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The complexes [Co(Him)2(μ4-bta)1/2]n 1 and {[Cu(phen)(μ4-bta)1/2]·H2O}n 2 were hydrothermally synthesized at 160°C and their structures were determined by single-crystal X-ray diffraction. Complex 1 was triclinic, space group P–1, a=7.9294(11) A˚, b=9.621(3) A˚, c=9.6461(16) A˚, α=116.772(19)°, β=96.791(13)°, γ=102.787(19)°, Z=2, V=620.3(2) A˚3, R1=0.0252 and wR2=0.0640 [I>2σ(I)]; complex 2 was monoclinic, space group P21/c, a=7.386(3) A˚, b=12.723(4) A˚, c=15.831(3) A˚, β=102.66(2)°, Z=4, V=1451.5(7) A˚3, R1=0.0389 and wR2=0.1033 [I>2σ(I)]. In both of the structures the metal ions were linked by the μ4-bridging benzene-1,2,4,5-tetracarboxylate ligands, resulting in one-dimensional double-metal chains. The synthesized products were characterized by IR spectroscopy, UV–VIS spectra, inductively coupled plasma (ICP), elemental, thermogravimetric (TGA) and magnetic analyses. [Copyright &y& Elsevier]

Abstract: Three novel hetero-polyoxovanadates, [Cd(2,2′-bpy)3]{[Cd(dien)]As8V14O42(H2O)} (1, 2,2′-bpy=2,2′-bipyridine, and dien=diethylenetriamine), [Zn(2,2′-bpy)2]2[As8V14O42(H2O)]·H2O (2) and [Ni(en)2]3[As8V14O42(HPO3)]·4H2O (3, en=ethlenediamine), were hydrothermally synthesized and characterized by single-crystal X-ray diffraction. Crystal data: 1 monoclinic, P2(1)/n, , , , , Z=4. 2, orthorhombic, P2(1)2(1)2(1), , , , . 3, triclinic, , , , , , , , . Compounds 1–3 are all made of the {As8V14O42} shells linked by corresponding transition metal complexes into extended structures. Compound 1 and 2 present 1-D wave-like and tubular structures, respectively, while compound 3 exhibits a novel 2-D structure containing interwinding puckery layers. Variable temperature susceptibility measurements demonstrate the presence of antiferromagnetic interaction between VIV cations in 1 and 2. [Copyright &y& Elsevier]

A novel cobalt phosphomolybdate: (NH3CH2CH2NH3)(NH3CH2CH2NH2)3Na3[Co4Mo12O24(OH)6(H2O)2 (HPO4)2(PO4)6]·8H2O 1, has been hydrothermally synthesized (200°C, 5 days, autogenously pressure) and characterized by IR, ESR, XPS, elemental analyses and X-ray crystallography. The crystal data: monoclinic space group C2/c, a=12.3281(3) Å, b=21.5729(4) Å, c=26.0242(5) Å, β=99.5401°(3), V=6825(2) Å3, Z=4, R1=0.0346, wR2=0.0650. The structure of compound 1 is based on Co[Mo6P4]2 units connected together via additional Co2+ ions to give a new three-dimensional framework. The interconnected void and channels in the cobalt molybdophosphate frameworks are filled with counter cations and water molecules. The magnetic property of 1 exhibits antiferromagnetic coupling interactions. [Copyright &y& Elsevier]

Abstract: Two novel polyoxometalate derivatives, {X IVWVI 10WV 2O40[Cu(en)2(H2O)]3} [X=V (1), Si (2); en=ethylenediamine], have been hydrothermally synthesized and characterized by elemental analyses, IR, UV–Vis, XPS, EPR, TG and single crystal X-ray diffraction analyses. They represent the first classical Keggin polyoxoanion supported by three transition metal complex moieties, which further act as the neutral molecular unit for the construction of the interesting three-dimensional supramolecular frameworks. The magnetic properties of 1 have also been studied in the temperature range of 4–300K, and its magnetic susceptibility obeys the Curie–Weiss law, showing antiferromagnetic coupling. [Copyright &y& Elsevier]

Abstract: Two new supramolecular compounds based on arsenic vanadates formulated as [H2As6V15O42(H2O)][Co(H2O)6]2·2H2O (1) and [H2As6V15O42(H2O)][Ni(H2O)6]2·2H2O (2) have been prepared by reacting V2O5, H2C2O4·2H2O, As2O3,·H2SO4, CoCl2·6H2O (NiSO4·6H2O) and enMe (enMe=1,2-diaminopropane) under mild hydrothermal conditions and characterized by elemental analyses, IR, ESR, XPS and single crystal X-ray diffraction analyses. Crystal structure analyses reveal that compounds 1 and 2 are isostructural and exhibit novel 2-D supramolecular layer structures constructed from arsenic–vanadium clusters and two different types of secondary building units (SBUs), respectively, the different SBUs are formed by joint of two adjacent [Co(H2O)6]2+ cations in compounds 1 and [Ni(H2O)6]2+ cations in 2, respectively. [Copyright &y& Elsevier]

Abstract: A novel polyoxometalate [Cu(phen)2]3{PW4 VIW5 VV3 IVO40(VIVO)3[Cu(en)2]}⋅4H2O 1 (en=ethylenediamine, phen=1,10-phenanthroline) has been synthesized hydrothermally and characterized by elemental analysis, IR, XPS, TG, EPR and single-crystal X-ray diffraction analysis. The crystal structure analysis shows that compound 1 contains a novel highly reduced tri-capped and mono-supported pseudo-Keggin-type heteropolyanion, {PW4 VIW5 VV3 IVO40(VIVO)3[Cu(en)2]}6−, three [Cu(phen)2]2+ cations and four lattice water molecules. They are further linked to form three-dimensional supramolecular networks through extensive hydrogen bonding and π–π stacking interactions. Interestingly, the water dimer and terminal oxygen of the cluster polyanion constitute a beautiful supramolecular helix chain. The heteropolyanion is the first example of tri-capped and mono-supported pseudo-Keggin-type tungstovanadophosphate and the pH value is crucial for obtaining compound 1 in synthetic procedure. [Copyright &y& Elsevier]

The title compound [NiII(phen)3]2[Cu10H2I16] 1 (phen=1,10-phenanthroline, C12H8N2) was hydrothermally synthesized from a simple reaction of CuI–NiCl2·6H2O–phen·H2O–H2O. X-ray analysis revealed that it consists of NiN62+ core cation and decanuclear iodocuprate(I) anion together with two dissociative H+ ions. In anionic unit, the discrete decanuclear iodocuprate(I) is formed by crystallographically independent five monovalent copper atoms and eight iodine atoms via an inversion center. There exist two types of Cu(I) coordination sites; only one copper(I) atom is in a highly distorted triangular planar site, and the other four copper(I) atoms display the tetrahedral geometries. It deserves to be noted that four types of bridging modes of I− ions in which two are ordinary μ2- and μ3-bonding modes can be found. But the other two are the rectangle planar geometry and the novel μ4-bridge like an “umbrella”, and both of them are rather rare in the halocuprates(I). Compound 1 was crystallized in triclinic space group P1¯ with a=11.6861(17), b=14.590(2), c=14.649(2) A˚, α=76.370(2), β=70.830(2), γ=81.320(3)o, R=0.075, and was characterized by elemental analysis, IR spectrum and UV-VIS spectrum. The third-order non-linear optical property of 1 was also investigated and the compound exhibits the reverse saturable absorption and self-defocusing performance. [Copyright &y& Elsevier]