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67650408462
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Synthesis of compound 1: A mixture of CuG2· 2H2O (1.2 g, Na2MO4·2H2O (1.6g, H3PO4 (0.5mL, 85, diethylene-triamine (NH(CH2CH2NH2)2, 0.8 mL) and water (15 mL) was simply stirred (the initial pH value was adjusted to 6.20 by 2 M KOH, then sealed in a Teflon-lined strainless steel autoclave and heated at 170°C for 7 days. After cooling to room temperature over 48 h, crystals as blue needles were obtained in 48% yield based on molybdenum. Elemental analysis Calcd for C12H50N9Cu3Mo 5O28.5P2 (1508.85, C, 9.55; H, 3.34; N, 8.35, Found: C, 9.33; H, 3.43; N, 8.24, IR (KBr) pellets, v/cm-1, 3317(w, 3238(w, 1621(m, 1454(w, 1384(w, 1262(w, 1096(m, 1068(m, 1034(s, 1017(s, 977(w, 91(w, 902(s, 882(s, 680(s, and 566w
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-1): 3317(w), 3238(w), 1621(m), 1454(w), 1384(w), 1262(w), 1096(m), 1068(m), 1034(s), 1017(s), 977(w), 91(w), 902(s), 882(s), 680(s), and 566(w).
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67650454701
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Crystal data for 1 C12H50Cu3Mo 5N9O28.50P2: Mr, 1508.85, orthorhombic, P 2(1)2(1)2(1, a, 9.2933(16) Å, b, 17.967(3) Å, c, 25.271(4) Å, V, 4219.57(121) Å3, Z, 4, Dcaled, 2.358g/cm3, μ, 3.093 mm-1, F(000, 2916, T, 296(2) K. 23690 reflections measured, 8288 independent (R int, 0.0332, R1, 0.0294 (1 > 2σ(I, wR2, 0.0828 all data, CCDC number: 696832
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2 = 0.0828 (all data). CCDC number: 696832.
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37049072826
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Supporting Information is available electronically on the CSJ-Journal web site
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Supporting Information is available electronically on the CSJ-Journal web site, http://www.csj.jp/journals/chem-lett/index.html.
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