By controlling the temperature of the reaction systems, three new inorganic–organic hybrid arsenomolybdates [Cu4(en)4O2(H2O)2][H2AsV2Mo6O26] (1) (en = ethylenediamine), [Cu(en)2(H2O)]4[Cu(en)2(H2O)2]{[Cu(phen)(en)][AsIIIAsVMoVI9O34]2} (phen = 1,10-phenanthroline) (2) and (H2en)[Cu(en)2][(CuO6)Mo6O18(AsIII3O3)2]·10H2O (3) have been hydrothermally synthesized and characterized by single-crystal X-ray diffraction analysis, elemental analyses (EDX-SEM), X-ray powder diffraction (XRPD), IR spectroscopy, UV spectroscopy, XPS spectroscopy and thermogravimetric analysis. The experimental phenomenon demonstrates that different temperature ranges correspond to different proportions of oxidized AsIII atoms. 1 presents an infinite 1-D chain structure based on the rare secondary building units [H2As2Mo6O26]4− and unprecedented tetra-Cu clusters [Cu4(en)4O2(H2O)2]4+. The dimer 2 is constructed from a dual-ligand transition-metal complex [Cu(phen)(en)]2+ sandwiched by two scarce [AsIIIAsVMoVI9O34]6− fragments. 3 shows a 1-D chain structure built by [(CuO6)Mo6O18(As3O3)2]4− units and [Cu(en)2]2+ bridges. The magnetic measurement indicates that 1 demonstrates the antiferromagnetic couplings within the {Cu4} cluster.
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