diameter of the molecular loop is ca. 1.0 nm.
