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Oligophosphine ligands. XI. Hexacoordinate halogenoiron complexes FeX2[P(CH2CH2CH2PMe2)3] (X = Cl, Br, I)

1985; Elsevier BV; Volume: 104; Issue: 1 Linguagem: Inglês

10.1016/s0020-1693(00)83785-8

1873-3255

Martin Antberg, L. Dahlenburg,

Metal complexes synthesis and properties

The reaction of anhydrous iron(II) halides with the tripod tetra(tertiary) phosphine P(CH2CH2CH2PMe2)3 gave the complexes cis-FeX2[P(CH2CH2CH2PMe2)3] with X = Cl (I), Br (II), and I (III). Crystals of I–III are monoclinic, space group P21/n (Z = 4) with a = 946.5(3), b = 1416.8(5), c = 1682.9(8) pm, and β = 104.85(3)° for the chloride I, a = 952.9(4), b = 1456.3(8), c = 1671(1) pm, and β = 104.89(4)° for the bromide II, and a = 959.8(9), b = 1510.1(7), c = 1688(2) pm, and β = 104.29(9)° for the iodide III, respectively. The X-ray structures were solved by conventional methods and refined to the following discrepancy indexes: I, R = 0.062, Rw = 0.067 (1109 data);II, R = 0.088, Rw = 0.080 (972 data); III, R = 0.097, Rw = 0.102 (799 data). The coordination geometry of the complexes corresponds to distorted octahedral. Selected bond lengths are (in pm): FePMe2 (trans-atom P); 233.8(5) and 230.6(5) for I, 230(1) and 229(1) for II, and 2 × 233(2) for III. FePMe2 (trans-atom X); 223.1(5) for I, 225(1) for II, and 228(2) for III. FeP; 220.2(5) for I, 223(1) for II, and 223(2) for III. FeX; 241.0(4) and 238.8(4) for I, 255.5(6) and 255.0(6) for II, and 273.9(8) and 272.5(8) for III.