Synthesis and Crystal Structure of [Ca(DMF)_6][Mo_6Br_8Cl_6]

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The reaction of MoBr2 with CaCl2 in DMF (N, N?-dimethylformamide) gives the cluster complex [Ca(DMF)6][Mo6Br8Cl6] 1 by using standard Schlenk techniques. This cluster complex crystallizes in triclinic, space group P1 with a = 10.329(4), b = 10.349(4), c = 12.510(5) ?, α = 103.793(5), β = 98.562(3), γ = 98.268(5)°, V = 1261.5(9) ?3, Dc = 2.509 g/cm3, Z = 1, C18H42Br8CaCl6Mo6N6O6, Mr = 1906.28, μ = 8.236 mm?1, λ(MoKα) = 0.71073 ? and F(000) = 894. The final R = 0.0589 and wR = 0.1458 for 2759 observed reflections with I > 2σ(I). The structure is composed of isolated octahedral coordination cations and discrete cluster anions, and these two kinds of ions connect each other to form a 3-D framework with similar packing patterns as CsCl through weak C–H···X (X = Br, Cl) hydrogen bonds. The reaction of MoBr2 with CaCl2 in DMF (N, N? -dimethylformamide) gives the cluster complex [Ca (DMF) 6] [Mo6Br8Cl6] 1 by using standard Schlenk techniques. This cluster complex crystallizes in triclinic, space group P1 with a = 10.329 (4), b = 10.349 (4), c = 12.510 (5) ?,? = 103.793 (5),? = 98.562 (3),? = 98.268 (5) ° and V = 1261.5 , D = 2.509 g / cm3, Z = 1, C18H42Br8CaCl6Mo6N6O6, Mr = 1906.28, μ = 8.236 mm? 1,? MoKα = 0.71073? And F000 = 894. The final R = 0.0589 and wR = 0.1458 for 2759 observed reflections with I> 2σ (I). The structure is composed of isolated octahedral coordination cations and discrete cluster anions, and these two kinds of ions connect each other to form a 3-D framework with similar packing patterns as CsCl through weak C -H ··· X (X = Br, Cl) hydrogen bonds.
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