Abstract The reaction of [Fe2S2(CO)6] with one equiv. of o-OCH3C6H4CH2Br under the reduction of LiBHEt3 in dry THF afforded a tetranuclear cluster [(µ4-S){(µ-SCH2(o- OCH3)Ph)Fe2(CO)6}2] (1). Complex 1 crystallizes in monoclinic, space group P21/n with a = 16.5623(6), b = 12.8265(5), c = 18.2702(7) Å, β = 115.95(1)º, V = 3489.9(4) Å3, Z = 4, μ = 1.87 mm-1, Dc = 1.709 Mg/m3, T = 296(2) K, C28H18Fe4O14S3, Mr = 898.03, F(000) = 1800, S = 1.10, R = 0.032 and wR = 0.058. Complex 1 consists of two diiron fragments possessing a {Fe2(CO)6} core. The two diiron units are bridged by an inorganic sulfide in a µ4-S binding mode and the sulfide is in a distorted tetrahedral geometry with the four iron atoms at each corner of the distorted tetrahedral. In its solid state, two types of non-classic intermolecular hydrogen bonding interactions plus a weak π-π stacking interaction led to a 2-D network.
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