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[{Cu(phen)(DMF)2}2(β-Mo8O26)] 1 (C36H44Cu2Mo8N8O30, Mr = 1963.39, phen = 1,10-phenanthroline) and [CuI(phen)2]2[{CuI(phen)}2Mo8O26] 2 (C72H48Cu4Mo8N12O26, Mr = 2518.90) have been synthesized from (Bu4N)2[Mo6O19], Cu(NO3)2·3H2O and phen using solution method and under solvothermal condition, respectively. Both compounds 1 and 2 are structurally characterized by elemental analyses, IR and single-crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic system, space group P21/n, with a = 16.3347(13), b = 9.861(1), c = 17.2827(14) A, β = 99.099(4)°, V = 2748.8(3) ·3, Z = 2, Dc = 2.372 g/cm3, F(000) = 1900 and μ = 2.614 mm-1. X-ray diffraction analysis reveals that compound 1 consists of discrete {[Cu(phen)(DMF)2]2(β-Mo8O26)} clusters constructed from β-[Mo8O26]4- subunits covalently bound to two [Cu(phen)(DMF)2]2- coordination groups. Compound 2 crystallizes in the monoclinic system, space group C2/c, with a = 33.1401(9), b = 16.4508(5), c = 16.2622(4) ·, β = 119.2460(10)°, V = 7735.7(4) ·3, Z = 4, Dc = 2.163 g/cm3, F(000) = 4896 and μ = 2.413 mm-1. X-ray diffraction analysis reveals that compound 2 consists of a centrosymmetric β-octamolybdate-supported complex anion [{Cu(phen)}2Mo8O26] and two bis-phenanthroline Cu(I) cations.
[{Cu (phen) (DMF) 2} 2 (β-Mo8O26)] 1 (C36H44Cu2Mo8N8O30, Mr = 1963.39, phen = 1,10-phenanthroline) and [CuI 2Mo8O26] 2 (C72H48Cu4Mo8N12O26, Mr = 2518.90) have been synthesized from (Bu4N) 2 [Mo6O19], Cu (NO3) 2 · 3H2O and phen using solution method and under solvothermal condition, Compound 1 crystallizes in the monoclinic system, space group P21 / n, with a = 16.3347 (13), b = 9.861 (1), c = 17.2827 (14) A, β = 99.099 (4) °, V = 2748.8 (3) · 3, Z = 2, Dc = 2.372 g / cm3, F (000) = 1900 and μ = 2.614 mm-1. 1 consists of discrete [[Cu (phen) (DMF) 2] 2 (β-Mo8O26)} clusters constructed from β- [Mo8O26] 4- subunits covalently bound to two [Cu groups. Compound 2 crystallizes in the monoclinic system space group C2 / c with a = 33.1401 (9), b = 16.4508 (5), c = 16.2622 (10) °, V = 7735.7 (4) · 3, Z = 4, Dc = 2.163 g / cm3, F (000) = 4896 and μ = 2.413 mm-1. a centrosymmetric β-octamolybdate-supported complex anion [{Cu (phen)} 2Mo8O26] and two bis-phenanthroline Cu (I) cations.