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The 15-cobalt-substituted polyoxotungstate [Co(6)(H(2)O)(30){Co(9)Cl(2)(OH)(3)(H(2)O)(9)(beta-SiW(8)O(31))(3)}](5-) (1) has been characterized by single-crystal XRD, elemental analysis, IR, electrochemistry, magnetic measurements, and EPR. Single-crystal X-ray analysis was carried out on Na(5)[Co(6)(H(2)O)(30){Co(9)Cl(2)(OH)(3)(H(2)O)(9)(beta-SiW(8)O(31))(3)}].37H(2)O, which crystallizes in the hexagonal system, space group P6(3)/m, with a = 19.8754(17) A, b = 19.8754(17) A, c = 22.344(4) A, alpha= 90 degrees, beta = 90 degrees, gamma = 120 degrees, and Z = 2. The trimeric polyanion 1 has a core of nine Co(II) ions encapsulated by three unprecedented (beta-SiW(8)O(31)) fragments and two Cl(-) ligands. This central assembly {Co(9)Cl(2)(OH)(3)(H(2)O)(9)(beta-SiW(8)O(31))(3)}(17-) is surrounded by six antenna-like Co(II)(H(2)O)(5) groups resulting in the satellite-like structure 1. Synthesis of 1 is accomplished in a simple one-pot procedure by interaction of Co(II) ions with [gamma-SiW(10)O(36)](8-) in aqueous, acidic NaCl medium (pH 5.4). Polyanion 1 was studied by cyclic voltammetry as a function of pH. The current intensity of its Co(II) centers was compared with that of free Co(II) in solution. Our results suggest that 1 keeps its integrity in solution. Magnetic susceptibility results show the presence of both antiferro- and ferromagnetic coupling within the (Co(II))(9) core. A fully anisotropic Ising model has been employed to describe the exchange-coupling and yields g = 2.42 +/- 0.01, J(1) = 17.0 +/- 1.5 cm(-1), and J(2) = -13 +/- 1 cm(-(1). Variable frequency EPR studies reveal an anisotropic Kramer's doublet.  相似文献   
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A synthetic route to a series of 4-alkyl- or arylquinolines, bearing in 2- and 3-position fluorinated and phosphonate functions at the same time, is reported for the first time. These compounds are synthesized via regioselective heterocyclization of XCF2-alkynylphosphonates (X=F, Cl, Br, H, CF3) with ortho-aminoaryl ketones (R=CH3, CF3, Ph) in the presence of K2CO3 or Li2CO3/TMEDA as mediators. 2-Fluoro- and 3-phosphorus-containing 4-Me, 4-CF3 or 4-Ph quinolines are obtained in good to excellent yields. The influence of substituents in the aromatic ketone, the XCF2-group in the alkyne as well as mediators and the reaction medium on the reactivity and specificity of the reaction is also investigated.  相似文献   
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We report on an improved synthesis and structural characterization of the cyclic 48-tungsto–8-arsenate(V) [H4As8W48O184]36? (1). The mixed lithium–potassium salt of this polyanion, K26.5Li9.5[H4As8W48O184]·90H2O (KLi-1), has been studied in the solid state by IR, single-crystal X-ray diffraction, and elemental analysis, and in solution by 183W NMR spectroscopy.  相似文献   
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The oxalato-titanium(IV)-containing, dimeric 18-tungsto-2-phosphate [Ti8(C2O4)8P2W18O76(H2O)4]18? (1) and the 32-tungsto-4-phosphate [Ti6(C2O4)4P4W32O124]20? (2) are formed upon reaction of the oxalato-titanium complex [TiO(C2O4)2]2? with the trilacunary Keggin precursor [A-α-PW9O34]9? and the hexalacunary Wells–Dawson precursor [H2P2W12O48]12?, respectively. Polyanion 1 consists of two {PW9} units encapsulating eight titanium centers and connected to each other via two Ti–O–Ti bridges, and crystallizes as a mixed potassium-sodium-lithium salt in the triclinic space group $P{\bar{1}}$ . Polyanion 2 comprises two {P2W16} units containing each two titanium atoms, and the two half-units are connected via two titanium atoms decorated by two oxalate groups each, and crystallizes as a mixed potassium-lithium salt in the rhombohedral space group $R{\bar{3}}c$ . Polyanions 1 and 2 were characterized in the solid state by single-crystal XRD, FT-IR, and TGA, whereas polyanion 2 was also investigated by 31P and 183W NMR.  相似文献   
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